CUSTOMS LABORATORY GUIDE

(September 2002)

WORLD CUSTOMS ORGANIZATION

 CLG/AS 1-Sep. 2002

I.

Chapter 1 : Model layouts of Customs laboratory

1. Introduction
2. Organization
3. Design
4. Administration
5. Safety and anti-pollution measures
6. Sampling
7. Operations
8. Preparation of laboratory worksheet and laboratory report
9. Quality assurance

Chapter 2 : Laboratory equipment, instruments and apparatus

1. Basic equipment, instruments and apparatus

2. Special instruments and apparatus required for Harmonized System classification
3. Other equipment, instrument and apparatus which may be needed in a standard and
advanced Customs laboratory
4. Instrument maintenance and attention

Chapter 3 : Chemical reagents, reference chemicals and materials

Chapter 4 : Technical literature and reference books

II. QUANTITATIVE CRITERIA IN THE HARMONIZED SYSTEM REQUIRING

LABORATORY ANALYSIS

III. RECOMMENDED ANALYTICAL METHODS

Chapter 1 : International standards and methods

Chapter 2 : Methods applicable to specific products in the Harmonized System

Chapter 3 : Illicit drug analysis.

Appendix I : 1. Safety design consideration

2. Basic chemical storage principles

3. Engineering considerations

Appendix II : Standard infra-red spectra compendium on illicit drugs

Appendix III : Summary information on Customs laboratories

1.
I. ESTABLISHMENT OF A CUSTOMS LABORATORY

Chapter 1 : Model layouts of Customs laboratory

1. Introduction

1.1. General

The Customs Laboratory Guide is primarily meant to be a practical handbook for

the establishment or improvement of Customs laboratories in developing countries. The
Guide includes the "best practices" covering a variety of laboratory operations. It is
recognized that it would not be possible or necessary for any laboratory, to implement
all of these provisions. Thus, the Guide can only present ideas and recommendations
to the reader who is expected to apply these to his or her own laboratory facility.
According to the need of his or her Administration to the extend possible and
appropriate.

A large part of the successful planning of a Customs laboratory depends on how

well the planner understands the needs of the laboratory. There is no fixed formula for
designing a Customs laboratory.

Customs laboratories differ from other laboratories principally in the fact that they
are called upon to analyse many different kinds of goods for Customs tariff, trade
statistical, drug enforcement and other purposes.

Customs laboratories must therefore be able to establish an efficient system

whereby samples of goods for analysis are channelled to the laboratory, prompt and
accurate analyses of such samples are performed, and the results of the analyses are
expeditiously conveyed to the Customs officer concerned for appropriate action.

The Guide's model layouts seek to provide the information necessary to plan all
aspects of the design of a Customs laboratory. The various organizational, design and
operational considerations are discussed in detail from the viewpoint of the
establishment of a standard Customs laboratory.

Taking into account the different needs of countries and the resources available
for Customs laboratories, model layouts of basic and advanced Customs laboratories
are also dealt with in relation to the model layout for the standard laboratory.

It is, of course, impossible to write a Customs laboratory guide that would be

suitable for all circumstances or cover all eventualities. It is hoped that the information
set forth in the Guide will help Customs administrations to participate actively in the
design or improvement of their own facilities.

The mark of a good laboratory design is that efficiency, safety and economy
complement each other. In essence, it is necessary to create an environment that is
conducive to an administration's way of operation, without compromising safety and
efficiency, or adversely affecting performance.

Finally, the user of this Guide should always keep in mind that the information and
principles presented are advisory and represent recommendations on how a Customs
laboratory could be organized, arranged, etc., not how it must be.

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1.2. Basic, standard and advanced Customs laboratories

It is not possible to define precisely what is meant by basic, standard and

advanced Customs laboratories; all Customs laboratories differ to some extent from
country to country in general terms. In the Customs Laboratory Guide, basic, standard
or advanced Customs laboratories are assumed to have the following characteristics
respectively :

A basic Customs laboratory is a non-instrumental laboratory, or a laboratory which

has only a few basic instruments, with a few staff to perform only specific analyses
required by the country for the classification of goods in the Harmonized System in a
cost-effective manner.

From the practical standpoint, it is not always desirable to establish a standard-

sized Customs laboratory. For example, a country where the total number of goods
traded is low, may wish, for financial reasons, to establish a small-sized Customs
laboratory for the analysis of key samples, specific samples of goods subject to rapid
clearance, or suspicious samples collected at Customs offices, rather than to set up a
standard-sized Customs laboratory.

A standard Customs laboratory is a basic-instrumental laboratory with sufficient

staff and equipment to perform most of the analyses required by that country at least for
the classification of goods in the Harmonized System.

An "advanced Customs laboratory" is characterized by its competency to carry out

a diversity of quantitative and qualitative analyses (especially the successful
characterization of diverse, unknown commodities). This requires most, if not all, of the
13 1
advanced instrumental technologies (GC, IRS, MS, HPLC, C/ H NMR, ICP, SEM,
XRD, etc.) and a staff experienced in the interpretation of data relative to a wide range
of industrial commodities.

The model layout of a Customs laboratory described below seeks to provide the
information necessary to plan all aspects of the design of such a laboratory. The
various organizational, design, administrative, safety, anti-pollution, sampling,
operational and quality-assurance considerations are discussed in detail.

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2. Organization

2.1. Organizational structure

Although there are obviously differences among countries as regards the type of
Customs laboratory which may be needed and the resources available for this purpose,
the organizational structure of a typical standard Customs laboratory should be as
follows :

Head of Laboratory

Supervisor of Supervisor of
analytical staff administrative staff

Chemists Technologists Building Administrative

Support staff

2.2. Head of the laboratory

The duties of the Head of the laboratory are numerous. For this reason it is not
possible to do more than to draw attention to certain aspects of the position.

The main mission of the Customs laboratory is to analyse a large number of

samples of all kinds of goods and to provide any necessary technical advice, as
required for Customs tariff, trade statistical, drug enforcement and other reasons, as
quickly as possible and with great accuracy. Consequently it is desirable for the Head
of the laboratory to be a graduate chemist with experience and training in Customs
procedures and particularly in the analysis of goods for tariff classification and drug
enforcement purposes.

The laboratory Head is responsible for the efficient and effective performance of
the Customs laboratory through the recruitment, hiring, training, development and
motivation of subordinates, the development of resource and work plans, the
establishment of responsibilities, priorities and objectives and the monitoring of work
performance.

The Head of the laboratory is also responsible for the preparation and the
administration of the laboratory budget. In this connection he must be able to bring the
needs of the laboratory to the attention of higher authorities for appropriate action to
allow as high a level of technical efficiency and expertise as possible to be maintained
and developed.

The laboratory Head may have to give evidence in court, provide guidance to staff
on court procedures, or otherwise provide information used in court. He should,
consequently, have some understanding of court procedures.

Usually the duties of the Head of the laboratory, in his or her absence, are
handled by a senior chemist or the head of the analytical staff.

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 2.3. Analytical staff

The basic function of the analytical staff is to analyse the samples received by the
laboratory and to issue a report therein providing the requested information. Analytical
staff may offer advice required for tariff or statistical classification, drug enforcement or
other requirements which are within the competence of the laboratory.

Depending on the size of the analytical staff, it may be necessary to divide the
group into two or more units. It is common to subdivide on the basis of principal types
of commodities, i.e. textiles, foods, polymers, etc. The division of the analytical staff into
commodity specific groups allows for specialization, which improves the overall
capabilities of the laboratory.

Whether, and to what extent, the laboratory undertakes the role of performing
work other than purely analytical work will be a matter of organizational policy. The
policy will depend on a number of factors including the sophistication of the laboratory
and the availability of alternative facilities. The analytical staff may also be required to
appear in court as fact or expert witnesses.

The analytical staff of a standard laboratory should consist of highly qualified

chemists, preferably university graduates, and trained technicians. The chemists should
have extensive experience and training in the analysis of goods for purposes of tariff
classification and drug enforcement, and a fairly good knowledge of Customs
procedures. This includes a thorough knowledge of the Harmonized System which is
necessary to ascertain which analyses should be undertaken.

It is not economical and not even wise from the point of view of efficiency of the
laboratory to involve only graduate chemists in analytical work. Specially trained
laboratory technicians who have received a two to three year practical training course in
laboratory analysis can be particularly useful in carrying out a number of routine or even
highly complex analyses under the supervision of a chemist. As is the case with
graduate chemists, laboratory technicians also need specialised on-the-job training in
tariff classification, drug enforcement and other Customs matters in addition to technical
training to remain current.

There is no fixed or accepted ratio for the number of laboratory technicians

needed in a laboratory per chemist but a team of one chemist and three or four
laboratory technicians have been demonstrated in practice to be appropriate where the
work is less repetitive and methods frequently have to be developed or modified, and
where data interpretation (such as in the qualitative identification of unknown or poorly
defined products) is common, then a higher ratio of chemists.

2.4. Supervisory staff

In laboratories where the number of analysts exceeds six to eight, a supervisor is

needed. In a laboratory of this size a supervisor cannot be expected to do analytical
work; his or her time is usually taken up with the management of the analytical staff. In
smaller laboratories, it is desirable for the supervisor to spend a portion of his or her
time on a variety of non-routine analyses to retain familiarity with instruments and to
keep abreast of state-of-the art techniques.

The duties of a supervisor are numerous. He or she assists the Head of the
laboratory in over-all management, work planning, receiving and assigning samples for
analysis, work review, ensuring the availability of the necessary supplies and
equipment, etc. The supervisor should also recommend training for the analytical staff.
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2.5. Administrative staff

The administrative staff include all administrative assistance such as secretarial,

typing and filing, record-keeping (logging and tracing samples, financial record-
keeping), maintenance of laboratory stores, management assistance, cleaner service
and library services (if the laboratory library is of a size to need a librarian).
Administrative staff are very important to the effective operation of a laboratory.

In addition to clerical support staff, the laboratory may also require building
support staff (described below).

It is uneconomical to have inadequate administrative staff because then their work

must be performed by chemists or other staff who should be involved only in analytical
work. Support staff should usually number 15 to 20% of the number of total analytical
staff.

2.6. Building support staff

Part of the work performed in any laboratory, regardless of the size, is not directly
connected with the actual analytical or administrative duties. Some of this support work
includes maintenance of the heating, cooling, water, and electrical systems; removal of
garbage; upkeep to the exterior of the building and land or parking around the building;
cleaning of the laboratory; heavy lifting and moving; etc. These duties can be
performed by support staff without special educational qualifications. Personnel doing
these duties should be made aware of laboratory hazards and instructed in safety
procedures immediately on starting the job and on a regular basis they should be
informed of all the risks associated with chemicals or instruments they may come in
contact with.

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3. Design

3.1. General considerations

When a new laboratory is being built, close co-operation is required between the
architect who designs it and guides its construction and the chemists who are familiar
with the technical needs of the laboratory. It is important to employ architects that are
familiar with laboratory operations and design in corporation with chemists of the
laboratory. Standard construction techniques are not always the best for laboratories.
The users must be involved starting from the design stages and there must be open
lines of communication between the architects, engineers, contractors, tradesmen and
users throughout the design and construction process.

However, it is not often that chemists have the chance to take part in the planning
of a completely new laboratory building. More often one has to make do with an old
and, sometimes, inadequate facility. In both cases, whether designing a new laboratory
or renovating an old one, it is important to take into account the possibility of the need of
future expansion or improvement of the laboratory, however unlikely that may seem at
the time. The installation of new scientific instruments and equipment will require
additional space.

Wherever possible, the placement of controls, the location of safety equipment

and room layouts should be standardized.

3.2. Basic structure

In planning a Customs laboratory, whether for an old facility or a new one, the
rooms for the different laboratory activities must be located and designed in a manner
well adapted to the purpose. For this reason it is necessary to know the goods which
are to be analysed in the laboratory and the volume and frequency of submissions to
the laboratory of the principal types of commodities. With the help of this information it
is possible to calculate the number of analyses to be carried out, the level of analytical
examinations involved and to determine the specific instruments and equipment
needed.

After the number and quality of analyses required has been evaluated it is
possible to determine the time needed for analyses. Based on this information the size
of the staff and surface area of the laboratory premises can be estimated.
2
It is normal to allow about 10 m of laboratory space and 3 m of bench surface per
analyst (minimum value from which to start). In addition to actual laboratory premises,
space is also needed for offices (including a meeting room), storage and major pieces
of analytical equipment. These generally make up roughly 40% of the total area of the
laboratory.

In planning a Customs laboratory, for flexibility in meeting changing needs, it is

best to allow some areas of the laboratory building to remain "open-plan" to the extent
possible, including the area used as offices. However, there are certain basic concepts
for the layout of the laboratory which should be taken into consideration when planning
a Customs laboratory (e.g., segregation of the office area from the laboratory area is
highly desirable).
These are :

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 (a) Separation of the instrumental analysis area and the chemical analysis area in
order to avoid contamination of expensive scientific instruments by various chemical
reagents and to ensure their long operating life.

(b) Ensuring that the analysis area for flammable or hazardous goods is separated
from the office area, but close to it. If the Customs laboratory is large enough, the
floors for offices (including meeting room and library) and for the operational
laboratory zone should be separated (e.g., the ground floor for administrative
offices and the first floor for the operational laboratory zone). The area must be
constructed with the necessary ventilation, precautions against electrical (including
static electricity) sparks or other ignition sources.

(c) Allocation of a quiet but convenient location for a weighing or balance room. A
separate balance room is recommended to avoid unnecessary draughts and
vibrations caused by ventilation systems, laboratory workers, machines, etc.

(d) A special room is desirable for an infra-red spectrophotometer (with air-conditioning

in areas of high temperature and humidity, and with a filter system for dust).

(e) A separate outside storage room is recommended for flammable or hazardous

chemical reagents and laboratory waste materials in a large laboratory.

(f) A separate outside storage room is recommended for high-pressure gases (e.g.,
hydrogen and nitrogen).

(g) The location of fume cupboards and exhaust fans should be carefully considered to
ensure effective ventilation throughout the laboratory. The air intake for the heating
and cooling system should be located upwind of the fume cupboard exhausts and a
good distance from them. The fume cupboards should also have high stacks on
them to allow the fumes to dissipate thoroughly.

(h) The sample preparation area should be separated from laboratory rooms where
analysts are working on trace analyses or using sensitive instruments.

Cylinder Hazardous chem ical

stores stores

Receiving Stores

Instrum ent
laboratory
area
O ffices O ffices

Chemical laboratory
area

Adm inistrative area

Front
Fig. 1. Basic structure of a Custom s laboratory

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 Taking these basic concepts into account a Customs laboratory layout that offers
flexibility, safety and good work flow is shown in Fig 1.

The administration section is located at the front of the building. This office area
has up to four enclosed offices and a conference room with open-area work areas for
the rest of the computer and clerical staff. If the staff is large enough, a cafeteria or
coffee room should be provided in this area.

Separated from the administration area by a fire wall are the chemical and
physical instrumental laboratories with closed and open offices for supervisors, chemists
and technologists running along the outer walls and separated from the laboratories. At
the rear of the building, there is a sample and equipment receiving area, and stores
areas for new and old samples, chemicals and supplies. Separated from the main
building should be two fireproof and locked storage facilities. One should contain
flammable solvents and hazardous chemicals used for analyses, as well as old
hazardous samples which are awaiting disposal. The other building should contain
compressed gases, both full and empty cylinders.

3.3. Space utilization

The work space in a laboratory must be planned and designed to accommodate

laboratory activities and to ensure proper work flow. The most common equipment in
laboratory facilities consists of benches. An important consideration in this connection
is that the benches be designed and equipped for the intended purpose and that their
placement be carefully considered. The placement of furnishings can significantly affect
operational efficiency and safety.

Bench setups for chemical laboratory rooms and for analytical instrumentation
(Figure 2) are quite different.
60 75 60
Blocking to fasten cabinets

Access Base
Wall unit space unit
75

Analytical centre bench

Electricity
60
Fixture
Electricity

Fixture
60 3

Piping 90 Piping
20 Base unit

Base unit

Wall bench

Fig. 2. Traditional casework system - wall supported. (Measures in centimetre)

3.3.1. A Room for chemical analysis

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 The benches in a room for chemical analysis can be placed in two different
ways as shown in Figure 3 and Figure 4 (often referred to as island benches and
peninsular benches, respectively).

Sink Sink

Fume cup-board
Fume cup-board

•• • • • •
•• • • • •
•• • • • •

Space for people to pass

Wall bench

0 1 2 3 (m)
Fig. 3. Fig. 4.

Both of these placings have their advantages. The standard width used for a
single bench is 60 cm, which is about the same as the width of the space required by
a standing analyst.

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 By comparing peninsular benches and island benches it can readily be seen
that the maximum bench area is obtained with the peninsular bench placing, which
makes this placing preferable if floor space is limited. With the island bench placing,
the working surface is somewhat more accessible and allows more flexibility for the
placement of windows and doors.

One of the other benefits of the peninsular bench placing is that the analyst
working between the benches has access, in effect, to three working surfaces at
once. This is, of course, very convenient if there are several different analyses in
progress at the same time. It should be stressed that the space between benches
should be enough to allow two analysts to work back to back (at least 1.5 m).

It could also be argued that the peninsular bench placing is safer since the
traffic patterns in the laboratory tend to be more restricted and predictable. In the
final analysis the choice of bench placing depends very much on the size and shape
of the room available.

For health and safety reasons, analysts should not have desks in rooms where
chemical work is performed. However, the desks or offices should be close to
analytical work stations.

Another important aspect to remember is that furniture and equipment in

laboratory work areas should be arranged so that an exit may be reached easily from
any point. Two means of egress are required at a minimum for every laboratory
room and they should be remote from each other and so arranged as to minimise
any possibility that both may be blocked by fire or other emergency condition.

Bench with cupboards and shelves above

(EXIT) CHEMIST # 1 CHEMIST # 2 (EXIT)

Sink Sink
Bench Hood 1 Hood 2 Bench

Fig. 5. Two-chemist/technologist chemical laboratory module

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 For a laboratory with more than 10 or 12 chemists/technologists, consideration
should be given to using two person modules as shown in Fig. 5. These modules are
safer than large open laboratory areas since chemical operations are separated from
each other. Further consideration should be given to arranging the modules around
a laboratory core which houses the more commonly used pieces of equipment (e.g.
infra-red, gas chromatography), and arranging the analysts' offices around the
outside of the laboratory modules. This arrangement keeps each
chemist's/technologist's work area separate, allowing the analyst to work safely,
while integrating his or her analytical work area with their office area and the more
commonly used instruments in the laboratory core.

3.3.2. A Room for physical instrumental analysis

Before planning an instrument laboratory room (i.e., a room for physical

analysis) it is necessary to determine the specific instruments (as well as their
accessories) which are likely to be installed in it. The room should reflect the
specifications of the instruments.

The physical specifications and service requirements of the instruments should

be obtained from the instrument suppliers. On the basis of this information the size
of the room needed can be determined and the physical layout of benches drawn,
taking into consideration not only the area required for instruments but also the
surrounding area that must be left open for operations and maintenance.

This room should also be temperature controlled and provided with ventilation
ducts or hoods to remove gases formed during operation of instruments, such as gas
chromatographs, etc. The room should be reasonably vibration free and be equipped
with uninterruptible electrical power. As far as possible, this room should be open to
allow for reconfiguration as new pieces of equipment are obtained.

In a larger laboratory, one room for all the large analytical instruments will not
suffice. Instruments such as gas chromatographs (GC), gas chromatograph-mass
spectrometers (GC-MS), nuclear magnetic resonance spectrometers (NMR), X-ray
diffractometers (XRD), etc., will probably require their own room and specific
technologist. These separate rooms are necessary for various reasons, e.g., health
and safety considerations, special cooling requirements, low vibration areas, etc.

3.3.3. Balance room

The balance room should be designed to protect precision balances from

corrosive atmosphere, dust and draughts. If possible, the room should have a
filtered, low-velocity air supply and be vibration free. The balance table must be
made of stone or concrete in order to reduce vibrations. While the balance room will
not be occupied full time, it should be conveniently located.

Because of great improvements in balances in the last few years, it may not be
necessary to have a separate balance room if the laboratory can afford some of
these newer balances. These balances, because they are very shockproof and are
small, fit well in the individual laboratories and save valuable analyst time.

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 The balance table for high precision balances (resolving to better than 0.001 g)
should be of high mass construction, free standing and physically separate from
surrounding benching, etc. (to prevent vibration transmission). Also, it should be
designed to avoid the operator knocking or resting his/her feet on the balance table
(low level rails), again to prevent upsetting the solving capability of the balance.

3.3.4. Storage facilities

3.3.4.1. General recommendations for chemical storage :

The main factors that should be considered in providing for the safe and
efficient storage of hazardous chemicals are compatibility, optimum use of storage
space, separate air supply and exhaust, safety, and convenience of storage and
retrieval.

Storage racks and shelves should be designed to prevent breakage or

leakage, which might cause damage or endanger those who enter or work in the
storage area. Storing large and small containers on the same shelf can make
retrieval difficult and breakage likely. For this reason shelves should be sized and
spaced appropriately for storage of compatible materials by container size.
Ventilation should be provided to prevent corrosion or dangerous concentrations of
vapours.

National regulations may provide some important guidelines for the design of
storage areas in order to minimize danger from fire, explosions and contamination
of the environment. However, such regulations usually cannot address all of the
safety and health aspects of chemical storage, particularly as new chemicals come
into use and new hazards are discovered. Furthermore, national regulations are
generally written for the storage of large containers and industrial quantities and,
therefore, may not be appropriate for the storage of chemicals in small or break-
resistant containers.

The type and size of containers to be stored will affect the need for special
storage practices and safety procedures.

Ventilation is needed for chemicals and containers which may release

dangerous quantities of vapours or gases which are flammable, corrosive, irritating
or toxic.

Doors to chemical storage areas should be identified with the hazards of the
materials stored in the area.

Another important safety consideration for storage areas is, of course,

sufficient and explosion-proof lighting.

The laboratory designer should seek guidance from chemists with respect to
the design of storage areas.

3.3.4.2. Location of storage facilities :

Storage facilities should be located where they will be safe, convenient and
economical.

The storage facility should be separated from the rest of the laboratory and
protected so that a spill or fire is not likely to spread beyond the storage area.
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 Within laboratory work areas, storage for working quantities should be
provided under the fume cupboards in ventilated cabinets for volatile, flammable
chemicals. Such storage should be limited to chemicals which are used frequently,
quantities that are the minimum necessary and container sizes that are the
minimum convenient.

Stockrooms or similar accessible supply areas should be provided for small

amounts of frequently needed chemicals that are not stored in laboratory work
areas. If these chemicals are flammable or reactive, or give rise to health concerns
they should be placed in an isolated, independently ventilated room or preferably in
an exterior fire-proof locked storage building.

3.3.4.3. Flammable liquid storage cabinets :

Special storage is commonly required for flammable liquids. Liquids which

require such storage have flash point temperatures at or below 95 °C.

Depending on the quantities of such liquids within the laboratory they should
be stored in either an approved storage room or in a storage cabinet. Laboratory
facilities usually require a separate, fire-protected room used only for the storage of
bulk quantities of flammable liquids.

Preferably, large stock supplies of flammable and hazardous liquids should be

stored in a fire-proof locked building separated from the main laboratory area. If
possible, no more than two or three 20-litre containers of each solvent should be on
hand at any time.

Storage cabinets should be designed to insulate their contents so that in case

of fire outside of the cabinet, the internal temperature will not exceed 165 °C within
10 minutes. There are commercially available double-walled storage cabinets
which provide the minimum protection required.

There should be a mechanical system to provide effective ventilation and

exhaust of hazardous and flammable vapours from chemical storage cabinets. The
ventilation ducting of these cabinets should also be fire resistant.

3.4. Equipment and instruments

3.4.1. General considerations

When planning a Customs laboratory one should not underestimate the

complexity of equipping the laboratory.

At the stage of establishing a new laboratory the requirements for equipment

and instruments may seem large and complex since certain types of analysis may
require several individual pieces of equipment and if even one is not available the
analysis cannot be performed. On the other hand most of the instruments and
equipment are common to different analyses so that once they are procured there
comes a point at which productivity of the laboratory can rise sharply compared to
investments in new instruments.
Plan the laboratory so that it is very flexible - design for the future !

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 The total operating expenses depend, of course, on the size of the laboratory
and are related to many different factors. One of the important expenditures involves
the maintenance, repair and replacement of equipment.

In the developing world, one of the major problems in carrying out effective
laboratory operations is broken equipment. The degree of sophistication of
equipment varies greatly from a straightforward pH meter to a complex instrument
such as a spectrophotometer. It is therefore necessary that adequate provisions be
made for obtaining professional repair services and replacement parts. It is false
economy if analysts are being paid but cannot perform an important part of their work
due to lack of maintenance.

Although Customs laboratories may require special equipment for specific tests
under the Harmonized System, it should be noted that few Customs administrations
(if any) possess all such instruments and apparatus, given that some are rarely used
and are very expensive. Careful consideration should be given to cost and benefits
when purchasing these special instruments and apparatus. It is recommended that
laboratory facilities outside of Customs be found to carry out these special
examinations.

Some of the basic instruments and equipment needed in a Customs laboratory

are listed in Part I, Chapter 2, Sub-Chapter 1. Special instruments for specific
examinations required for HS classification and additional equipment which may be
needed are set out in Part I, Chapter 2, Sub-Chapters 2 and 3, respectively.

The needs of Customs laboratories vary from country to country, depending on

differences in tariffs, the volume of and type of trade, etc. Therefore it is only
possible to outline some of the instruments which may be useful for a standard
Customs laboratory.

3.4.2. Fume cupboards

3.4.2.1. General considerations :

The major items of fixed equipment in a Customs laboratory are the fume
cupboards. The use of solvents, and noxious chemicals in analysis require a
greater use of fume cupboards than other types of laboratory work. The number of
fume cupboards in the laboratory should be sufficient so that work is safe and all
handling of volatile compounds can be done in the hoods.

A fume cupboard should be designed so that it ensures a high degree of

personal safety. Remember that the fume cupboard is probably the most important
piece of safety equipment available to the analyst. The hood should be large
enough to accommodate most common operations. Fume cupboards may be
purchased prefabricated with utility outlets and are available in standard sizes
ranging from 90 cm to 1.5 m in length with larger hoods available on a custom-
made basis. However, today with energy costs rising and because the size of the
hood is directly proportional to its energy consumption it is not wise to select a
larger-than-necessary unit.

It is advisable to make the hood as flexible as possible by placing many utility

outlets in it, although costs may limit this possibility. It is necessary, however, if
purchasing or constructing the hood locally to specify the type, quantity, and
placement of every required service fixture such as for water, gas, electricity and
drainage.
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 The installation of exterior controls for the utility service fittings is highly
recommended. This permits access to the services from outside the hood while the
unit is in operation. It is also prudent to have the fixture outlets colour coded for
easy identification of each fixture.

Lighting inside the hood chamber is very important. Normally, a vapour-proof

fluorescent light fixture is used, which gives a pleasant light as well as adequate
illumination.

The fume cupboard is usually opened by lifting the vertically-rising front glass
window which is counterbalanced with weights. The window is normally constructed
of 6 mm laminated glass. The fume cupboards with windows that move from left to
right instead of up and down are not recommended. (see Figure 6).

The material for the construction of fume cupboards is most important,

especially if a fume cupboard must withstand acid fumes, in general, and perchloric
acid fumes, in particular. The hood lining is normally made from 6-7 mm thick
material that is both heat- and chemical- resistant.

S ta n d a rd v e rtic a l ris in g H o riz o n ta l s lid in g x

F ig . 6 . F u m e c u p b o a rd

Linings made of plastics or stainless steel are used. Figure 7 shows the
schematic structure of a fume cupboard.

I/C1/3/10
 1 5 0 /1 2 0 /1 0 0 85

140

220

80

F ig . 7 . S c h e m a tic s tr u c tu r e o f fu m e c u p b o a r d ( M e a s u r e s in c e n tim e tr e )

Some recommendations for the materials and equipment for a fume cupboard
are set out below :

Sliding window

- The sliding window should be made of 6 mm laminated glass and

counterbalanced with weights

Worktop

- Acid-resistant stainless steel, ceramic material, epoxide resin or polypropylene

Lighting

- Fluorescent tube or any other explosion-proof source

- Switches on front panel

Taps

- 1 Cold-water tap
- 1 Gas tap
- 1 Compressed-air tap

All taps should be front-operated.

3.4.2.2. Ventilation of fume cupboards :

Generally the fume cupboard is so constructed that air flows in through the
front opening and goes up along the rear wall of the hood's interior. The hood is
normally designed with adjustable slots at the top of the chamber as well as at the
countertop level. By opening or closing these slots the direction of the exhaust can
be adjusted and controlled.

I/C1/3/11
 The total volume of air needed for a fume cupboard depends on the size of
the front opening and the velocity of air circulating through the hood. If, for
instance, the airflow through the open face of a fume cupboard is 0.5 m/sec (which
is the minimum requirement), the width of the fume cupboard is 180 cm and the
3
height of the face opening is 60 cm, the volume of air needed is 540 cm /sec or
3
1944 m /h.

The size of the fan motor of the exhaust duct must be sufficient to meet the
requirements of the hood's ventilation and to overcome the static pressure
generated by the ventilation duct (static pressure is the loss in efficiency caused by
friction as the air passes through the exhaust system).

Static pressure varies directly with the length of the ventilation duct as well as
with the number and type of bends. Incorrect determination of static pressure can
lead to selection of incorrect exhaust fans. It is therefore recommended to use the
assistance of a qualified engineer in designing the ventilation system.

The exhaust fan should be located as far away from the hood as possible,
preferably on the roof of the laboratory, away and downwind from fresh air intakes
for the building. Exhaust gas should be released outside through a filter, if
possible. In this way negative pressure can be maintained throughout the duct
system preventing duct leakage which may contaminate the laboratory.

The fume cupboard should be placed in an area in which cross-currents of air

are minimal. One of the major factors in reducing hood efficiency is locating a hood
near an active doorway. The movement of the door can draw vapours out of the
chamber. Walking past a hood can also have a negative influence.

The chamber of the hood should be kept as clear and open as possible to
allow air to pass through. A fume cupboard used for chemical work should not be
used to store chemicals.

If any apparatus that does not have legs is housed in the hood it should be
placed on blocks in order to allow air to flow beneath it. It is also good work
practice to place the source of contamination at least 15 cm inside the hood as this
will dramatically increase the margin of safety.

The ventilation system of the fume cupboard should be kept operating all the
time, even over night. If a fume cupboard is not in use and the glass window is
closed, ventilation can be reduced to half in order to save energy. Two-speed fans
will also significantly reduce energy costs. Constant ventilation prevents dust from
collecting in a fume cupboard and moisture from condensation in ventilation ducts.
There should be a signal light in the fume cupboard which indicates when the
ventilation is on (a small piece of thin paper attached to lower edge of the glass
window also works as an indicator by vibrating if the ventilation is working).

It is well recognized that fume cupboards represent probably the single

greatest safety feature in any laboratory. Therefore it is advisable for all
laboratories using fume cupboards to have an instrument used to measure the air
velocity so that periodic checks may be performed to ensure that the hood is
operating up to its design capacity.

I/C1/3/12
 If there is more than one fume cupboard in the laboratory the capacity of the
ventilation system of the laboratory should be such that incoming air volume is
sufficient for all hoods to be in full use at the same time. Each fume cupboard
should have a separate exhaust fan, as there is danger of cross-contamination from
a common ducting system.

3.4.3. Bench system

The bench system for a chemical laboratory consists of a work surface, storage
cabinets and knee-space below and shelving or storage cabinets above. The system
includes service fixtures, sinks, electrical devices and the associated piping, drain
lines and electrical conduits.

There are many choices available for the work surface. The primary reasons
for selecting one surface over another are appearance and how well the finish resists
the chemicals used without blistering, bleaching, staining or absorbing.

Epoxy top benches are recommended since they are highly resistant to the
wide variety of chemicals that are used in a Customs laboratory. Plastic laminated
countertops, which are much less expensive, are also widely used in areas where
there is less exposure to solvents, strong acids, bases and heat.

For laboratories that require greater chemical or heat-resistant countertops,

natural stone materials could be considered. Ceramic tile is sometimes used but its
disadvantage lies in the many joints. In general, ceramic tile is not recommended.

Many laboratory furnishing manufactures offer a wide variety of laboratory

furnishings of different standard sizes which allow adaptation to nearly any room size
and shape. Bench modules are either free-standing or can be wall-mounted and are
interchangeable allowing great flexibility.

Some examples of bench, cupboard and cabinet assemblies are reproduced in

Figure 8.

I/C1/3/13
 Upper cupboard Drawer units

100 100 100

525

605
700

200
1160 400 600
320
Lower cupboard
100 100 100

525
525

605
200

800 600

Fig. 8. Example of Bench, cupboard and cabinet assemblies

3.5. Ventilation and air-conditioning

The ventilation of a laboratory should be such that the whole volume of laboratory
air is changed 6 to 12 times every hour. For instance, if the floor space of a laboratory
is 60 m and the height is 2.5 m, the volume of air needed is 1800 m per hour. This
amount of air is about the equivalent of air exhausted by one good-sized fume
cupboard. The total volume of air that is required for a laboratory is dictated by the
number and size of fume cupboards. This fact should be taken into consideration when
designing the laboratory ventilation system.

The large quantities of air needed in a laboratory can best be introduced through
perforated plate air outlets or diffusers which are specially designed for large air
quantities. Air should not be introduced in the immediate vicinity of fume cupboards in
order to avoid affecting the performance of these units.

I/C1/3/14
 Perforated ceiling panels provide a better air supply than ceiling diffusers in that
system design criteria are simpler and easier to apply and the precise adjustment of
fixtures is not required. Perforated ceiling panels should be sized so that panel velocity
is less than hood-face velocity, preferably no more than two-thirds of hood-face velocity.

Natural ventilation, which may provide large quantities of air without filtering or air-
conditioning is not generally suitable for laboratories.

In a standard laboratory air-conditioning is essential. An air-conditioning system

is, of course, costly as it must be sufficiently powerful to provide a clean, filtered air
supply which passes through fume cupboard exhaust fans as well as other outlets. Air-
conditioning provides a stable temperature environment for sensitive and sophisticated
analytical instruments. Most volumetric glassware is calibrated at 20 °C and must be
recalibrated if used at significantly different temperatures.

The volume of incoming and exhausted air should be so regulated that the air
pressure inside of the laboratory is somewhat lower than air pressure outside. This
prevents odours from spreading from laboratory rooms to other parts of the facility.

Instruments such as gas chromatographs and atomic absorption

spectrophotometers as well as vacuum pumps used to evaporate solvents must be
provided with ventilation ducts or hoods to remove gases formed during operation,
otherwise toxic levels of poisonous gases may accumulate in the laboratory
atmosphere.

A simple and effective way to ventilate instruments is to install an exhaust duct on

the wall about 40 cm above the instrument table and to connect a flexible duct (10 cm in
diameter) to it just above the instrument. The flexible exhaust duct (also called an
"elephant trunk") can then be bent in such a way that the opening comes close to the
point of the instrument where gases are released.

3.6. Utilities

3.6.1. Electricity

3.6.1.1. General considerations

Many models of laboratory instrumentation available on the market today

incorporate micro-circuitry type components. While greatly enhancing the
capability, reliability and speed of the instrument, this type of hardware has also
created problems. Such instruments are becoming increasingly vulnerable to
disruption and abuse caused in great part by difficulties experienced with the
electrical system of the laboratory. This makes the reliability of a laboratory's
electrical service and distribution especially important. The electrical system in
laboratory facilities should be designed to provide adequate, flexible, uniform and
reliable power.

Periodic reconfiguration of laboratories may change overall power needs.

Consequently, designers should estimate power needs not only for short-term
projections, but also with long-term needs in mind.

Because of these short- and long-term needs, electrical distribution should

provide the laboratory with as much flexibility as possible. The most important
considerations are quantity of power, frequency and voltage levels. Generally,
I/C1/3/15
 most laboratory equipment is designed for the normal power provided by the utility
company.

Many instruments draw relatively few amperes. Since the demand does not
appear to be that high, there is a tendency for operators to attempt to connect more
than one major instrument to single circuit. This practice should be avoided
wherever multiple circuits are available in order to avoid overloading the circuits.

The outlets to which instruments are to be connected can be mounted either

on the countertop, on the wall or on a shelf. However, it will be necessary to
anticipate the actual number of outlets required at each instrument's location. The
number of outlets in a laboratory must be sufficient since this adds considerably to
the efficiency of analytical operations and to their safety.

3.6.1.2. Voltage stability

Ideally voltage should be supplied at its rated value and remain relatively
constant. Unfortunately, fluctuations occur from time to time, generated either by
the source or by local conditions within the laboratory.

Voltage fluctuations also can be created by electrical equipment located in or

near the laboratory. Elevators, air-conditioners, furnaces and hot plates are
capable of producing this effect under certain circumstances.

Many instruments are equipped with filter systems to minimize or avoid this
problem, although they may not be completely effective. If there is a reason to
believe that equipment malfunction might be caused by voltage fluctuation the
problem can be analysed by means of special instrumentation.

The use of AC power conditioners as energy supply to instruments

guarantees output voltages within +/- 5 % and noise filtering in lines as well.

Special attention should be paid to the location of computers in the laboratory.

High-voltage lines under the floor or in ceiling spaces can cause monitor screens to
flicker. Therefore, major electrical trunk lines should be kept to the perimeter of the
building.

3.6.1.3. Grounding

Normally, laboratory instruments are tied into the common ground of the
laboratory facility. However, it may be necessary, depending on specific
circumstances, to create a separate or "isolated ground". If a common ground is
utilized, the line should be inspected carefully by a qualified electrician to ensure
that all ground connections are intact.

I/C1/3/16
3.6.2. Utility gases

3.6.2.1. General considerations

The demand for high-pressure gases for instruments, e.g., hydrogen and
nitrogen, has increased dramatically in laboratories in recent years.

The primary means of supplying instruments with these gases is via cylinders.
This method of delivery has the advantage of creating an isolated source of supply
in which purity and composition of the gas can be controlled.

As safe as these cylinders are, there is always a potential for an accident.

Therefore, the storage of these cylinders in a laboratory is not recommended. An
alternate approach is to create an area adjacent to the instrumentation laboratory
as a "cylinder room".

The cylinder room must be wide enough to hold at least two cylinders of each
type of gas used in the laboratory. The cylinders should be placed side by side
instead of one behind the other, eliminating the need for unnecessarily moving a
cylinder. Each cylinder should be strapped to a wall for safety. The depth of the
room need only be enough to store the largest diameter cylinder.

Construction of a cylinder room should be based on the degree of hazard of

the specific gases used. In most cases brick construction would be suitable. The
doors should be constructed so that the entire length of the room can be exposed
at one time.

Two similar gas cylinders can be connected together to allow for the use of an
automatic low-pressure switch-over mechanism. In this way it is ensured that there
will be no interruption or reduction of gas flow. When switch-over does take place,
it should activate a flashing light in the laboratory thus alerting the operator of the
need to deliver a replacement cylinder.

Gases are normally transported from the cylinder room to the instruments
through flexible copper tubing. This tubing should be mounted directly to the wall in
a fully exposed fashion as it enters the instrument room.

3.6.2.2. Gas system

One or more gas points are needed per bench. If natural gas is available
from a utility company the gas system should be designed in accordance with the
utility company's requirements. Where no street mains are available, gas must be
provided via a liquefied petroleum "bottled" installation.

Wherever possible, gas mains and risers should run exposed rather than
concealed in shafts or hung ceilings. This prevents the possible accumulation of
gas in these closed spaces due to leakage from the gas piping system, which may
explode if it occurs in the proper concentration and is subject to an igniting spark.
Gas supply lines should be designed to supply small areas (e.g. 12 outlets) and
each area should be controlled by a well marked shut-off valve. Handles for these
valves must never be removed.

I/C1/3/17
 3.6.3. Compressed air

Compressed air is very useful in the laboratory. If obtained from a compressor

2
machine, the optimum pressure should be between 5 and 6 kg/cm , and the air
should be purified by filtering and drying before being used in laboratory instruments.

3.6.4. Water

Benches must be provided with several cold-water taps to allow for rinsing,
condensers, etc. Hot-water taps can be restricted to those sinks where apparatus
are washed.

Electric wires, water, sewer and gas piping require space and easy access for
repair reasons. Because of this it is advisable for them to be mounted under the 20 -
40 cm wide separate centre-bench section between free-standing laboratory benches
or, where benches are placed against a wall, between the wall and the bench
(Figure 9).

60 75 60
Blocking to fasten cabinets

Access Base
Wall unit space unit
75

Analytical centre bench

Electricity
60
Fixture
Electricity

Fixture
60 3

Piping 90 Piping
20 Base unit

Base unit

Wall bench

Fig. 2. Traditional casework system - wall supported. (Measures in centimetre)

3.7. Anti-pollution guidelines

Guidelines for waste disposal vary from country to country. Many countries do not
allow any hazardous wastes to be disposed of through the sewer system. In these
cases, chemical wastes and hazardous samples which have been analysed should be
labelled with the proper safety labels (i.e. numbered, recorded and safely stored in an
explosion-proof, well-ventilated, locked, exterior building) prior to disposal by a qualified
company.

Design of an in-house waste disposal system depends on the types and quantities
of laboratory waste water. Waste treatment concepts can range from simple dilution to
full-scale on-site treatment facilities. Wastes may also be regulated by state or local
authorities. Review of this matter with those authorities at an early stage in the design
of the laboratory is advisable.

The following principals should be considered when designing process waste and
vent systems :
I/C1/3/18
(a) Waste and vent systems should be separate piping systems from storm water and
sanitary waste drainage systems.

(b) Wastes from all fixtures and equipment where acids have been used should be
neutralized before discharge into the sanitary drainage system.

(c) The system should be sized to anticipate future expansion and also provide for
flexibility of the laboratory areas.

(d) Central acid-neutralizing sumps should be provided for areas with numerous sinks
and located in an accessible place for easy maintenance.

(e) All waste piping connecting laboratory sinks and cup drains (where acids might be
used) to acid-neutralizing sumps and all vent piping for these fixtures should be of
acid-resistant materials.

Neutralization is accomplished by chemical reaction or dilution. Wastes are

normally discharged to sumps filled with limestone or marble chips or, for large
laboratories, to a treatment tank using an injected sodium hydroxide (NaOH) solution to
raise the pH and sulphuric acid (H2SO4) to lower the pH (Figures 10 and 11).

CAUSTIC
STORAGE CONTROL
TANK PANEL

EFFLUENT
pH 7 +/- 0.5
PREFAB
MANHOLE/
INTERCEPTER

LIMESTONE NEUTRALIZING FINAL NEUTRALIZING

SUMP SUMP

Fig. 10. Laboratory neutralization sump

I/C1/3/19
 TO INCINERATOR
VENT
(OPTION)

O.2 MICRON
FILTER

GRAVITY OR BACKFLOW PREVENTOR

PUMPED COLD WATER
WASTE (FOR COOL DOWN CYCLE)

AGITATOR

TANK
OR
PIT
STEAM CONDENSATER

DISCHARGE

Fig. 11. Waste treatment tank schematic

In waste piping connecting laboratory sinks to neutralizing sumps high density

polyethylene or polypropylene materials can be used, since these show good resistance
to most organic and inorganic chemicals. Pipes and fittings should have screwed joints.

The method of sizing the laboratory waste and vent piping is the same as that
used for sanitary waste and vent systems.

Acid-neutralizing sumps are usually constructed of chemical stoneware, acid-

proof, tile-lined steel tanks or high-density polyethylene. The sizing of tanks is usually
based on the number of sinks and cup drains used during peak periods.

Acid-neutralizing sumps should be sized on the following basis :

Diameter x Height Users or sinks *

30 cm 30 cm 1
45 cm 30 cm 2
45 cm 60 cm 3-6
60 cm 90 cm 7 - 20
75 cm 142 cm 21 - 50
90 cm 175 cm 51 - 100

* Users : the number of people likely to use the sinks and/or cup drains during a peak-
hour period.

I/C1/3/20
 Given the high cost of such facilities, it may be more practical in small laboratories
to store waste water separately according to its content and to send it to specialists for
treatment or to treat it in-house from time to time. Waste water containing the following
substances should not be drained :

- Cyanates and cyanate complexes

- Chromium (IV) ions
- Mercury and its compounds
- Other heavy metal elements.

Dilute water solutions containing organic solvents which are easily decomposed
by micro-organisms can be drained. Halogenated solvents or solvents containing
halogen compounds should be stored and sent to specialists for treatment. Burning out
of these substances is not recommended since toxic substances, e.g., dioxin, would be
produced. It is possible to burn out other organic solvent wastes.

I/C1/3/21
4. Administration

4.1. Budget

The budgetary system should be flexible. Contingency funds are important for the
running of a laboratory. Budgets should be arranged so that funds are readily available
for urgent supplies and repairs and the other day-to-day needs of the laboratory.

The Laboratory Head must have adequate control of the budget and operate it
under clearly defined rules. These should be sufficiently flexible.

Budgets are typically planned for one year, but major equipment purchases should
be planned for a three-to-five year period.

4.2. Purchasing

In case of a new laboratory the selection and specification of laboratory equipment

together with the planning of space requirements (including flexibility for future
expansion) should always precede, or at least go hand in hand with building design.
Before selecting any equipment, a careful study should be made to determine :

(a) Which of the many possible suppliers and manufacturers of equipment are capable
of providing installation and maintenance services.

(b) What experience potential suppliers have in dealing with the special conditions
existing in less industrialized countries.

Equipment specifications must be prepared very carefully and clearly in order to

avoid purchasing of incomplete or unsuitable apparatus. Information is needed, for
instance, with regard to essential accessories not included with the basic instrument and
optional accessories (with explanations for their particular application), essential
operating supplies and recommended spare parts. Precise specifications are essential
in obtaining reliable and comparable offers. For example, instruments equipped with a
library data system (e.g., infra-red spectra, mass spectra, etc.) are recommended, since
the library search system has recently been developed to identify unknown contents in
samples.

Among the demands imposed on equipment suppliers, it is very important to

include the standards certificate issued by international organizations, and to start to
request standard written procedures and preventive maintenance, as well as manuals in
the user’s language.

Large laboratory supply companies offer a more comprehensive range of

supplies, including a full range of instruments and auxiliary equipment, than is offered by
individual manufacturers. Service facilities for the installation and maintenance of
equipment can also be co-ordinated and provided much more easily by a large
organization.

Complex apparatus requires special training for the operators. Engineers

performing the installation usually provide some basic training. However, a more far-
reaching programme of training may be necessary. In such cases, special training
programmes should be arranged in advance of the purchase, preferably before the

I/C1/4/1
 equipment is delivered. The exact training requested should be specified in the contract
to purchase the equipment.

Normally, the service representative will provide basic operator training while the
instrument is being installed. A more specialized follow-up training is usually provided
by the vender 6 to 12 months after installation.

4.3. Supplies management

Supplies routinely used by a laboratory include solvents, reagents, chemicals,

glassware and other analytical materials. These supplies must be regularly replaced as
used. Particular attention should be paid to supplies that are consumed and are very
important to the daily operation of the laboratory.

There should be an accurate accounting system to record receipt, use and future
need of supplies in order to be aware of the stock situation and the need to purchase
replacements. Replacement orders should be made and the replacements received
before the total depletion of items occurs. Some supplies may take months to obtain.
The procurement process must take this time into consideration.

Stock records can be maintained in a variety of ways but a card system is perhaps
the most versatile. The Supplies Record Card should contain such data as :

- Name of product
- Date purchased
- Where purchased
- Amount
- Expiration date (if any)
- Special storage requirements (if any)
- Amount dispensed
- Minimum reorder quantity (when the material reaches this level, it should be
reordered as soon as possible).

Proper supplies management prevents the occurrence of the situation where

analyses have to be stopped because a critical material is suddenly used up.

4.4. Equipment maintenance

It is important that all items of equipment be properly and promptly maintained and
repaired when needed. The degree of sophistication of equipment varies from a
straightforward pH meter to a complex instrument such as a spectrophotometer.

It may be difficult and expensive in developing countries to repair any instrument,

sophisticated or otherwise. Therefore the routine maintenance of instruments is
important since this should delay the day when outright repairs are necessary.

Under these circumstances it is recommended that laboratory analysts or

technicians be given training in repair and maintenance techniques. Training can best
be provided by instrument suppliers.

If adequate service is not readily available locally, serious consideration should be

given to the purchase of a service contract. The usual service contract involves
checking the instruments at specified intervals and performing necessary maintenance.
Service contracts are expensive and should be considered when the expense can be

I/C1/4/2
 justified. Services of expert from the suppliers could also be made up of. A basic in-
house maintenance capability should be developed if possible.

Recording the history of an instrument's maintenance and repair is important. It

provides a summary of the instrument's operation over a given period and provides a
justification for the replacement of old and worn out instruments with new ones when an
instrument costs more to maintain than it is worth.

4.5. Training

The following staff training may be required :

(a) Training on the Harmonized System. Chemists must have knowledge of the
Harmonized System in order to determine, carry out or direct the necessary
analyses.

(b) Training on certain basic techniques (e.g., titrimetry, gravimetry, TLC, IR, GC)
especially for assistant analysts.

(c) Training on analytical methods for specific products (e.g., petroleum products,
foodstuffs, organic chemicals, textiles, metals).

(d) Training on safety and emergency measures.

(e) Training in the use of computers.

(f) Training on sampling procedures for field Customs officers

(g) Languages

(h) Automatic data processing

(i) Customs legislation

(j) Quality assurance

(k) Statistics.

4.6 Information systems

It is recommended to acquire an "information system" with an adequate database

designed to store and integrate the technical data of analysed samples and other data
generated in other areas within the analytical process, and to allow users from the
administrative, support and analytical staff to consult and recover information in
accordance with their specific needs.

Final reports of analyses performed can be keyed directly into the system,
allowing information recovery by multiple means : name and synonyms, physical-
chemical data, properties, HS classification, uses of the product and data from samples
analysed in the past.

Administrative and support staff can obtain the necessary information to prepare
statistical reports on the work performed and to control and supervise operations and
the laboratory.

I/C1/4/3
I/C1/4/4
5. Safety and anti-pollution measures

5.1. The safety programme

The common responsibility requires that the best possible working conditions and
safest possible environment is provided in which to carry out analytical procedures.

The Head of the laboratory and supervisors have overall responsibility to ensure
safe working conditions in the laboratory, including the responsibility :

(a) To ensure that workers know and follow chemical hygiene rules.

(b) To ensure that protective equipment is available, in working order and used
according to established guidelines.

(c) To provide appropriate training.

(d) To know the current legal requirements concerning substances.

(e) To determine the required levels of protective apparel and equipment.

(f) To establish a general security plan for all staff in the Customs laboratory (e.g.,
scheduling of fire safety drills, scheduling of medical examinations, etc.).

(g) To introduce certain techniques for identifying risk (e.g., use of radiological
exposure monitoring badges, pest control, etc.).

One senior analyst should be appointed the "Safety Officer" and given the
responsibility to monitor safety procedures, practices and equipment on a routine basis.
In a large laboratory, the Safety Officer may be assisted by a committee of two or three
analysts.

The duties of the Safety Officer (and committee where appropriate) should be
detailed in the laboratory Safety Programme. This programme should indicate safety
requirements, hazards, equipment and emergency procedures. Items which should be
included in a laboratory Safety Programme are discussed in the following paragraphs.

5.2. Basic safety rules

Each laboratory should develop its own set of General Safety Rules, and make
sure that all members of staff are aware of them by supplying personal copies of the
rules and by posting copies on notice-boards. The rules should be changed and
developed in the light of experience. Some that should be included are :

(a) Become familiar with the location and use of emergency equipment (e.g., fire
extinguishers, eyewash fountains, safety showers, first aid cabinets). Know where
to go in case of fire.

(b) Before beginning a sample analysis, review possible hazards connected with the
assignment and take necessary precautions to eliminate or counteract the hazards.

I/C1/5/1
 (c) Use, as appropriate, the safety equipment provided for protection (e.g., safety
goggles to protect eyes, face shields, various types of gloves). Wear a laboratory
coat routinely since its purpose is to serve as protective clothing.

(d) Bring all accidents and hazardous conditions to the attention of the supervisor
immediately.

(e) Be extremely careful of loose clothing, neckties, scarves, dangling jewelry (such as
necklaces) and long hair when using revolving or reciprocating equipment. Keep
such items bound or confined so that they will not be entangled in the equipment.

(f) Turn off laboratory services (gas, water, etc.) at the service cock when not in use.
Changes in pressure may suddenly dislodge tubing connected to an apparatus and
lead to an accident or possible injury.

(g) Always use mechanical aids, such as safety bulbs or pipette fillers, when pipetting
hazardous material. Never use the mouth.

(h) Use fume cupboards for any analytical operations involving significant amounts of
solvents, or when noxious fumes will be generated.

(ij) Keep the work area neat and tidy, with all containers labelled with their contents.

(k) Any chemicals, whether toxic or not, which come in contact with the skin must be
washed off immediately and completely.

(l) Keep fire escape routes and doors clear at all times. Do not block, even
temporarily.

(m) No one should work alone in the laboratory, so that assistance is available in the
event of an accident.

(n) The last person to leave the laboratory at the end of the working day must check
that all equipment which should be turned off has been (this does not release each
individual operator from his or her duty to turn off equipment no longer in use).

(o) Do not smoke in any of the laboratory areas.

(p) Do not eat or drink in any areas of the laboratories other than those designated for
this purpose.

(q) Use biological safety cabinets for products that pose a biological hazard.

(r) Ensure that personnel exposed to radiation wear radiological exposure monitoring
badges.

5.3. Fire safety

5.3.1. General considerations

A laboratory must be regarded as one of the more likely places in which a fire
will occur. Therefore, a laboratory facility should be designed so that the building and
its contents will be protected from fire and so that any fire that occurs can be
extinguished, with no injury to personnel and with minimum loss to building and
contents.
I/C1/5/2
 It is also prudent to have the local chief fire officer visit the building, be
familiarized with the problems and advise the laboratory staff about local fire
regulations and further safety measures that should be taken.

Fire and smoke detectors should be installed in the building and connected so
that in the event of fire, an alarm is given at a fire station.

Staff must have clear instructions of the action to be taken in case of fire. Such
instructions should be posted prominently in various parts of the building.
Occasionally, there should be a fire drill to check that everyone knows what to do in
case of a serious fire and to make sure that the building can be evacuated in an
orderly and rapid manner. Fire evacuation must include switching off the electricity
supply to the affected area, since short-circuits may result in a further fire hazard.

When new staff is introduced, they should be trained in safety procedures, be

shown where fire extinguishers, blankets, hoses and buckets are kept and how the
sprinkler system works, if there is one.

5.3.2. Fire extinguishers

Laboratory facilities should be provided with portable fire extinguishers that can
be used by laboratory employees to put out small fires effectively. Fire extinguishers
must provide adequate fire extinguishing capacity for litre bottles of flammable
solvents (liquids).

Multi-purpose extinguishers are often recommended for areas where fires may
involve different classes of materials. However, pressurized dry chemical
extinguishers which are suitable for general use, should not be used around
computers or other sensitive electronic equipment. It is nearly impossible to clean
the dry chemical out of such instruments and the instruments could be irreparably
damaged.

Many hand-held carbon dioxide fire extinguishers on the market have the
required capacity and are often preferred because they are suitable for small solvent
fires and leave no residue.

Fire extinguishers should be located near the doors of laboratory work areas,
either just inside or just outside. This location is preferred because a person who
seeks the extinguisher in case of fire will be heading toward the exit.

It is recommended that all laboratory buildings be provided with standpipes and

4 cm hose, for use by occupants to supplement fire extinguishers, and that the hoses
be equipped with special nozzles.

5.3.3. Spill kits and respiratory protection

If spill control material is to be provided, it should be of a type and in a quantity

adequate to provide safe control of potential spills. Storage of spill control material
should be located in a corridor or other area away from those in which spills are likely
to occur so that a spill does not prevent access to emergency equipment.
Respirators with the proper filters should be used when dealing with toxic
fumes from analyses or spills. They should be available at one central point (i.e. spill
cart) in the laboratory.

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 Electrical equipment may be the source of a fire due to faulty wiring,
inadequate grounding, failure causing sparks or local overheating or switch gear
sparks. All electrical equipment should carry a fuse which blows at an amperage
slightly in excess of that required by the equipment. It is commonplace to find that
equipment drawing only one or two amps have a 13 or 15 amp fuse which is unlikely
to be of any use if anything goes wrong.

Flammable vapour near electrical equipment represents a fire hazard unless

the instrument has been rendered "explosion proof" by sealing those sections where
a spark could occur. Motors must be serviced regularly. Lack of attention may result
in overheating and subsequent fire. Centrifuging of volatile flammable solvents is
hazardous if the centrifuge motor is not explosion proof, especially if the tube breaks.

5.4. Emergency water

Readily available supplies of water are needed for emergency flushing of

chemicals from the eyes and body in every work place in which irritating, corrosive or
toxic chemicals are used. Emergency showers and eyewash stations should be
standard features in every laboratory.

Time is of the essence in emergencies. The location of and distance to an

emergency shower are important and there should be no door in the path of travel
between the spill area and the shower. The first few seconds are most critical to
preserve life and avoid major injury. The distance should therefore be no greater than
30 metres from any location in the laboratory to the nearest shower. That is the
maximum distance. Shorter distances are advisable.

Eyewash stations are used to rinse the eyes and face in case of chemical spill.
Close proximity is essential since an individual must be able to find the eyewash blinded
and unaided within seconds of the spill. Locating such devices at a sink in the work
area will take less floor area, provide an economical and convenient water supply and
drainage and is easy to find in an emergency. Never hook up the eyewash to a hot
water supply. If possible, provide water within the temperature range of 10 to 20 C.

5.5. Chemical hazards

Many chemicals are hazardous and should be handled carefully. Hazardous

chemicals can be flammable, explosive, toxic, corrosive or poisonous and can be
identified with the help of technical literature and manufacturers leaflets. It is desirable
to check on the nature of chemicals and to take adequate precautions before handling
chemicals in order to avoid accidents. The suppliers of chemicals should be asked for
Material Safety Data Sheets (MSDS) every time (new) chemicals are ordered. Any
laboratory should, of course, have the necessary first aid facilities.

Chemicals can be harmful (1) when coming into contact with the skin or eyes, (2)
when inhaled or (3) when swallowed.

Contact of corrosive chemicals with the skin or eyes can cause irritation,
discoloration of the skin and even burns. Serious effects can be avoided in most cases
by rinsing immediately with running water. Treatment with dilute solutions of
neutralizing chemicals is sometimes effective (e.g., the use of a diluted ammonia
solution in the case of acid burns).

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 Contact of hazardous chemicals with the eyes is, of course, extremely dangerous
and it is, therefore, highly advisable to wear goggles or spectacles while doing analytical
work.

The inhalation of toxic or poisonous chemicals can result in the quick absorption
of chemicals into the body. For example, hydrogen cyanide gas is immediately
absorbed into the blood and is extremely toxic. Highly concentrated gases may lead to
asphyxiation. Breathing deeply, coughing and artificial respiration can be effective
countermeasures in some cases.

Swallowing of chemicals is usually the most dangerous of accidents. Toxic

chemicals such as acids, alkalis and heavy metal ions directly dissolve or coagulate
stomach proteins and are absorbed by the body. The most effective treatment is to
make the victim vomit as soon as possible. Treatment with neutralizing chemicals is
sometimes effective. For example, if acid is swallowed, sodium bicarbonate solution
should be administered. In the case of heavy metal ions, the victim should be made to
vomit.

It should also be noted that there are chemicals which are suspected or known
carcinogens. These chemicals must always be handled with extreme care, using all
available protective gear.

To the extent possible, hazardous chemicals should be stored away from the
laboratory and away from other chemicals with which they violently react.

All reagent bottles, flasks or other containers must be properly labelled, even if the
contents are considered harmless. Warning stickers can be used in addition to the
container label to highlight hazards.

Before sending containers (beakers, etc.) containing hazardous material to be

washed, they must be rinsed or otherwise treated by the analyst to remove the hazard.
The analyst is the only one who knows of the hazard and how to eliminate it.

When emptying acids and cleaning solutions into drains, the sink should first be
filled with water before pouring the acid or cleaning solution into the sink; only after this
should the water be drained. The tap should be allowed to remain on full for a few
additional minutes. Dilution should always be sufficient to reduce the acid concentration
to a pH of between 5 and 7.

5.6. Physical hazards

There are many physical hazards in a laboratory. Most are avoidable by the use
of common sense. It is advisable, however, to prepare some instructions for new
employees and periodically to remind others. The following are some suggested
instructions for glassware handling :
(a) Do not use broken or chipped glassware or return it to storage. Always use gloves
in handling broken glass.

(b) Remove sharp or jagged edges from glassware before using it. Fire polish the
edges on all glass tubing.

(c) Broken glass in sinks presents a definite hazard since glass may not be visible in
the presence of water. When broken in the sink, remove it promptly. Furthermore,
consider the possibility of the presence of broken glass when reaching into the sink
for any purpose.
I/C1/5/5
 (d) In handling beakers, support them by grasping the sides, never the top. Support
large beakers (one litre or more) from the bottom when in use.

(e) When heating liquids in glass by means of a gas flame, protect the glass from
direct contact with the flame by use of wire gauze or centred wire gauze.

(f) When placing liquids in bottles which have a positive closure, reserve more than
5 % of the volume as air space to allow for expansion due to temperature changes.

In vacuum operations, glassware under vacuum should be protected from physical

shock which might cause cracks and result in collapse with explosive violence. Flat-
bottom flashes should not be subjected to vacuum unless constructed with heavy walls
specifically for such service. Vacuum should be relieved before attempting to
disassemble equipment.

5.7. Safety and emergency equipment

5.7.1. General considerations

"Safety" equipment is that designed to protect and/or prevent injury and is used
before an accident happens. "Emergency" equipment is used after an accident (or
other emergency) to minimize the injury or damage. Therefore, eye goggles are
"safety" and eyewash fountains are "emergency" equipment.

Using these definitions, the following are lists of safety and emergency
equipment.

(Safety equipment)

- Rubber aprons
- Eye goggles
- Face shields
- Disposable plastic gloves
- Bench shields (portable, clear plastic)
- Pipetting bulbs
- Heavy rubber carriers for acid and alkali bottles
- Metal safety cans for flammable solvents
- Metal solvent storage cabinets (about 160 litres capacity) (for storage of solvents
used daily in the laboratory)
- Respirator filter masks (for dust or fumes).

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 (Emergency equipment)

- Hand-held fire extinguishers

- Fire blankets (wall mounted)
- Eyewash stations (built-in fountains or portable kits)
- Spillage absorbent kits for both acids and solvents (available commercially or can
be assembled locally)
- Emergency showers
- Respirator masks with oxygen supply
- First aid cabinets.

All such equipment is useless if not available or not in serviceable condition.

The Safety Officer should periodically check both the storage locations (if not in use)
and the condition of all safety and emergency equipment. The laboratory staff
should be trained in the use of the equipment and use must be enforced when
necessary.

5.7.2. Emergency showers and eyewash stations

Some of the most important emergency facilities in a laboratory are eyewash

stations, emergency showers, sprinklers and emergency exits.

Eyewash stations should be located near analytical work stations. It is, in fact,
desirable to locate eyewash stations next to each sink and by the emergency
showers, for easy and quick access.

Emergency showers should be located within a few seconds walk of the

analytical work stations. The distance should be no greater than 30 metres from any
location in the laboratory to the nearest shower.

In order to be effective, emergency showers (see Figure 1) need to release a

large volume of water at low velocity (120 - 180 litres per minute). Because of the
large volume of water, many installations have floor drains below the shower,
although this is by no means standard practice. Floor drains are expensive and dry
out because of infrequent use, allowing sewer gases to enter the laboratory.

Emergency shower valves should be installed so that they can be actuated by a

person of any height. One very effective way is to run a cord down a clear wall so
that it can be found easily and pulled.

Sprinkler systems are desirable and often required by law or regulation. They
must be located carefully since some chemicals react violently to water or create
inflammable gases when mixed with water. Sprinkler systems should be adjusted
carefully in order to function correctly.

The minimum flow rate for plumbed eyewash equipment should be at least
12 litres per minute and, preferably, 24 to 36 litres per minute.

Cold water (about 10 °C) is recommended for emergency flushing of chemicals

from eyes and body, as well as for emergency treatment of thermal burns. Cold
water is generally best because it will slow the reaction rate of the chemical splashed,
constrict blood vessels and minimize circulation of absorbed chemicals (hot water
can increase the injury).

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 Brightly coloured wall and sign

Corrosion-resistant valve
Potable water
30 gal/min
20 cm
(113.6 L)

50.8 cm spray 243 cm max.

208.3 cm min.
152.4 cm
175.3 cm max.

58.4 cm max.
137.2 cm max.
(handicap)

40.6 cm min. max. to electric

devices
Obstruction

30.5 cm

to any point in laboratory

Fig. 1. Emergency shower - critical dimensions

Finally, two emergency exits should be located at the opposite ends of rooms
for chemical analysis. They should be installed to allow the doors to push open in
order to permit easy escape.

5.8. Training on safety and emergency measures

The Safety Officer should conduct emergency drills at least twice a year.
Demonstrations of safety and emergency equipment should be included in such
training. All safety and emergency equipment should be checked and, if inoperable,
should be repaired or replaced as soon as possible.

New employees should be briefed by the Safety Officer on the location and use of
safety and emergency equipment, the location of hazardous chemicals, ways to avoid or
minimize accidents, escape routes and how to notify fire authorities.

5.9. Anti-pollution measures

Every employee in a laboratory should understand the importance of anti-pollution

measures. Analysts should be familiar with the drainage equipment in the laboratory, its
functions and efficiency. (See also Section 3.7 of this Guide on anti-pollution
guidelines). Before used chemical compounds are drained, they should be neutralized,
precipitated or separated, thus creating non-hazardous compounds of a consistency
which may be drained. For example, cyanates and cyanate compounds should be
burned or decomposed by the use of oxidising agents, such as chlorine or ozone before
introduction into the drainage system.

I/C1/5/8
 Certain hazardous chemical wastes require special disposal by professionals. For
example, heavy metal compounds, etc. should be stored separately and their disposal
should be entrusted to qualified companies.

For the purposes of pollution control the analytical staff should co-operate closely
with the building support staff, professional disposal companies and the sewer
authorities.

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6. Sampling

6.1. General considerations

In this section the normal sampling and sample preparation methods for analysis
are described. If standard sampling procedures are laid down in ISO 2859 1-3, etc.
(see III, Chapter 1 : International Standards and Methods), the sample collector should
prepare the sample according to those procedures.

During sample collection, care must be taken not to damage the goods. It is
recommended that the owner of the goods, or his or her representative, should be
present when sampling is performed to the extend necessary.

Chemical analysis leads to successful practical results only when the sample for
examination has a composition that is representative of that for the entire shipment.

The amount of the sample to be taken for analysis is usually predetermined. The
sample collector must collect at least the minimum amount of goods necessary for
laboratory purposes. In the case of an airtight container containing packages for retail
sale, the smallest packing unit may generally be regarded as a suitable sample for
analysis.

Since the sample being analysed must be representative of the shipment, the
method of obtaining it is important. Most non-liquid materials, and sometimes liquid
ones, may be far from homogeneous and careful work is necessary to obtain a useful
sample from a very large shipment. The procedures vary somewhat with the nature,
size and homogeneity of the original material and it would be difficult to provide set rules
for general applicability. In cases where the shipment being sampled is large, small
portions of the sample should be drawn systematically throughout the shipment with a
view to combining them into one easily handled sample having the same average
composition as the entire shipment. If the sample collector cannot mix the sample
portions technically or cannot identify whether or not they are homogeneous, he or she
should send each sample portion separately.

Liquid samples stored in a can or a drum should be drawn out after shaking,
mixing or stirring sufficiently because they are not always homogeneous. Powder,
particles or muddy samples which are packaged in a container should be gathered from
the portion which is not in direct contact with the air. These samples should generally
be taken from more than two separate containers. However, this rule need not apply to
uniform commodities such as canned or bottled products.

Samples such as petroleum compounds or molasses which are stored in a tank or

cistern should be taken from each of three layers (top, centre and bottom), after the
tank or cistern is filled and the contents are allowed to stabilize.

To prevent or minimize contamination, decomposition, or matrix change, care

should be taken with the sampling methods, sampling apparatus and sampling
containers (e.g., containers made of polyethylene or polypropylene with double caps
(one being a screw cap) to avoid loss and contamination of the content) being used.
For samples which are sensitive to the atmosphere (moisture, carbon dioxide, etc.),
rapid sampling is required. Clean and dry sampling apparatus and containers should be
employed every time. In particular, dark containers should be used for samples which
are sensitive to sunlight.

I/C1/6/1
 Once the sample has been collected, stringent precautionary measures should be
taken to prevent the samples being exchanged or tampered with. Such measures may
include sealing the sampling container or packaging with an official seal. Each sample
should also be labelled immediately to indicate the name, number, sampling date,
location, etc., in order to avoid any confusion.

Labels must be attached to samples in such a way that they cannot be torn off or
damaged when the seals are broken to open the sample. The identification label must
remain intact throughout the analysis.

Samples that are flammable, explosive, toxic, corrosive or poisonous should be

handled carefully and a special marking such as "Dangerous" or "Hazardous" should
appear on the sampling containers.

In the case of perishable goods, the containers should be prominently marked as

"perishable" and the samples should rapidly be dispatched to the Customs laboratory.

Samples should be securely packed and sent to the laboratory as soon as

possible with the accompanying sampling certificate which should give all necessary
details concerning the sample, such as :

(1) Name, number, quantity (total net weight or unit size) and quality of sample

(2) Port of loading and unloading

(3) Date of arrival and sampling

(4) Name of the sample collector and client

(5) Number and date of declaration

(6) Name, address and telephone number of importer or agent, consignee and
shipper

(7) Country of origin

(8) Use and price (f.o.b., c & f or c.i.f.)

(9) Sampling method

(10) Purpose and items of analysis

(11) Tariff number of declaration.

(12) Available technical information about the sample (e.g., technical literature, safety
data sheet, catalogue, CAS number, composition, chemical structure, typical
analysis results or specifications), etc.

I/C1/6/2
 Samples for analysis may be taken at many Customs stations. Therefore it is
important for chemists to inform the officers concerned on how best to take a
representative sample and on the necessary safety and security precautions related to
the handling and storing of samples.

6.2. Dispatch of the sample to the laboratory

The sample should be dispatched with great care to ensure that it arrives at the
laboratory in the same condition as when taken. The containers to be used and the
manner in which the dispatch is to be handled depend very much on local conditions.

6.3. Sample receipt

When a sample is received in the laboratory, the laboratory staff should first
identify the nature of the sample from the accompanying sampling certificate in order to
store the sample properly. All samples (with accompanying documents) must be
registered, marked and stored properly as soon as they arrive at the laboratory. The
system shall ensure that the necessary information to identify the sample (including its
origin) is recorded. It shall also ensure that there can be no confusion of samples (or
related documents) during the analytical operations.

A sufficient level of security must be maintained, so that unauthorized persons

cannot get access to the samples or the result.

Perishable goods should be stored in refrigerators or freezers to avoid

deterioration before analysis.

The Customs laboratory should have a system for tracking the sample through its
initial storage, its analysis and its subsequent disposal. This is usually done by means
of a record-keeping system based on a unique number assigned to the sample at the
time of sampling or on arrival in the laboratory. This number may be sequential, e.g.,
0001 to 9999.

The record must show each movement of the sample, e.g., its receipt, its
assignment to a laboratory analyst for analysis, its subsequent storage and its eventual
disposal.

One of the administrative staff should be given this record-keeping function and
be closely supervised by a senior administrator.

The use of a card record system rather than a book is recommended since cards
are more flexible and may be organized in groups under different headings. Certain
items of information should be included on each card :

(1) Sample number.

(2) Product name.

(3) Date sampled.

(4) Date received at the laboratory (the "date received" would normally be the date
that the request is received; however, if the request and sample are received
separately, the date received should be the latter of the two since that represents
the earliest date that the laboratory could begin work on the request).

I/C1/6/3
 (5) Method of storage (dry, refrigeration, freezing, dark room, etc.).

(6) Storage location (coded for easy reference).

(7) Date assigned for analysis.

(8) To whom assigned (the analyst should initial to show receipt).

(9) Date returned (from analyst).

(10) Final disposition or disposal of the sample, including the method and date.

The above sample record is to record only physical movement and location, not
the analytical results. The reason is that the analytical worksheet and the sample
record are usually in two different locations.

The sample record card should be in duplicate. One copy goes to the sample co-
ordinator who holds on to the sample until the analyst is ready to perform the analysis,
and another copy to the laboratory supervisor who assigns the sample. This sample
assignment could be done manually, by writing on the copy of the sample card the initial
of the assigned analyst and date, or through computer. It is then given to the analyst.
When the analyst is ready to analyse the sample, he or she retrieves the sample from
the sample co-ordinator who fills out the original copy of the sample card with the
relevant information, such as the name of analyst, date of assignment, date sample was
given to the analyst, etc. After analysis and preparation of the laboratory report, the
analyst returns the card with the remaining sample to the sample co-ordinator. The co-
ordinator fills out the original copy of the sample card with information such as the date
the sample returned, final disposition or method of disposal and date. This card should
then be filed separately from the laboratory worksheet and the laboratory report.

Sample record cards should be prepared and kept in the custody of one person
until the case is brought to a close and the sample is destroyed. This function is critical
to the operation of the laboratory and therefore the person employed in this post must
be reliable. However, this task should not usually occupy a person full-time and
therefore could be combined with other duties in the laboratory, such as store-keeping
of laboratory chemicals, glassware and other equipment, etc.

6.4. Sample storage and disposal

Sample storage, both initial and reserve, is critical to a sample analysis. Improper
storage can completely invalidate any analytical results. Ideally, the sample should be
stored in such a manner as to prevent any change in the attributes being examined,
from the time of sampling, through analysis, and into reserve storage.

The usual storage areas are dry (room temperature storage), refrigerated or
frozen. In order to minimize exposure to changes during storage it is important to use
proper sampling containers for the samples.

I/C1/6/4
 Samples are normally kept for a period of time after analysis in case further
information or analysis is requested or the results of the laboratory's work are disputed.
For this purpose, the remaining samples should be returned to the sample co-ordinator
after analysis. Samples should be kept at least as long as the time allowed for an
appeal from the importer or exporter. Samples for which analysis is susceptible to
dispute should be stored in a separate area to reduce the chance of their being
inadvertently destroyed.

Sample disposal is, or can be, a relatively simple matter. Problems only arise
when there is a hazard involved in destruction or when the sample itself presents a
hazard to the disposer. The analyst should know of any hazards involved and should
inform the person in charge of the sample storage of any special disposal requirements.

6.5. Analysis assignment

In a large laboratory, the assignment of a request for analysis might be a

two-stage process, i.e., initial assignment to a Section Head who then assigns the work
to a chemist within the Section. In a smaller laboratory the assignment of work might be
assigned directly to a chemist.

(Note : The sample should be retained in a "sample room" until the chemist is ready to
begin work on the sample since it is strongly recommended that chemical and other
potentially hazardous samples should not be handled in the general office environment).

The chemist who performs the analytical work must identify and define analytical
problems and establish results in accordance with the methods to be used. Generally, it
is preferable to use a method that has been subjected to collaborative study. If the
analyst has difficulty with such a method, it is likely to be due to a deficiency in training
or in facilities, rather than the method itself. If a method has been in use and found to
give reliable results it should not be changed to another until the new method has been
shown to be of equal or better reliability in that particular laboratory.

It should not, however, be forgotten that a reliable method is only a precondition to

obtaining the right answer. The ability of the analyst to apply the method properly is
equally important.

I/C1/6/5
7. Operation

7.1. Safety rules

It is essential for Customs laboratory staff to analyse the requested sample safely
and to furnish accurate and reproducible results after the examination.

All staff at Customs laboratories should observe the safety rules laid down in
"Safety and Anti-pollution Measures" (see Section 5). Analytical staff should wear a
laboratory apron or coat, laboratory shoes and protective eyeglasses; they should know
the location and proper use of safety equipment such as fire extinguishers, fire blankets,
safety fountains or showers, and equipment for handling spills. It is also recommended
that the laboratory be kept clean and that all chemical reagents, apparatus and samples
be put away when staff are finished with them. If they get into difficulties, analysis staff
should report to their supervisor or colleagues immediately.

7.2. Basic rules to be followed in the laboratory

Each experiment should be understood thoroughly in advance, and appropriate

experiment programmes and time-tables should be prepared by each analyst.

It is essential to use the minimum amount of reagents and samples necessary for
each experiment. To avoid contamination of the stock bottles, appropriate amounts of
reagents, chemicals or solutions should first be taken to each test-tube or beaker from
the stock bottle, and these materials should be used for each experiment. When the
experiment is over, dispose of reagents, chemicals, etc., properly. Never return them to
the stock bottles.

Walk slowly and be careful when handling any apparatus in the laboratory. Do not
heat any apparatus for quantitative analysis and any glassware at the point where two
thicknesses of glass meet. Wash your hands before and after every experiment and
check the labels or markings at least twice before taking anything from a bottle or
container.

It is, of course, essential to keep all rooms clean and to put away apparatus,
sample containers and tools after each experiment. Before locking up, someone must
check that, in all the rooms, the gas and liquid valves are closed and electrical
instruments switched off.

7.3. Investigation of samples and analytical methods

With reference to the nature and quantity of the sample, it is essential to draw as
much information as possible from the accompanying certificate and relevant
documents. Past data relating to a similar sample should be used, if possible. If the
analyst wants to obtain additional information on the sample, he or she may ask the
importer or exporter. If necessary, simple screening tests are carried out in advance to
ensure a successful experiment. On the basis of all this information, the analyst can
draft an experiment programme for systematic analysis. As far as analytical methods
are concerned, validated methods should be employed.

In addition, standard test methods for samples analysed frequently should be

developed to facilitate analytical work and to ensure accuracy and precision of data.

I/C1/7/1
 7.4. Procedures for using laboratory apparatus

Since many different types of apparatus are used for analytical experiments, it is
necessary to understand the purpose, use, capacity, etc., of each of them. When an
experiment is finished, it is recommended that the apparatus be cleaned and stored
properly.

7.4.1. Procedures for using glassware apparatus

It is necessary to check all glassware to determine whether there are any

cracks or chips. If so, the glassware should be disposed of.

The analyst must wash glassware carefully with a brush in warm water and
detergent, then rinse completely with tap water and finally rinse with a minimal
amount of distilled and/or deionized water until the water spreads out evenly on the
clean glass. In the case of quantitative glassware, a brush and cleanser should not
be used. After analysing oils or fat with any apparatus, the analyst should wash the
apparatus with an organic solvent in which the sample is soluble. The analyst may
use a solution of CrO3 or K2Cr2O7 in concentrated H2SO4; however these solutions
must be handled carefully.

(Volumetric flasks)

A volumetric flask is used to dilute a certain volume or weight of sample or

solution with diluent to a certain volume.

The proper method of reading a meniscus in volumetric measurements of liquid

with quantitative glassware is with the eye on a level with the meniscus, and where
the bottom of the meniscus is used to indicate the volume of the liquid.

When handling the volumetric flask, the sample or solution should be diluted in
stages, shaking the flask to ensure thorough mixing. The diluent should be added
slowly so that the bottom of the meniscus is even with the middle of the calibration
mark at eye level.

The solution should then be thoroughly mixed, keeping the stopper securely in
place.

(Burettes)

A burette is used to determine the accurate volume of a standard volumetric

solution which is used for volumetric analysis.

When using a burette for quantitative analysis, it must first be rinsed a few
times with about 10 ml of standard volumetric solution. It should then be filled with
standard volumetric solution and the stopcock should be opened several times until
all air is removed from the tip. Finally, it should be filled to just below the zero mark
with standard volumetric solution and the volume of standard volumetric solution can
be read. An erlenmeyer flask, in which a constant volume of the test sample solution
is poured, is placed on white paper under the burette. The standard volumetric
solution may be added from the burette rapidly until it is almost at an end point; the
flow of the solution should then be reduced until individual drops fall into the flask.
Add the last few drops slowly, shaking the flask to ensure thorough mixing.

(Transfer pipettes)
I/C1/7/2
 A transfer pipette is used to transfer a constant volume of a solution.

When using a transfer pipette, it is desirable to use a safe pipette controller to

avoid any problems. The solution should be drawn up past the calibration mark. The
outside of the pipette should then be wiped with tissue paper and the solution allowed
to flow out until the bottom of the meniscus is just at the calibration ring; to pick off
the last drop adhering to the outside of the tip, touch the side of the flask with the tip.
Then withdraw the pipette from the flask and hold it over the container into which the
solution is to be transferred. Allow the pipette to drain in a vertical position, with the
tip against the side of the container. Allow 15 to 20 seconds for drainage after it
appears that most of the solution has drained out. The liquid remaining in the tip of
the pipette should not be blown out, if the pipette is calibrated for this amount to
remain.

7.4.2. Analytical balance

Weighing is necessary to measure the weight of the sample, standard

substance and reagent in any analysis. In Customs laboratory, the analyst deals with
a broad range of weights, from a few kilogrammes down to a few milligrammes or
less. The analyst uses mass rather than weight, because mass is an invariant value
worldwide. In Customs laboratories, a single-pan balance is more useful than a
double-pan balance for reasons of rapidity. More recently, electronic analytical
balances have been introduced into Customs laboratories. No weights or knife
edges are involved. The weights are automatically indicated by placing a weighing
bottle on the pan after setting the balance to zero. There are two kinds of weighing:
"rough" and "accurate". The former is normally used when it is not necessary to
measure the accurate weight, where reagents are simply added to adjust the solution
conditions. On the other hand, the accurate weight of the samples or reagents may
be necessary, particularly, in quantitative analysis. Accurate weighings are
performed on an analytical balance, usually to the nearest 0.1 mg.

Avoid vibration or jarring when determining accurate weights and keep the
analytical balance clean to protect all parts from dust or contamination. Hot or cold
samples (or reagents) must be brought to room temperature in a cool desiccator to
avoid the influence of the atmosphere, and they should then be weighed at room
temperature. The door of the balance case should always be kept closed, except
when the weighing bottle is being put in or taken out. The sample should be weighed
in the weighing bottle (or dish) or on powder paper. If the sample includes volatile
constituents or tends to absorb moisture in air, it should be dried and weighed in a
weighing bottle which is capped to prevent evaporation or moisture absorption during
weighing. After setting the balance to zero, the analyst should weigh the empty
weighing bottle, which has been preheated for more than two hours in an oven at an
agreed temperature (e.g., 110 ± 2 °C) and has been cooled in a desiccator, or
powder paper (1), then weigh the weighing bottle or powder paper with the sample
added (2). The sample's weight is as follows:

Weight of sample = (2) - (1)

If the weight of an empty weighing bottle or powder paper is already set at zero
on the balance, the weight of the sample is displayed directly. During weighing, the
sample should not be added to the weighing bottle on the pan or be removed from
the weighing bottle on the pan. The weighing bottle should not be handled directly
with the hands. It is desirable to handle the weighing bottle with tongs, a piece of

I/C1/7/3
 paper or clean gloves. If the sample or reagent spills over the pan, the analyst should
immediately clean it up with a brush or with a paper towel or tissue paper.

7.5. Screening analysis

7.5.1. Appearance and nature of sample

When an analyst receives a sample, the appearance, weight and nature of the
sample should first be observed. The appearance and nature of the sample should
be examined using the sense of sight, smell or hearing. The state, colour, smell,
size, appearance, weight, etc., of the sample should be noted in writing. If
necessary, wet samples should be dried and the dry matter tested.

Next, the solubility in various solvents, the melting point, the boiling point, the
specific gravity, etc., should be examined if necessary.

7.5.2. Colour test and precipitate reaction

7.5.2.1. Apparatus

The reagent bottles, test-tubes, test-tube support, test-tube holder, centrifuge

tube, porcelain spot test plate, glass stirring rods, platinum wire, burner, wire gauze
with asbestos centre, medicine dropper, funnels, paper filter, spatula, pH test paper,
etc., should be prepared in advance.

7.5.2.2. Reagents

Each experiment should be understood thoroughly and the necessary

reagents should be prepared by analyst in advance. Each reagent must be
prepared according to the interpretation of each test method. Some reagent
solutions are unstable and their period of use limited; freshly prepared reagents
should be employed whenever possible or necessary. Even if the solution is stable,
the analyst ideally should prepare a quantity of that solution once or twice a year to
avoid any problems. It is also desirable to prepare reference chemicals or materials
for the control experiments.

7.5.2.3. Purpose

These tests are carried out to provide a rapid screening of ions, functional
groups, compounds and elements included in the sample; they are very useful for a
systematic analysis.

I/C1/7/4
7.5.2.4. Test

A preliminary test should be carried out in advance if the analyst has enough
sample and reagent, so as to provide a guideline for the following test. In parallel
with the test of the sample, the analyst should carry out a control and blank test
using the same quantities of all reagents to ensure the detection of the analyte.
The suitable amount of the sample or reagent prescribed in the analytical methods
should be used in order to avoid any problems. The analyst should note (in writing)
the degree of colour change and the amount of precipitate for future testing.

7.5.2.5. Methods

Some testing methods generally used in Customs laboratories are as follows :

Beilstein test : halogens

Alkali metal fusion method : halogens, sulphur, nitrogen, phosphorous

Liebermann reaction : phenol (also reaction with ferric chloride)

Simon reaction : secondary amines

Chromotropic acid-sulphuric acid reaction : form-aldehyde

Precipitation reaction : SO42- + Ba2+ Þ BaSO4 ↓

+
Ag + X- Þ AgX↓

X : Halogen

These and other testing methods are set out in many technical publications
(see Chapter 4. Technical literature and reference books).

7.6. General concept of chemical equilibrium

The chemical reaction between the reacting species A and B is generally as

follows :

aA + bB ↔ cC + dD

a, b, c and d : coefficients
C and D : reaction products from the chemical reaction between A and B

When this system is at equilibrium, the equilibrium constant k is described as

c d
[C] [D]
k = _______
a b
[A] [B]

[A] : molar concentration of species A,

e.g., the equilibrium constant for water

+ -
(2H2O ↔ H3O + OH ) is

I/C1/7/5
 + -
[H3O ] [OH ]
k = ___________
2
[H2O]

Because the activity of water is constant in dilute solutions (~ 55.3 M), the self-
ionisation constant kw is as follows :
+ - -14
kw = [H3O ] [OH ] = 1 x 10 (at room temperature)

The pH of the solution is defined as

+ + -
pH = -log[H3O ] or -log[H ] = 14 - log[OH ] = 14 - pOH

On the other hand, if the solubility of one species is limited and exceeded, e.g.,
[C] ~ 0, this species is called "insoluble" and the chemical reaction between the species
A and B proceeds to the right and the precipitate C occurs in the solution.

aA + bB → cC↓+ dD

In a redox reaction, oxidation involves the loss of electrons by species and

reduction involves the increase in electrons. The reaction is as follows:

Reduction
-
aOx + ne ↔ bRed
Oxidation

The potential of this reaction depends on the concentration of the species and the
relationship between them is described by the Nernst equation as follows :
b
2.3026RT [Red]
E = Eo - _________ log ______
a
nF [Ox]

E : Reduction potential
Eo : Standard potential
-1
R : Gas constant (8.3143 V coul eq )
T : Absolute temperature (K : 274.16 + °C)
n : Number of electrons
-1
F : Faraday constant (96.487 coul eq )

Molarity calculations are as follows :

sample weight (g)
moles = ____________________
molecular weight (M.W.)
mol mmol
M (molar concentration) = _____ = ______
l ml

Normality calculations is as follows;

Eq. = mol x number of reacting units*

*) e.g., reacting unit ; HCl = 1, H2SO4 = 2, NH3 = 1,

I/C1/7/6
 Eq. mEq.
N (normal concentration) = ____ = ____
l ml

7.7. Gravimetric analysis

There are mainly two types of weighing. One involves a sample being chemically
converted into another substance of low solubility and known composition, which is then
filtered, dried, sometimes ignited, and weighed. The other involves one component in
the sample being volatilized, collected and weighed; similarly, after one component is
removed, the remaining residue may be weighed.

7.7.1. Precipitation method

Precipitation methods with inorganic reagents are very useful for quantitative
- 2-
analyses for Cl , SO3 , etc., in a cost-effective manner.

Organic reagents have been used more selectively in the precipitation method
for inorganic ions.

However, these analyses are not specific to a particular ion but rather form
precipitates with groups of ions; for example, the chloride ion is determined by
precipitation of the salt by Ag+ to form AgCl, but other halogen (iodide and bromide)
ions in the sample will also be coprecipitated and the resulting analysis will be high.
- +
Cl + Ag → AgCl↓ (precipitate)
- - +
and Br + I + 2Ag → AgBr↓ + AgI↓
(precipitate : impurity)

A test sample solution is placed in a container (beaker) and a small excess of

reagent is added to the test sample solution, inducing precipitation of a reaction
product. The precipitate is transferred onto a filter and properly washed with a
solvent or solution in which the precipitate is insoluble. The precipitate is then dried
and weighed.

There are several means of increasing the particle size of the precipitate to
increase purity and optimise the effectiveness of filtration, including the following

- heating the sample container gently in advance;

- using a dilute sample and reagent;
- adding the reagents slowly, while stirring;
- cooling the sample solution gradually to room temperature.

Application : Quantitative analysis of e.g., halogen ions, sulphuric acid ions and
silicone oxide. Ion-chromatography is now employed in advanced Customs
laboratories to determine halogen ions and sulphuric acid ions.

I/C1/7/7
 7.7.2. Volatilization method

Volatilization methods are used for the determination of dry residue and volatile
matter in water or volatile organic solvent solutions.

(Determination of dry residue)

A 1 g sample is accurately weighed in a sample container (weighing bottle

(containing a glass rod), etc.) which has been preheated for more than two hours in
an oven at a temperature of e.g., 110 ± 2 °C and then cooled in a desiccator. The
container is then placed on/in a water bath to evaporate the volatile matter. After
wiping the outside of the sample container with tissue paper, the residue is dried in
the oven, again at a temperature of 110 ± 2 °C, to constant mass (see ISO 759,
3251, etc.).
Constant mass of residue
Dry residue (%) = ________________________ × 100
Weight of original sample

(Determination of volatile matter)

In the case of aqueous solutions, the Karl Fischer method (ISO 3733) has often
been employed in Customs laboratories to determine water. For the determination of
volatile organic solvents, the following distillation methods can be employed : ASTM
D 86, 850, 938 and ISO 918, etc.

7.8. Volumetric analysis

This technique is based on the measurement of the volume of a standard

volumetric solution (a reagent) that must be titrated to react completely (equivalence
point) with all material in a sample to be analysed. The following experiment should be
carried out at constant temperature, since the volume of standard volumetric solutions
depends on the temperature.

There are two types of preparation methods for obtaining standard volumetric
solutions. If a standard substance is sufficiently pure, a weighed quantity of standard
substance is dissolved and diluted to a specific volume. Otherwise the standard
volumetric solution is standardized indirectly by titrating a weighed quantity of primary
standard or secondary standard solution.

The end point of titration is generally detected by a colour change (brought about
by an added indicator) or other physical properties such as conductivity, electrical
potential, etc.

The following are required for volumetric analysis :

- The equilibrium constant is very large and the reaction proceeds quantitatively;
- The reaction speed is rapid;
- An appropriate indicator, etc., to identify the end point is often present;
- There should be no component in the sample to interfere with the reaction.

I/C1/7/8
7.8.1. Acid-base titration analysis

This technique is very useful for determining the concentration of acid or base
in a sample solution in a cost-effective manner.

If a marked change in pH cannot be obtained, a back-titration method is

employed. In the case of a weak acid or base, which cannot be determined in water,
non-aqueous titration techniques can be employed.

The sample is titrated with a standard volumetric solution of a strong acid or a

strong base. A titration curve is constructed by plotting the pH of the solution as a
function of the volume of the standard volumetric solution added. An example of a
titration curve is shown in Fig. 1. The end point is usually indicated by a sharp
change in pH that occurs at the equivalence point. Indicators and a pH meter are
used to detect the end point. The concentration of acid or base in the sample
solution is calculated as follows;
N × y × 1000 × d
M = _______________
u × 1000 × x

u : Number of reacting units

e.g., HCl = 1, H2SO4 = 2, NH3 = 1,
M : Molar concentration of sample solution
x : Volume of sample solution (ml)
N: Normal concentration of standard volumetric solution
y : Volume of standard volumetric solution at the end point (ml)
d : Degree of dilution

14

12

10

Phenolphthalein
8
pH
6 Methyl red

2 Equivalence point

0 25 50 75

Volume of 0.1 M NaOH (ml)

Fig. 1. Titration curve for 50 ml of 0.1 M HCl versus 0.1 M NaOH

I/C1/7/9
 a. Preparation of standard base solutions

A saturated NaOH solution is prepared with distilled deionized water and

NaOH, and stored in a dark room. Several days later, this solution is filtered to
remove Na2CO3 and diluted to appropriate concentration with distilled deionized
water. As a primary standard, potassium acid phthalate is employed to
standardize the NaOH solution. Phenolphthalein is normally used as an indicator.
The standardized NaOH solution should be stored in a plastic bottle with a screw-
cap. Commercially available standardized NaOH solution is also widely used in
Customs laboratories.

b. Preparation of standard acid solutions

Concentrated HCl is diluted to the appropriate concentration with distilled

deionized water. This solution is standardized by titrating a primary standard
(sodium carbonate or tris(hydroxymethyl) aminomethane (THAM)). A
standardized NaOH solution is also employed to standardize the HCl solution as a
secondary standard. Commercially available standardized HCl solution is also
very convenient.

c. Indicators

Transition ranges of pH and colours of some common indicators are shown

in table 1.

Table 1 Indicators

Indicator Colour* pH*

Bromophenol blue yellow ↔ blue 3.0 - 4.6
Methyl orange red ↔ yellow 3.1 - 4.4
Methyl red red ↔ yellow 4.4 - 6.2
Bromothymol blue yellow ↔ blue 6.0 - 7.6
Phenolphthalein colourless ↔ deep-red 8.5 - 9.0

* Source : The Merck Index, Eleventh Edition.

d. Titration procedures

A sample is generally diluted to the appropriate concentration with distilled

water by means of pipettes and volumetric flasks; this solution is called the test
sample solution. A constant amount of reference, blank and test sample solutions
should be titrated with the standard volumetric solution in advance in the presence
of a few drops of the indicator to ascertain the colour change of the indicator and
to determine the approximate concentration of the test sample solution. Titration
of the blank and the test sample solutions should subsequently be carried out.
The standard volumetric solution should initially be added rapidly and, on nearing
the end point, it should be added slowly drop by drop; the flask should be shaken
frequently to ensure thorough mixing.

Application : Quantitative analysis of e.g., inorganic acids and bases, organic

carboxylic acids, organic amines, amino acids, drugs. Ion-chromatography is
often employed in advanced Customs laboratories to determine inorganic and
organic acids, etc. The Kjeldahl analysis for determining nitrogen is well known.
I/C1/7/10
7.8.2. Precipitation titration analysis

The Mohr method is well known as the most commonly used precipitation
titration. This technique is used to determine the concentration of anion in a sample
solution. The sample is titrated with a precipitating agent (standard volumetric
solution). Two types of indicators are generally used for the detection of the end
point. One indicator reacts with the precipitating agent in excess after the
equivalence point and forms a coloured compound. Another is adsorbed on the
surface of the precipitate at the equivalence point and a colour change takes place.
An example of the Mohr method is as follows :
+
- + Ag (in excess)
nCl + Ag →→→→ nAgCl↓ ______________ → Ag2CrO4↓ (red)
-
CrO4 (yellow)

a. Indicators

Some common indicators are shown in table 2.

Table 2 Indicators

Indicator Colour* pH*

(Mohr method)
Potassium chromate yellow ↔ red

(Fajans' method)
Fluorescein yellowish-red 7-8
Dichlorofluorescein orange 4

* Source : The Merck Index, Eleventh Edition.

b. Titration procedures

A sample is generally diluted to the appropriate concentration with distilled

water by means of pipettes and volumetric flasks; this solution is called the test
sample solution. A constant amount of reference, blank and test sample solutions
should be titrated with the standard volumetric solution in advance in the presence
of a few drops of the indicator to ascertain the colour change of the indicator and
to determine the approximate concentration of the test sample solution. Titration
of the blank and the test sample solutions should subsequently be carried out.
The standard volumetric solution should initially be added rapidly and, on nearing
the end point, it should be added slowly drop by drop; the flask should be shaken
frequently to ensure thorough mixing.
- - - -
Application : Quantitative analysis of e.g., Cl , Br , I , SCN .

7.8.3. Complexometric titration analysis

This technique can be used to perform quantitative analyses of certain metal

ions in a cost-effective manner; however, it requires skilled and experienced analysts
and is also time consuming. ICP (see 7.12.1.2) or AAS (see 7.12.2) methods are
now often employed in advanced Customs laboratories on account of their accuracy,

I/C1/7/11
 rapidity and simplicity (these techniques do, however, require expensive and complex
instrumentation).

This technique is a complex formation titration to determine the concentration

of a certain metal ion with an electron pair donor (ligand). Ethylenediamine
tetraacetic acid (EDTA) is well known as a complexing agent (ligand) and usually
indicated as "H4Y". Since the selectivity of EDTA depends on the pH of a test
sample solution, varying the pH of the solution with a buffer solution and the use of
masking agents make it possible to titrate different groups of metal ions.

a. Preparation of high-purity EDTA and standard volumetric solutions

A high-purity EDTA solution is prepared by drying disodium ethylenediamine

tetraacetate dihydrate at 80 °C for two hours. In a back-titration, high-purity metal
solutions are used as standard volumetric solutions and the kinds of metals to be
used depend on the sample element to be analysed.

a. Indicators

Eriochrome Black T (BT, EBT; HIn2-) is well known as a typical indicator

for this technique. Calmagite and Xylenol orange are also used as indicators.

pKa=6.3 pKa=11.55
- 2- 3-
H2In ↔ H2In ↔ H2In
red (≤ pH 6) blue (pH 7-11) red orange (≥ pH 11)

b. Back-titration procedure

After pre-treatment of a sample, a constant volume of EDTA solution is

added to the test sample solution and after adjusting to the appropriate pH of
this solution with hexamethylene tetramine, the excess EDTA is titrated with the
standard volumetric solution.

Application : Quantitative analysis of e.g., metal ions

7.8.4. Reduction-oxidation titration analysis

This technique is based on an oxidation-reduction (redox) reaction. While

oxidizing agents tend to take on one or more electrons and be reduced to a lower
oxidation state, reducing agents tend to bring the reverse change. For example :
- + - 2+
MnO4 (pink) + 8H + 5e ↔ Mn (colourless) + 2H2O
+7
(Oxidizing agent : Mn )

This technique is often employed in Customs laboratories for quantitative

analyses (e.g., sucrose, MnO4-, etc.) and is accurate, useful, and less costly; other
more accurate, more rapid and simpler methods (e.g., high-performance liquid
chromatography (HPLC) for quantitative analysis of sugars, ion chromatography for
quantitative analysis of certain inorganic and organic ions, etc.) have now been
developed.

a. Preparation of standard oxidizing solution

I/C1/7/12
 Potassium permanganate solution is well known as a standard oxidizing
solution. This solution is boiled and placed in a dark room overnight. Next
morning it is filtered to remove the impurities (MnO2) and then standardized by
titrating a weighed quantity of primary standard, sodium oxalate (Na2C2O4), in an
acid solution.

b. Preparation of standard reducing solution

Sodium thiosulphate solution is widely used as a standard reducing solution

and is stable in air for a long time. This solution is prepared from pure sodium
thiosulphate and is also commercially available.

c. Indicators

Potassium permanganate solution is also used as a self-indicator.

A starch indicator is used for titration involving iodine. In the presence of

starch, any occurrence of I2 in a redox reaction changes a colourless solution to a
dark-blue one.

Other redox indicators are shown in table 3.

Table 3 Other redox indicators

Indicator Reduced Oxidized Solution*

form* form*
Methylene blue blue colourless 1 M acid
Indigo tetrasulphonate colourless blue 1 M acid
Diphenylamine colourless violet 1 M H2SO4

* Source : The Merck Index, Eleventh Edition.

d. Preparation of test sample

Sample elements to be analysed should be converted to the appropriate

oxidation state for titration, by adding certain oxidizing or reducing agents. The
excess of these agents can be removed before titration. Reference and blank
solutions should also be prepared in the same manner. The preoxidizing and
prereducing agents generally used are shown in table 4.

I/C1/7/13
 Table 4 Preoxidizing and prereducing agents

Agents Oxidation state Removal method

(Prereducing agents)
Sodium sulphite and sulphur Th(III) → Th(I) Boiling or bubbling with CO2
dioxide Fe(III) → Fe(II)
Cu(II) → Cu(I) Adding HgCl2
Fe(III) → Fe(II) (excess)
Stannous chloride U(VI) → U(IV) Filtration
Sn(IV) → Sn(II) Filtration
Pb 2H
+
→ H2
Zn
(Preoxidizing agents)
Perchloric acid Cr(III) → Cr(IV) Boiling the diluted solution

Potassium persulphate Cr(III) → Cr(IV) Boiling

V(IV) → V(V)
Permanganate V(IV) → V(V) Adding hydrazine and boiling
Cr(III) → Cr(IV) Boiling
Bromine Ti(I) → Ti(III) Boiling
Hydrogen peroxide Co(II) → Co(III)

e. Titration procedure

A constant amount of reference, blank and test sample solutions should be

titrated with the standard volumetric solution in advance in the presence of a few
drops of the indicator to ascertain the colour change of the indicator and to
determine the approximate concentration of the test sample solution. Titration of
the blank and the test sample solutions should subsequently be carried out. The
standard volumetric solution should initially be added rapidly and, on nearing the
end point, the standard volumetric solution should be added slowly drop by drop;
the flask should be shaken frequently to ensure thorough mixing.

Application : Quantitative analysis of samples which have oxidation and reduction

ability, e.g., metal ions, saccharides, aldehydes.

7.9. Electrolytic analysis

This technique is based on the transfer of electrons from one species to another.
In redox reactions, oxidation involves a loss of electrons by species and reduction
involves an increase in electrons.

This technique can be used to perform quantitative analysis of certain metal ions
in a cost-effective manner; however, it requires skilled and experienced analysts and is
also time consuming. ICP (see 7.12.1.2) or AAS (see 7.12.2) methods are now often
employed in advanced Customs laboratories on account of their accuracy, rapidity and
simplicity; these techniques do, however, require expensive and complex
instrumentation.

I/C1/7/14
7.9.1. Potentiometric analysis

This technique is used to ascertain the concentration of sample elements by

determining the potential between reference and indicator electrons without the
passage of current in the cell. The saturated calomel electrode (SCE) is well known
as a reference electrode. There are two types of indicator electrodes : metallic
electrodes such as silver, copper and mercury, and membrane electrodes such as
the glass electrode used for pH meters.

7.9.1.1. Potentiometric titration

Standard and test sample solutions should be prepared including a high

concentration of electrolyte. For the preparation of a standard solution, any species
in the sample which affect the determination of sample elements to be analysed
should be added to this solution. An appropriate amount of solution is added to a
beaker on a stirrer. After setting with the indicator and reference electrode and
switching on the stirrer, the standard and test sample solutions are titrated with a
standard volumetric solution. A standard volumetric solution should initially be
added rapidly and, on nearing the end point, standard volumetric solution should be
added slowly drop by drop. The burette and potential reading should be recorded.
The titration is continued through the end point. The end point is determined by
interpolation or from the titration curve. After standardization of the standard
volumetric solution by a primary standard, the concentration of the sample is
calculated. Whenever transferring the electrode from one solution to another,
thorough washing with ionized water and carefully wiping with clean tissue are
required.

7.9.1.2. pH meter

This is a device for determining the pH of a sample solution. As glass

electrodes tend to break, careful handling is required.

The voltage of this cell E is as follows :

2.3026RT 1 +
E = k - _________ log ____ = k + alog[H ] = k + apH
+
F [H ]

(E-k)
pH = _______
a

This technique can normally be calibrated at two points : one at pH 4.00 or

9.22 and another at pH 6.88 in the pH buffers at 20 °C. When transferring the
electrode from one solution to another, wash thoroughly with deionized water and
wipe carefully with clean tissue. After adjusting of the pH, the potential of the test
sample solution is then determined and the pH value of the test sample solution is
indicated on the display. Once finished, the electrode should be thoroughly washed
with deionized water and capped with deionized water to prevent it from drying.

I/C1/7/15
 7.9.2. Voltametry analysis

7.9.2.1. Polarography

Polarography is a kind of voltametry and a dropping mercury electrode (DME)

is used as working electrode. The plot of current (µA) versus voltage (V) is called a
polarogram. An example of a polarogram is shown in figure 2 (not reproduced).
Half wave potential E1/2 depends on the species being analysed and the diffusion
current id is proportional to the concentration of the analytical species.

Preparation of calibration curve and determination of concentration of sample

elements

After preparation of several kinds of standard solutions and test sample

solutions, each polarogram is determined under the same conditions. A calibration
curve of the diffusion current id (y axis) versus the concentration of metal ion in
standard solutions (x axis) is first plotted. The induced equation is calculated as
follows :

y = b + ax

a : slope of calibration curve

b : intercept of y axis

The concentration of the sample element is then calculated on the basis of

the above equation.

7.9.2.2. Amperometric titration

In this technique, the current passing through a cell at fixed potential is

measured at different points in a titration and plotted against the titrated volume of
standard volumetric solution. From the equivalence point, which is given by
extrapolation to the intersection of the two lines, the concentration of the sample
elements can be calculated.

7.9.2.3. Electrophoresis

This technique is extremely good for identifying the species of water-soluble

proteins. A variety of supports may be prepared or are commercially available,
including paper, gels such as starch, agar and polyamide.

After developing and colouring, characterized chromatograms are available; a

detailed comparison of the sample chromatograms with standard chromatograms of
proteins makes it possible to identify the kind of protein.

Application : Qualitative analysis of water-soluble proteins to identify the species of

meats, plants, etc.

I/C1/7/16
7.10. Separation of mixture samples

Separation procedures are essential for identifying the composition of traded

commodities. In the case of mixture samples which consist of more than two kinds of
constituents, analysts are often required to separate and to identify each constituent
qualitatively and quantitatively. Though certain separation procedures are laid down in
7.7 "Gravimetric analysis", further separation procedures especially for organic
samples are described in this section.

7.10.1. Separation procedures by appearance

This separation technique is occasionally possible for mixture samples

where each constituent has a different appearance, e.g., a different colour, size,
crystal form, etc. Analysts can separate these constituents by hand with a pincette
or using a sieve with various sizes of aperture (see Chapter 11, Notes 2 (B) and 3,
and Chapter 16, Note 2).

7.10.2. Separation procedures using filtration

This is a convenient and widely used technique for the separation of

insoluble matter in a liquid sample. A paper, glass or membrane filter may be used,
according to the kind of insoluble matter in the sample. The sample is passed
through the filter and the insoluble matter is trapped in the filter. The insoluble
matter is washed with a solvent or solution in which it is not soluble. The residue is
then dried and analysed. The filtrate is also collected and used for further analysis.

7.10.3. Separation procedures using distillation

This separation technique is often used for samples which consist of more
than two constituents having different boiling points. For example, a volatile
component in the sample may be removed by first heating on/in a water bath in a
fume hood (allowing most of the volatile matter to evaporate) and then heating in an
electric drying oven/vacuum drying oven to obtain a dry residue. (see heading
27.07; ASTM D 86, 850 and 938; and ISO 759, 918, 3251, etc.)

(Distillation apparatus and separators)

These are used for distillation and the separation of components in samples.
It is necessary first to check all glassware for any cracks or chips. If any are found,
the glassware should be disposed of. When a flammable or volatile sample is
analysed, the sample should be heated with a water bath or an electric heater in a
fume cupboard and not directly with a gas burner or other open flame. Do not
forget to ensure that water flows freely through the reflux condenser. When
distillation is finished, the temperature of the sample residue should be lowered
slowly at room temperature, and the apparatus and separators should be cleaned
with an appropriate solvent.

7.10.4. Separation procedures using solvent extraction method

These techniques are based on the difference in solubility of two

compounds in a solvent.

The mixture is dissolved in a solvent and filtered. The insoluble product

recovered on the filter is dried and the solute is evaporated to dryness.

I/C1/7/17
 The soxhlet system makes it possible to extract completely from a mixture
the components that are hot-soluble in a volatile solvent : the solvent, placed in a
flask, is volatilized then condensed in a thimble containing the mixture; when part of
that mixture has been dissolved, the solvent returns to the initial flask where it is
once again volatilized. The dissolved components, which are non-volatile, are
concentrated in the flask until completely extracted.

The Kumagawa system, which operates on similar lines, is also widely used.

7.10.5. Separation procedures using centrifugation

This technique is very useful for separating the precipitate from a "muddy"
sample solution. The sample is poured into a container for a centrifuge, and water
is poured into another container to equal the sample container in weight to ensure
equilibrium in the centrifuge. The precipitate is "concentrated" at one end of the
sample container by centrifuge force, e.g., at 2000 rpm for 10 minutes. The
precipitate is allowed to settle and physically separated from the solution by
decantation or filtration. Sample solutions containing volatile matter require the use
of a sample container with a cap.

7.10.6. Separation procedures by means of chromatography

Chromatography is a very convenient separation technique for complex

samples and is based on the difference of distribution of each component between
two phases, i.e., the "stationary phase" (solid or liquid) and the "mobile phase"
(liquid or gas). A sample placed at the beginning of the stationary phase, is
"developed" by the mobile phase which flows through the stationary phase and
each component is separated according to its characteristic tendency to be
"retained" by the stationary phase. This procedure is explained in detail under
section 7.11 (Chromatography).

7.10.7. Other

The precipitation procedure, electrolysis, ignition to ash, etc., are also used
for the separation of samples in Customs laboratories.

7.11. Chromatography

7.11.1. Column chromatography

This technique is inexpensive and widely applicable to the analysis of

organic preparations in Customs laboratories. If a high-performance liquid
chromatograph (HPLC) (7.11.5) is available in the laboratory, column
chromatography would be less used. However, this technique remains useful and
worthwhile (e.g., for preparative-type analysis, etc.).

I/C1/7/18
 M o b ile p h a s e (s o lv e n t)

S a m p le

S ta tio n a ry p h a s e (s u c h a s s ilic a g e l)

A b s o rb e n t c o tto n

F iltra te

F ig . 2 . D ia g ra m o f c o lu m n c h ro m a to g ra p h y

A diagram of column chromatography is shown in Fig. 2. A sample is

placed at the top of the column which is packed with the small uniformly-sized
particles of polar adsorbents such as silica gel or alumina (stationary phase);
absorbent cotton wadding is placed at the end of the column. Successive elutions
take place with solvents (mobile phase) of gradually increasing polarity. Each
component in the sample is developed slowly downward according to its polarity.
Non-polar materials, e.g., hydrocarbons, are initially eluted with non-polar solvents,
e.g., n-hexane. More polar materials are retained on the column until a sufficiently
high polar solvent passes through the column. The eluent is fractionated and dried.
Dry residues are weighed and analysed to identify the contents and composition of
the sample. The analytical conditions, e.g., the column (diameter and length), the
adsorbent, the sample weight, the kind of eluent and the detection method should
be noted.

Application : E.g., separation of petroleum oils from lubricating preparations;

separation of each component in surface-active preparations; separation of
mixtures of chemicals.

7.11.2. Paper chromatography (PC)

This is an economical and qualitative method for examining a mixture and

establishing the number of components. This method is less costly than the TLC
method (7.11.3), though it is time consuming and less sensitive than TLC.

A diagram of PC is shown in figure 3. The stationary phase is a piece of

filter paper. A 0.1 - 1 g sample is dissolved in 10 ml volatile solvent. About 1 - 5 µl
of the sample solution is spotted on a paper plate by means of a capillary tube and
the solvent is allowed to evaporate. Each spot must be at least 2 cm away from the
next one and at least 2 cm from the bottom of the plate. It is recommended that
location of the origin of spots be marked on the plate in advance with a pencil. The
I/C1/7/19
 plate is then suspended in a chromatographic chamber, the bottom 1.0 to 15 cm
(below the line of sample spots), solvent (mobile phase). Each spot is "developed"
as the solvent front migrates upward (by capillary action) through the plate,
reaching a height of 15 - 20 cm on the plate. The plate is then removed from the
chromatographic chamber and dried thoroughly in a fume cupboard. The
movement of the spots is generally detected by exposing the plate to ultraviolet
(UV) light or iodine vapour or by spraying the plate with colouring agents.

Development

Spot

Development

Solvent front
2 cm
Solvent (Mobile phase)

Chromatographic chamber
2 cm
Fig. 3. Paper chromatography procedure

The Rf value (distance the sample or its components has travelled from the
origin divided by the distance the solvent front has travelled) of each component in
the sample is compared with the values of standard substances. Apparent
identification is made by comparing the Rf value with the standard substances.
Sometimes each spot is cut from the plate, extracted with an appropriate solvent,
and analysed to identify the chemical structure. The analytical conditions, e.g., the
system, the plate, the mobile phase, the detection method and the spot volume,
should be noted.

Application : Separation of e.g., saccharides, organic acids and amino acids in food
preparations; mixtures of chemicals.

7.11.3. Thin-layer chromatography (TLC)

This is an excellent, inexpensive and qualitative technique for rapidly

examining mixture samples and achieving good separation. High-performance thin-
layer chromatography (HPTLC) is also employed in Customs laboratories. The
HPTLC plate enables more rapid and more accurate determination than normal
TLC.

I/C1/7/20
 The stationary phase is a thin layer of adsorbent material supported on a
glass or plastic plate. Sometimes, this plate is dried in an oven to make it active. A
0.05 - 0.5 g sample is dissolved in 10 ml volatile solvent. About 1 µl of the sample
solution is spotted on the plate by means of a capillary tube, and the solvent is
allowed to evaporate. Each spot must be at least 1 cm away from the next one and
2 cm away from the bottom. It is recommended that the location of the origin points
of spots be marked on the plate in advance with a pencil. The plate is placed in a
chromatographic chamber containing a suitable developing solvent (mobile phase);
and each spot is then developed until the solvent front reaches 10 or 15 cm. For
successful separation, it is essential to select an appropriate mobile phase. The
plate is removed from the chromatographic chamber and dried thoroughly in a fume
cupboard. The spots are generally detected by exposing the plate to ultraviolet
(UV) light or iodine vapour, or by spraying the plate with colouring agents.

The Rf values (see 7.11.2 above) of the spots are calculated and compared
with the Rf values of standard substances. Apparent identification is made by
comparing the Rf value with the standard substances. Individual spots may be
extracted with an appropriate solvent and analysed to identify the chemical
structure. Standard thin-layer plates or sheets may be commercially available. The
analytical conditions, e.g., the plate, the spot volume, the mobile phase and the
detection method, should be noted.

Application : Separation of e.g., saccharides, organic acids and amino acids in food
preparations; mixtures of chemicals; drugs.

7.11.4. Gas chromatography (GC)

GC is an excellent method for determining volatile mixtures qualitatively and

quantitatively, and is an essential requirement for Customs laboratories. GC is
better than any other chromatography system in terms of analytical speed,
sensitivity and reproducibility. For non-volatile and unstable substances,
trimethylsilicification (TMS), acetylation (e.g., trifluoroacetic acid(TFA)) and methyl
esterification are employed.

TMS

R-OH → R-O-Si(CH3)3

TFA

R-OH → R-O-CO-CF3

BF3 + MeOH, etc.

R-CO-OH → R-CO-O-CH3

The gas chromatograph instrument is equipped with a carrier gas (N2 or He)
cylinder and its line, a hydrogen gas cylinder (for FID detector) and its line, an air
compressor and its line, columns and a recorder (integrator) to calculate the
retention time (Rt) and peak area.

I/C1/7/21
 The nature of the components in a sample (e.g., boiling points, whether non-
volatile components such as non-volatile acid, alkali or oxidizing agent, or reactive
components are included, etc.) should be investigated in advance and an
appropriate column should be selected according to the nature of the sample, in
order to ensure a successful experiment. If non-volatile components are injected,
the analyst should sweep an injection portion. The sample is generally diluted with
a volatile solvent (e.g., diethyl ether, etc.) to an appropriate concentration to keep
the column and injection portion free from contamination. The degree of dilution
depends on the composition of the sample.

The stationary phase is generally an adsorbent or particles of porous

support impregnated with a non-volatile liquid. This phase is packed in a glass or
stainless steel column, or maintained/chemically bonded in the inert wall of a
capillary column. Before a capillary column is used, its splitter, connector, etc.,
must be prepared. 0.1 - 5 µl of the test sample or its solution is rapidly injected into
the injection port with a micro-syringe, through a rubber septum. The injection port
is adequately heated to convert the sample or its solution to the vapour state. The
vapour state components are introduced by carrier gas (mobile phase) to the
column. Each component is developed and separated by its distribution between
the gas and liquid (solid) phases through the column, in the same manner as the
foregoing chromatographic processes. Eventually, each component reaches the
detection portion separately and is automatically detected and recorded.

For GC detectors, a flame ionization detector (FID) is widely used in

Customs laboratories, though a thermal conductivity detector (TCD) and an electron
capture detector (ECD) may also be used.

The time between the injection and the detection of each peak is called the
"retention time (Rt)". A comparison of Rt between a standard substance and an
unknown substance may make it possible to identify the unknown peaks.

For quantitative analysis, the internal standard procedure is widely used in

Customs laboratories. An internal standard (IS) substance should be pure and its
structure must resemble that of the component to be determined. It must be
possible to separate the peak of the IS from all peaks of the sample sufficiently.
The sample and the standard substances are dried, if necessary. A variety of
standard solutions, which include a constant amount of IS, are prepared where the
object component in the sample is present in concentrations varying from 0 % to
about 10 %. The test sample solutions are prepared in the same way as the
standard solutions. A constant volume of the standard solution and of the test
sample solution is injected rapidly into the GC, under the same conditions. A plot of
peak area ratio (standard substance/IS) versus weight ratio (standard substance/IS)
shows a good correlation. An example of the calibration curve is shown in figure 4.
Since the peak area is roughly proportional to the concentration, calibration curves
obtained from the standard solutions are linear with excellent correlation factors.
The concentration of the object component in the sample is calculated from a
calibration curve.

The analytical conditions, e.g., the system, the column (name, diameter and
length), the mobile phase, the gas flow (split ratio for the capillary column), the
temperature programme, the detection method, the injection volume should be
noted.

I/C1/7/22
 y

1 .5
P e a k a re a ra tio
(sa m p le A /IS )

1 .0

0 .5

0 .5 1 .0 1 .5 2 .0

W e ig h t ra tio (s a m p le A /IS )

F ig . 4 . A ca lib ra tio n cu rve fo r p e a k a re a ra tio (sa m p le A /IS ) ve rsu s w e ig h t ra tio (sa m p le A /IS )

Application : Qualitative and quantitative analysis of e.g., fats and butters,

constituting fatty acids of fats and butters (methyl esterification), aromatic
components in foods, beverages and spirits, alcohols, saccharide (TMS), vegetable
oils, wax, theobromine in cocoa, petroleum oils, volatile chemicals, medicaments,
essential oils, perfumery, sorbitol (derivative), fungicides, oligomers, drugs.

7.11.5. High-performance liquid chromatography (HPLC)

HPLC is an excellent method for determining organic or inorganic mixtures

qualitatively and quantitatively, particularly non-volatile and unstable mixtures which
cannot be analysed by GC. In many Customs laboratories, this technique is
employed instead of volumetric methods for the quantitative analysis of
saccharides.

A high-performance liquid chromatograph instrument is equipped with a

pump to provide high pressure (0.1 - 9.9 ml/min, approximately 400 pascal),
columns (with pre-column), and a detector and recorder (integrator) to calculate the
retention time and area of detected peaks.

The nature of components in a sample (e.g., polarity, etc.) should be

investigated in advance and an appropriate column should be selected according to
the kind of sample, to ensure a successful experiment. The sample is generally
diluted with mobile phase to an appropriate concentration to gain a good separation
and to keep the column free from contamination. The degree of dilution depends
on the composition of the sample.

There are generally two types of stationary phase: a normal phase and a
reversed phase. In the case of the former, less polar mobile phase is used. For
the latter, more polar mobile phase is employed. A column packing with chemically-
bonded stationary phase is commercially available, ensures high pressure and
high-speed conditions and avoids removal of the stationary phase. These phases
are packed in a straight stainless steel column. A test sample solution is prepared
as 0.1 - 10 % solution in the mobile phase to be used. All solvents should be HPLC
I/C1/7/23
 grade. All mobile phases and the test sample solutions must be filtered through 0.2
- 0.45 micron filters (e.g., membrane filter) before use. If an aqueous mobile phase
is employed, it is necessary to carry out the de-air procedure of the mobile phase
with a supersonic instrument or under vacuum conditions. 0.5 - 10 µl of the sample
solution is generally injected through the external sample loop into the column. An
automatic injection system is convenient for injecting a constant volume of the test
sample and standard solutions. Each component is developed and separated in
the column in the same way as the foregoing chromatographic process. Eventually,
each component reaches the detection portion separately and is automatically
detected and recorded.

For HPLC, an ultraviolet (UV) detector is widely used in Customs

laboratories, and a differential refractometer (RI) detector, a fluorescent detector
and an amperometric detector may also be employed. A more recent development
is the diode-array detector (DAD) which gives a high degree of sensitive and
selective detection.

The time between the injection and the detection of each peak is called the
"retention time (Rt)". Apparent identification is made by comparing the Rt of the
sample with that of the standard substance.

As the peak area is roughly proportional to the concentration, the analyst

can determine the amount of substance quantitatively, in the same way as with GC.
The analytical conditions, e.g., the system, the column (name, diameter and
length), the mobile phase, the flow rate, the detection method, the injection volume,
should be noted.

Application : Qualitative and quantitative analysis of e.g., fats, fatty acids, amino
acids, saccharide, vegetable oils, theobromine in cocoa, vitamins, hormones,
proteins, peptides, steroids, antibiotics, organic chemicals, medicaments, sorbitol,
fungicides, oligomers, drugs.

7.11.6. Size exclusion chromatography (SEC)

This is an excellent technique for qualitative and quantitative analysis of a

sample which contains components of different molecular size (e.g., polymers,
oligomers, etc.). The average molecular weight of the sample can be estimated
using this technique. The prepared fractions (preparative-type system) are of a
sufficient quality to be utilized for the following analysis.

This system is also called "gel permeation chromatography (GPC)" and is

similar to HPLC mentioned above.

The stationary phase is a molecular sieve which has different sizes of pores
formed by the cross-linking of polymer chains. The stationary phase is packed in a
straight stainless steel column and a few columns are connected in series, and then
used for determination. The distribution of each component depends on its size
and shape. All solvents should be HPLC grade. A sample is dissolved at about 5
% solution in the mobile phase. The test sample solution must be filtered before
injection. Several ml of the test sample solution are injected through the external
sample loop onto the column. Immediately following the injection, the external
sample loop should be cleaned with the mobile phase. Each component is
developed and separated according to its size and shape. Eventually, each

I/C1/7/24
 component reaches the detection portion separately and is automatically detected
and recorded.

For SEC (GPC) detectors, an ultraviolet (UV) detector connected in series

with a differential refractometer (RI) detector is widely used in Customs
laboratories.

The time between the injection and the detection of each peak is called the
"retention time (Rt)". Since log(molecular weight (M.W.)) values generally vary
inversely to the time of elution, a comparison of the Rts of an unknown substance
and a standard substance, the average molecular weight of which is already known,
makes it possible to estimate the average molecular weight of the sample.

A fraction collector automatically fractionates the elution at regular intervals.

The dry matter of each fraction is weighed and analysed to clarify the content of the
sample and the composition.

Application : e.g., synthetic polymers and oligomers, hormones, proteins, peptides,

steroids, polysaccharide, nucleic acids, organic chemicals, etc.

7.11.7. Other

Ion-exchange chromatography, super-critical-fluid chromatography and

counter-current chromatography are also widely available.

7.12. Optical and spectrophotometric analysis

7.12.1. Emission spectrophotometry

Emission spectrophotometry is an excellent technique for qualitative and

quantitative analysis of elements in samples, especially inorganic samples. With
this technique, the existence and intensity of the characteristic and essential
spectra lines derived from each element are determined.

7.12.1.1. Emission spectrophotometry

This method has many advantages in qualitative analysis, since the analyst
can determine many elements in a sample simultaneously in a short time and with
good accuracy. The cost of the analysis is reasonable. This method is also used
for quantitative analysis. However, analysts need to be very careful when
preparing the sample.

A small amount of sample, generally solid, is placed in a graphite electrode,

subjected to energy by an electron arc or spark and is vaporized. Each element in
the sample is raised to an excited energy level. When it drops back to the ground
state, photons with energy equal to electronic transitions are emitted. They are
separated by a prism or grating, and an atomic spectrum arranged in order of
wavelength is produced. A photographic film or plate is generally used as a
detector. By measuring the existence and intensity of the characteristic and
essential spectra lines derived from each element, the analyst can identify the
kinds of elements in the sample. Iron is generally used as the standard
substance.

I/C1/7/25
 Application : e.g., qualitative analysis of elements in a sample, especially an
inorganic sample.

7.12.1.2. Plasma emission spectrometry (inductively coupled plasma (ICP))

This technique is extremely good for quantitative analysis of inorganic

compounds. Test sample solutions are easily prepared. This technique exhibits
low concentration detection limits and is extremely sensitive in respect of many
elements. ICP analysis can be used to detect more than 70 % of elements,
including boron, silicon, titanium and phosphorous. Through the use of high-
temperature plasma, much chemical interference is eliminated. The dynamic
range is extremely broad (i.e., four to six orders of magnitude). It enables
quantitative multi-element analysis under the same conditions, which is a major
advantage over AAS (7.12.2).

Most advanced Customs laboratories employ this technique, since it is more

accurate, simple and less time consuming than volumetric and electrolytic
analyses.

Samples are dissolved in inorganic acid (or acid solution) and the solution is
transferred to a volumetric flask and diluted to an appropriate concentration. A
variety of standard solutions of pure metals for making a calibration curve are
prepared when the object component in the sample is present in concentrations
varying from 0 ppm to about 30 ppm. The standard may be prepared solutions by
an analyst or are commercially available as 1000-ppm standard solutions.

The concentration depends on the element to be analysed. The matrices

should be added to these solutions to match those of the test sample solutions.
These solutions are prepared in the same way as the test sample solutions.

The test sample solutions and the standard solutions are introduced to the
inductively coupled plasma (ICP), which is argon plasma, through a spray
chamber nebulizer at a constant flow rate under the same conditions. Excited
elements in this plasma emit characteristic photons with energy equal that
resulting from the transition back to the ground state. They are separated by a
grating or monochromator, and each atomic spectrum is determined by a
photomultiplier tube manually set, by the analyst, at the wavelengths for specific
elements.

By measuring the intensity of each spectrum, a calibration curve is initially

prepared for each element. These calibration curves are linear with excellent
correlation factors, and the concentration of elements in the test sample solution
can therefore be calculated with good accuracy.

Application : Qualitative and quantitative analysis of many elements in samples,

especially inorganic samples (e.g., quantitative analysis of low levels of tungsten
and vanadium in steel).
7.12.2. Atomic absorption spectrophotometry (AAS)

This technique is well-suited to quantitative analysis. It is easy to prepare

the test sample. This technique exhibits low concentration detection limits and is
extremely sensitive in respect of many elements. Through the use of a different
radiation source for each element, much chemical interference is eliminated, but the
fact that the radiation source has to be changed frequently is a major disadvantage
of this technique.
I/C1/7/26
 Test sample solutions and standard solutions are prepared using the same
procedure as for ICP. These solutions are introduced to the flame through a burner
and converted to atomic vapour under the same conditions. Though some are
thermally excited by the flame, other residual atoms in the ground state absorb
characteristic radiation for each element; the source of this radiation is a hollow-
cathode lamp. The intensity of absorption is determined by a photomultiplier
through a grating. A calibration curve is obtained from standard solutions, and the
concentration of element in the sample can then be calculated.

Application : Quantitative analysis of many elements in samples, especially

inorganic samples.

7.12.3. Absorption spectrophotometry

Gamma rays
X rays λ v (cm-1)

10 nm 106

Vacuum ultraviolet
Ultraviolet 100 nm 105

Near ultraviolet

Visible

Near infra-red 1000 nm 104

Infra-red NaCl infra-red 10 µm 103

Far infra-red 100 µm 102

1000 µm 10

Radio waves

Fig. 6. Electromagnetic spectrum

The energy of the electromagnetic radiation E is related to the frequency ν

-1
(s ) or wavelength λ (cm) as follows :
hc'
E = hν = _____
λ

h : Plank's constant, 6.62×10-27 erg/s

10
c': Velocity of light (3×10 cm/s)

The Beer-Lambert law is described as follows :

I
A = -logT = -log ___ = ε l c
I0

A : Absorbance
T : Transmittance
I : Power of transmitted radiation
I0 : Power of incident radiation
I/C1/7/27
 ε : Molar absorptivity
l : Path length
c : Concentration of sample solution

I o I

l
Fig. 7. Absorption of radiation

7.12.3.1. Ultraviolet (UV) and visible spectrophotometry

This technique is widely used for quantitative analysis, since the relationship
between the intensity of the absorption and the concentration of the sample
follows the Beer-Lambert law accurately. This technique is also used to identify
the sample by comparing the spectra of the sample and the reference/standard.

To analyse a sample by determining its UV and visible spectra is called "UV

and visible spectrophotometry". The absorption of radiation energy in the UV and
visible region causes electron transition of molecules from the ground state to the
excited state. In fact, one of the primary uses of UV and visible
spectrophotometry is to determine the extent of conjugation within the molecule.
The intensity of the absorption varies according to the wavelength. Each molecule
has a characteristic UV and visible spectrum.

A deuterium discharge lamp (D2 lamp), which covers the UV region from 168
nm to 400 nm, and a tungsten filament incandescent lamp (W lamp), which covers
the visible region from 320 nm to 3,000 nm, are generally used as sources. The
analyst should select the source on the basis of the region of spectrum to be
determined. After stabilization of the source, the determination should be started.

The polychromatic radiation from the source is separated to each

wavelength radiation through a monochromator, such as a grating.

A sample cell made from quartz, in the form of a square cuvette (e.g., 1 cm
thick), is widely used as a sample container. The analyst should select an
appropriate solvent which has little absorption in the wavelength region to be
determined. More than two cells should be prepared, one for reference and the
others for a test sample and standard solutions. Before the determination,
background corrections of the cells should be carried out. The solvent is added to
I/C1/7/28
 one cell as reference and the test sample solution or standard solutions for a
calibration curve are added to the other cells. If necessary, a centrifugation
separation procedure should be carried out, in advance, for the test sample
solution and standard solutions. The relationship between appropriate
concentration and the value of ε is shown in Table 1.

Table 1 Appropriate concentration of test sample solution on the basis of ε value

ε c (mole/l) A (absorbance)
101-102 10-2 0.1 - 1.0
102-103 10-3 0.1 - 1.0
3 4 -3
10 -10 10 0.1 - 1.0

If the solvent tends to be volatile, the analyst should use a cell with a cap.
The analyst should initially wash cells with the solvent and then with the test
sample solution; finally the test sample solution is poured into the cell (but not up
to the top) and the outside of the cell should be carefully wiped with a piece of
clean tissue paper. Hold the sides, which UV and visible light does not pass
through, and keep the transmittance sides of the cell clean. After use, these cells
should be carefully washed with the solvent and stored in a wide-mouthed reagent
bottle to which sufficient alcohol or water has been added.

(Double-beam technique)

This technique is generally used for determining UV and visible spectra. An

electronic recorder is an indispensable tool in this device. After proofreading of
the wavelength, adjustment of the indicator and background corrections of the
cells, the reference cell and sample cell are inserted in the sample rooms
respectively. The test sample solution is scanned in the region to be determined.
Any difference of the transmittance between the reference and sample is detected
by a detector tube (phototube or photomultitube) in each wavelength and the
spectrum is simultaneously recorded.

(Single-beam technique)

This technique is capable of greater precision and is employed for

quantitative analysis. The procedure is similar to that of the double-beam
technique. A reference cell is initially inserted in a sample room and transmittance
or absorbance is set to 100 (%T) or 0 (A). A sample cell is subsequently inserted
in the sample room in place of the reference cell and the transmittance or
absorbance value is determined individually; the value should be noted by the
analyst.

Application : Qualitative and quantitative analysis of samples including molecules

which have paired non-bonding outer-shell electrons, such as nitrogen, oxygen
and sulphur, or having electrons in the π orbital (e.g., double bonds, triple bonds
and aromatic rings, etc.).

7.12.3.2. Infra-red (IR) spectrophotometry

IR spectrophotometry is based on the study of the interactions between a

substance and electromagnetic radiation with a wavelength of between 2.5 and
25 µm.
I/C1/7/29
 The energy is insufficient to modify the electronic energy of the molecule;
the excitations observed will be confined to vibrations and rotations.

The absorption spectrum obtained represents the transmittance (proportion

of light transmitted through the sample) in terms of the wave number.

Certain vibration frequencies may undoubtedly be associated with the

presence in the molecule of certain well-defined groups. The IR spectrum
-1
provides a real "identity card" for the molecule. The region 1,500 cm to
-1
400 cm , which is particularly rich in information is known as the molecule's
fingerprint.

Spectra libraries have been set up and make it possible automatically to

identify pure compounds.

7.12.3.2.1. Quantitative analysis :

The intensity of absorption is linked to the intrinsic properties of the

molecule and to the number of molecules present in the beam. This enables
quantitative analysis applications by applying the Beer-Lambert law.

7.12.3.2.2. Instruments

There are two types of IR spectrometers : the dispersion spectrometer and

the Fourier transform spectrometer, which uses optical interference.

The operating range is between 4000 cm-1 and 400 cm-1.

7.12.3.2.3. Technique for the preparation of samples :

a. Liquid spectra

Pure liquid :

These can be examined very simply in the form of a capillary film obtained by
placing one or two drops between two appropriate plates and introducing
these into observation cell.

To make the measurements easier to reproduce and more quantitative, thin

cells (0.005 - 0.1 mm) may be used depending on the intensity of absorption
of the vibration to be studied.

Spectra of dissolved substances :

In this way, it is possible to examine solid, liquid or gaseous substances,

which have to be dissolved in an appropriate solvent (i.e., one which has a
low level of absorbency and is within the region limits of the IR field under
examination).

The most widely used solvents are : CCl4, CS2, C6H12, CHCl3. They must be
completely anhydrous.

The double-beam technique can be used to compensate the absorption of the

solvent : for this, a cell of the same thickness as used for the sample beam
I/C1/7/30
 has to be placed in the reference beam; it is filled with pure solvent. In this
way, only the bands attributable to the solute are visible. However,
examination is not possible in regions of high absorption of the solvent.
Indeed, all the energy being absorbed, no light will come either from the
sample beam or from the reference beam, and the apparatus will merely plot
a straight line.

The examination of aqueous solutions poses many different problems :

- the constituent material of the plates which must be sufficiently transparent

to IR and also be water-resistant (AgCl, CaF2);

- very high absorption of water in a wide area.

b. Gas spectrum

A sample is introduced in a gas cell which should be capped at both ends by

discs of substances that are transparent to IR rays (e.g. NaCl).

c. Solid spectra

Examination by transmission

(Examination in the form of a film)

The methods of obtaining a suitable film depend largely on the substance to

be examined :

- evaporation of a solution on a disc;

- melting and compression (in a heating press) then solidification by cooling

of the film obtained (method often used for polymers).
(Examination in the form of a dispersion)

- Dispersion in a paste

The particles obtained by grinding are dispersed in a substance whose

viscosity is such that a paste-like slurry is formed which is observed between
two NaCl plates.

For this purpose, the oils are used; Paraffin oil ("Nujol") and fluorocarbon oil
(fluorolube).

When examining the spectrum, account has to be taken of the absorption of

the oil used.

- Dispersion in a pellet of alkali halide :

This is the commonest method used for solids

The finely ground particles are mixed with KBr powder, also ground to obtain
as homogenous a mixture as possible; the whole is rendered transparent by
2
recrystallization under very high pressure (10 tonnes/cm ). Generally, 1 mg of
solute is used in 300 mg of KBr.

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 Examination by reflection :

There are several techniques for depositing the sample on a reflective surface
and establishing the spectrum :

- specular reflection

- diffuse reflection

- attenuated (total) reflection (ATR).

These techniques are useful where very little of the matter is available.

(Analysis of IR spectrum)

It is necessary for Customs laboratories to have standard/reference IR

spectral data and publications in order to identify an unknown substance. If
standard/reference substances such as pure chemicals, drugs and polymers,
are available, the IR spectra should be determined and be stored. It is, of
course, desirable for the IR data to be arranged on the basis of the
Harmonized System/molecular weight/molecular formula. If the structure of a
sample can be assumed from the accompanying certificate and relevant
documents, the analyst should compare the sample spectrum with
standard/reference spectra of the same or similar substances. In the case of
insufficient information from the accompanying certificate, the analyst can
identify the functional groups (e.g., benzene ring, alcohol, ether, carbonyl,
sulphonate, etc.) empirically. On the basis of these analyses and other data
such as appearance, melting point, colouring test, etc., the analyst can
analogize the structure of the sample component and compare the sample
spectrum with the spectra of similar substances. By comparing both spectra,
especially in a fingerprint region, the structure of the sample can be identified.
The correlation tables between functional groups and the IR region are set out
in many publications. The sources of IR spectral data generally used in
Customs laboratories are as follows :

Aldrich Library of IR Spectra : Aldrich Chemical Co.

The Sadtler Handbook of Reference Spectra : Sadtler Research Lab. Inc.

Application : Qualitative analysis of organic and inorganic substances.

Quantitative analysis of the composition of e.g., polymers.

7.12.4. Other

The microscope Fourier transform infra-red detector, the raman

spectrophotometer and the spectropolarimeter are generally used in Customs
laboratories.

7.13. Electromagnetic analysis

7.13.1. X-ray diffraction analysis

I/C1/7/32
 This technique is well-suited to qualitative analysis of inorganic samples,
particularly mineral products, on the basis of information with reference to the array
of atoms in a crystal, crystallite or grain, as available from an X-ray diffractometer.

When struck by X-ray, a reinforced X-ray intensity is detectable in the

vicinity of the crystal, provided that the angle of reflection is equal to the angle of
incidence. The following equation is given :

nλ = 2dsinθ
n : Integer 1,2,3 (1 is applied to a powder and multi-crystal sample)
λ : X-ray wavelength
d : The interplanar spacing
θ : The angle of incidence and reflection

(Preparation of sample)

a. Powder and mass sample

Such samples are placed in a mortar and ground to extremely small particles by
a vigorous back-and-forward motion of a pestle across the mortar. Strong hand
pressure and diligence in grinding at this point are essential for preparing small
particles, since insufficient guiding of the sample causes line broadening. The
sample powder is hand-pressed to an aluminium plate or a glass sample plate.

b. Metal sample

The surface of a metal sample is smoothed and flattened by polishing; it is then

cut to an appropriate size to fit an aluminium plate.

(Analysis of data)

Data from the X-ray diffractometer scan for a sample are compared to
standard patterns. The following reference source is widely used in Customs
laboratories :

The Joint Committee for Powder Diffraction Standards (JCPDS) Powder

Diffraction File

The matching of line positions and relative intensities between the sample
and a standard pattern makes it possible to identify the sample. In the case of
mixtures, overlapping X-ray diffractometer scans are observed, except where there
is formation of a solid solution.

Application : Qualitative analysis of mineral products, ores, slags, inorganic

chemicals, textiles, metals, fertilizers, etc.

7.13.2. Mass spectrometry (MS)

This is one of the most useful techniques for identifying molecular structure,
especially molecular weight, in Customs laboratories. Since this technique is very
sensitive, very small amounts of sample can be employed to identify the molecular
structure. It can also be incorporated with a gas chromatograph (GC-MS). GC-MS
is one of the most useful instruments for identifying each component in a complex
sample, drugs, etc.; however it is expensive and the maintenance is difficult. GC-

I/C1/7/33
 MS equipped with a library data system is recommended, since that makes it
possible to identify each peak in a sample automatically and very quickly.

In high-vacuum conditions, volatilized molecules in a sample are bombarded

by high energy, e.g., a beam of electrons (usually 70 eV; EI method), to form
molecular ions (radical cations/anions), some of which are then fragmented into
smaller ions or radical ions (fragment ions). These ions are then separated
according to their mass-to-charge ratio (m/z) by means of electronic and magnetic
fields (e.g., a high-resolution double-focusing mass spectrometer), and detected in
proportion to their relative abundance. A quadrupole mass analyser is also
commercially available at a reasonable cost. Observed data (mass spectrum) are
displayed or plotted as relative abundance versus mass-to-charge ratio. These
fragmentation patterns provide detailed information with reference to molecular
structure.

(Ionization method)

The electron impact (EI) method is widely used. The chemical ionization
(CI) method, field ionization (FI) method, secondary ion mass spectrometry (SIMS),
etc., are employed to determine the molecular weight of unstable or non-volatile
substances.

(Introduction of sample)

a. Direct inlet (DI) method

A very small amount of non-volatile liquid or solid sample is placed on the end of
a probe and the probe is directly inserted into an ionization chamber. The
sample is vaporized and ionized in the ionization chamber.

b. Gas chromatography-mass spectrometry (GC-MS) method

GC-MS uses a mass spectrometer incorporating a gas chromatograph and is

one of the most useful methods for identifying each component of a complex
sample.

The nature of the components in the sample (e.g., boiling point, whether
non-volatile components are included, etc.) should be investigated in advance and,
after GC analysis, a GC-MS analysis should be carried out in the same conditions.
A 10 - 100 mg sample is dissolved in 1 ml of a suitable solvent (e.g., diethylether).
0.01 - 1 µl of the solution is injected into a GC with a micro-syringe. Each
component reaches the ionization chamber separately and is ionized. Ionized
molecule ions and fragment ions are detected in a detection chamber. A total ion
chromatogram, which is similar to a gas chromatogram, is initially displayed/plotted
and a mass spectrum of each peak can automatically be displayed/plotted.

(Analysis of data)

The highest ion in a mass spectrum generally corresponds to the molecular

ion; however, no molecular ion is observed in the case of an unstable molecular ion.
Since the fragmentation patterns are usually characteristic of types of compounds,
identification is obtained by a comparison of the mass spectrum determined and
reference/standard spectrum under the same conditions.

I/C1/7/34
 Application : Qualitative analysis of organic samples, such as alcohols, saccharides
(TMS), petroleum oils, volatile chemicals, medicaments, essential oils, perfumeries,
fungicides, oligomers, especially drugs, and aromatic components in food
preparations, beverages and spirits, etc.

7.13.3. Nuclear Magnetic Resonance (NMR) spectrometry

This is one of the major techniques for the study of the molecular structure
of organic samples in Customs laboratories. The necessary instrument is very
expensive and difficult to maintain; however, NMR is probably the best means of
analysis and identification of complex molecular structures.

NMR is employed with atomic nuclei which have angular momentum, e.g.,
1
H, 13C, 31P, etc. For example, three different types of information, i.e., chemical
shift, spin-spin coupling and peak area (quantitative determination), are available
1
from a H-NMR spectrum. Since the information is characteristic of the type of
molecular structure, NMR is an excellent analytical technique to identify the
structure of organic substances.

A deuterated solvent (e.g., deuterated chloroform or deuterated water) is

generally employed to dissolve the sample as an external lock for the NMR signal.
Tetramethylsilane (TMS) is widely used as reference for comparing chemical shift;
its chemical shift is defined as zero. A 1-5 % solution of the sample is placed in a
sample tube (e.g., 5 mm in diameter) and the sample tube is placed in a magnetic
field; the NMR spectra can then be determined.

Application : Qualitative and quantitative analysis of saccharides, petroleum oils,

organic chemicals, medicaments, fungicides, oligomers, polymers, drugs, etc.

7.13.4. Electron microscope analysis

Electron microscopes have a wide range of magnification (20 X to 100,000

X) and provide information such as particle size, shape and texture of solid
materials. Observation of the surface of samples enables analysts to identify the
nature of each sample, its processing condition, etc.

There are several types of electron microscope available, e.g., the

conventional transmission electron microscope (CTEM), the scanning electron
microscope (SEM) and the scanning transmission electron microscope (STEM).
Secondary electrons, which are excited by the primary electron beam from a
source, are collected and amplified. An image of the sample surface is generated
by scanning with the primary electron beam and is displayed on a cathode ray tube
(CRT).

A mass sample is cut to a square piece (e.g., 1 cm × 1 cm), taking care not
to damage the surface to be scanned. Other types of sample (e.g., powders,
particles or crystals) are mounted on a supported holder, after preparation of
carbon or metal evaporated films only for the non-conductive sample. The sample
holder is placed on a mounting stage for analysis.

Application : Surface analysis of mineral products, ores, slags, inorganic and

organic chemicals, starches, textiles, plastics, raw hides and skins, leathers,
furskins, wood articles, precious stones and metals, drugs, etc.

I/C1/7/35
 7.14. Other

An elemental analyser (C,H,N,O), a densimeter/pycnometer, a thermal analyser,

a surface tension meter (see Chapter 34, Note 3), a melting point analyser, a
refractometer, etc., are also employed in Customs laboratories.

I/C1/7/36
8. Preparation of laboratory worksheet and laboratory report

8.1. Records

A bound notebook should be used in the Customs laboratory. All data,

calculations and results should be recorded during the actual experiment or later the
same day in a manner readily understandable to all.

It is usually recommended that any relevant notes and comments be written in this
notebook for further reference.

Laboratory notebooks constitute original data, which are important to keep,

especially for cases where the Customs laboratory report is disputed. Reference is
made to them on laboratory worksheets and laboratory reports. They must therefore be
systematically labelled (e.g., with a code consisting of the laboratory room number or
the analyst's abbreviated name and a sequential number). Old laboratory notebooks
should be stored in a central location.

8.2. Reporting results

On the basis of experiment data, reference data and calculation results, an

accurate, detailed and understandable laboratory worksheet and report should be
prepared for each sample analysed, in accordance with sections 8.3. (Laboratory
worksheet) and 8.4. (Laboratory report).

Original data sheets with details of the experiment conditions, a photograph,

calculations, reference data, etc., should be appended to that report.

8.3. Laboratory worksheet

After completion of the analysis, a laboratory worksheet and a laboratory report

should be produced for each sample tested.

The following information should appear on the laboratory worksheet :

(1) Relationship to any previous sample analysed by the laboratory.

(2) Product description (physical appearance, any significant markings or packaging,

the preparation of the analytical sample, etc.).

(3) Relevant excerpts of information from the manufacturer or importer.

(4) All analyses performed on the sample data analysis and the results of the analyses,
whether positive or negative (e.g., physical properties, chemical name, chemical
structure, chemical composition, key components of mixtures, type of polymer,
textile or paper, where relevant).

(5) Any other factual information that is relevant to the classification of the goods or to
any other question raised.

(6) Additional background information, e.g., encyclopedia references, journal articles.

(7) Comparison with similar products previously analysed by the laboratory.

I/C1/8/1
 (8) Interpretation of data, conclusions and a brief rationale for opinions and
conclusions.

(9) Reference to any supporting information in texts, encyclopedias, journals, etc.

The laboratory worksheet should be filed in such a way that it can be easily
retrieved. This may be facilitated by storing the information on a computer. It is
important that all work data are accessible to the reviewer in the event of a question so
that the entire sequence of work can be reconstructed later, if necessary. Calculations
must also be clear, with all equations stated (results must be reported only to a number
of significant digits justified by the accuracy and precision of the method).

Typing errors may occur when transferring data and results to a laboratory
worksheet or a laboratory report. Data stored on a computer may accidentally be lost
and, if no special precautions are taken, data may easily be altered on a computer
without allowing the detection of such changes at a later stage. It is therefore essential
to print out all instrumental analyses. Laboratory worksheets and reports should always
contain a reference to where the original data can be found.

8.4. Laboratory report

The formal typed laboratory report is the end product of all laboratory work and
therefore must be complete and accurate.

The following structure is recommended for laboratory reports :

(1) Name of Customs laboratory

(2) Series number and date of the report

(3) Name of the client

(4) Name and number of the sample

(5) Information related to the need of the Customs officers.

(6) Opinions and conclusion of the technical work performed by the analyst, with
explanations.

(7) Signature and title of analysts accepting technical responsibility for the test report
and date of issue.

(8) Reference as to where the original data can be found.

I/C1/8/2
9. Quality assurance

9.1 Introduction

One of the main purposes of a Customs laboratory is to produce high-quality

analytical data through the use of analytical measurements that are accurate,
authorized and adequate for Customs purposes. To achieve this objective, the
laboratory's activities must be carried out in a cost-effective manner under a planned
and documented quality system.

Insufficient attention to the quality of the work product often causes serious
deficiencies in Customs laboratory operations. Controls and checks are necessary to
ensure quality. These entail not only a thorough knowledge of the Customs laboratory's
purpose and operation, but also a dedication to standards of excellence on the part of
the supervisory and analytical staff.

Since Customs laboratory reports may be used before the courts, they must be
not only scientifically credible, but also legally defensible. To achieve this, Customs
laboratories will find it necessary to operate with a quality assurance system that
includes extensive documentation of their activities.

The United States Federal Register's "Good Laboratory Practice Regulations" (21
CFR Part 58), European Standard EN 45001, the OECD's "Principles of Good
Laboratory Practice", etc. (see III, Chapter 1 : International standards and methods)
would be extremely useful when drafting an implementation plan for a quality assurance
system in any laboratory.

9.2 Quality assurance programme

Personnel, laboratory design, management of equipment and supplies, training of

staff, safety and antipollution measures and sampling are documented in detail in other
draft sections.

9.2.1. Objectives of a quality assurance programme

The main objectives of a quality assurance system in Customs laboratories are

as follows :

- To facilitate uniform application of the Harmonized System.

- To facilitate enforcement activities.
- To develop the quality of Customs laboratory practices and operations.
- To establish or identify authorized and reliable methods for Customs purposes.
- To produce reliable and accurate analytical results by using authorized and
reliable analytical methods.
- To maintain a continuing assessment of the quality of data reported by analysts.
- To achieve high-quality Customs laboratory performance in a cost effective
manner.
- To improve sample and record handling.
- To carry out safety and anti-pollution measurements.
- To carry out safe operating practices.
- To give appropriate training.

I/C1/9/1
 9.2.2. Quality assurance committee

A quality assurance committee must develop a quality assurance plan and

achieve the objectives of the quality assurance programme. The committee is
composed of representatives from the supervisory and analytical staff, preferably
with a quality assurance co-ordinator serving as a chairman of the committee.

First and foremost, the committee examines and evaluates laboratory activities
in terms of the following quality assurance elements :

- Programme objectives.
- Work planning for quality.
- Organizational structure.
- Policy of management.
- Laboratory design.
- Procurement of laboratory facilities.
- Supplies' management.
- Equipment maintenance.
- Safety and anti-pollution measurements.
- Training of staff.
- Sampling.
- Sample and data handling.
- Personnel practices.
- Customs laboratory operations.
- Standards and methods employed in Customs laboratory (selection and
evaluation).
- Reporting procedures.
- Technical literature and reference books.
- Statistical procedures.
- Audit procedures.
- Evaluation of costs and benefits for laboratory performance.
- Improvement of the quality assurance programme.

The committee develops quality assurance requirements on the basis of its

findings and it documents quality assurance procedures to meet its requirement.
The committee is important for ensuring that laboratory staff are properly involved in
the planning and development stages of the programme.

The committee decides on the format of a quality assurance manual and

assigns the writing of various sections to competent individuals. Every quality
activity, such as policies, organizational objectives, functional activities, etc., is to be
documented in this manual. Each section of the manual is discussed and modified, if
necessary, by the committee. The latter implements the programme, monitors it and
make changes, if necessary, to achieve the quality goals set for the operation of the
system. All activities should be documented.

9.2.3. Statistical applications

9.2.3.1. Treatment of scatter

To obtain reliable analytical results, chemists usually divide a sample into

several test samples and then analyse each of these; they repeatedly determine the
end points of test sample solutions in titration analysis. Some scatter of analytical
data based on unavoidable error and essential variation is normally allowed for.
Variation of analytical data based on random errors usually shows the normal
I/C1/9/2
distribution around a true value. However, the distribution of analytical data
sometimes shifts to one side or the other, due to specific factors such as
determinate errors (instrument errors, operational errors, method errors, etc.).

Treatment of analytical data should be carried out on the basis of statistical

procedures. For example, the average x of a series of values x1, x2,...., xn, is
obtained simply by adding all the individual values and dividing the sum by the
number of values n.
Σnx x1 + x2 + ..... + xn
x = ____ = _______________
n n
It is important to know the degree of scatter and the most widely used
measures for determining scatter are as follows :
2
The sample variance : V = Σ(xi - x) / (n - 1)

The standard deviation : σ = (V)1/2

The coefficient of variation : CV = (σ/x) x 100 (%)

On the basis of the measurement of scatter, whether certain analytical data

fall within a certain distribution (e.g., confidence limit) should be considered from
the standpoint of probability.

The precision of a measurement can be improved by increasing the number

of observations. When a chemist performs a series of replicate analyses, one of
the results sometimes deviates considerably from the others. In that case, a
decision has to be taken as to whether the results should be rejected or retained.
Statistical application is one useful means to determine whether the scatter of
analytical data is based on unavoidable error and essential variation or significant
errors in analytical technique.

The significance of σ in relation to the normal distribution curve is shown in

Figure 1. The mathematical treatment from which the curve was derived shows
that 68 % of the individual deviations fall within one standard deviation from the
mean x, 95 % are less than twice the standard deviation, and 99 % are less than
2.5 times the standard deviation. Consequently, 68 % of the individual values will
fall within the range x ± σ, 95 % will fall within x ± 2σ and 99 % will fall within x ±
2.5σ. The normal distribution curve assumes no determinate errors, but only
random errors. Determinate errors, in practice, shift the normal curve from the true
value.

I/C1/9/3
 Probability of occurrence

99 %

95 %

Frequency
58 %

x - 2.5 σ x-2 σ x -σ x x- σ x+2 σ x - 2.5 σ

Magnitude of deviation

Figure 1 Normal error curve

A control chart is one of the most useful statistical tools in the quality
assurance programme and is

+3σ

+2σ
♥
σ
♥ ♥ ♥
♥ ♥
♥
♥ ♥
♥
σ
- 2σ

- 3σ

1 2 3 4 5 6 7 8 9 10

Date

Figure 2 Example of control chart

frequently used for routine analysis. An example of a control chart is shown in

Figure 2. The control chart consists of a centre line representing the known and
assumed value of the control and one or two pairs of limit lines, the inner and outer
control limits.

Day-to-day results of the analysis are plotted on the chart to ascertain

whether the analysis is in the range of statistical control.

For a detailed description, professional literature and publications (e.g., ISO

Standards 2602, 2854, 3207, 3301, 3494, 3534, etc.) should be consulted.

I/C1/9/4
9.2.3.2. Significant figures

Digit treatment of data corresponds to the purpose of the experiment and the
analytical accuracy of the instruments used. For example, chemists can read 10 %
of the minimum scale in the case of analog-type instruments.

In a calculation process of addition or subtraction, a standard digit is the

maximum one (see Example 1). In the case of multiplication or division, the
accuracy of the results is controlled by the most inaccurate digit (see Example 2).

Example 1
207
20.7
+) 12.8
_________
240.5

Example 2

2.3 × 0.71 = 1.633

The figures underlined are indefinite and they are rounded off.

If the digit following the last significant figure is greater than 5, the number is
rounded up to the next higher digit. If it is less than 5, the number is rounded down
to the present value of the last significant figure :

240.3 Þ 240
240.7 Þ 241

If the last digit is a 5, the number is rounded off to the nearest even digit :

240.5 Þ 240
241.5 Þ 242
249.5 Þ 248

However, if there is another digit following the 5, the figure is rounded off as
follows :

240.50 Þ 240
240.51 ~ 240.59 Þ 241

9.2.3.3. Handling of analytical data

It is important that analytical data be arranged in such a way as to produce an

effective and successful conclusion, which can be widely applied. Tables, graphs
and mathematical treatment are effective means of achieving this.

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 (a) Table

A table indicates a qualitative relationship. Contents are expressed according

to size against analytical conditions and the placing of the decimal point is
important.

(b) Graph

When chemists set out analytical data in a graph, the relationship between
variables becomes apparent. The results can be recorded on section paper,
semi-logarithmic graph paper, log-log graph paper, etc. If analytical data give
linear plots, chemists can estimate the analytical value of an objective
component by extrapolation and intrapolation. On the basis of a slope of
calibration curve (a) and intercept of y axis (b), the chemist can give
coefficients of the analytical equation. The analytical results correspond to the
following equation :

y = ax + b

(c) Mathematical treatment of analytical data

It is desirable to produce an analytical equation from the analytical results. An

analytical value (differential value, integral value, etc.) is directly calculated
from the equation and the phenomenon in experiment is accurately expressed
in the form of the equation both qualitatively and quantitatively.

The linear equation above is one of functions. The method of least squares is
widely known to give the best straight line through a series of analytical results.
The best straight line occurs when the sum of the squares of the deviations of
the data from the line are minimum. Calculations of a and b are made as
follows :
Σ(xi - x)(yi - y) Σxiyi - [(Σxiyi)/n]
a = ____________ ≈ ______________
2
Σ(xi - x) Σxi - [(Σxi)2/n]

b = y - ax

Where x is the mean of all values of xi and y is the mean of all values of yi, and
n is the number of the data points.

If the analytical results do not give straight plots, the chemist must find a simple
function which fits with the calibration curve of the analytical data.

9.2.4. Quality control of qualitative analysis

Qualitative analysis is as important as quantitative analysis for a Customs

laboratory. The key purpose of qualitative analysis is to identify clearly the kind and
structures, etc. of the components in a sample.

In parallel with testing or determination of the sample, the analyst usually

carries out control and blank tests under the same conditions, to ensure the detection
of the target substance. However, there are many substances which show the same
colouring reactions (e.g., colouring tests, etc.), Rf values (thin-layer chromatograms

I/C1/9/6
 (TLC)), retention times (e.g., gas chromatograms (GC), high-performance liquid
chromatograms (HPLC), etc.), spectra (e.g., ultraviolet and visible (UV-VIS), mass,
infra-red (IR) spectra, etc.), etc.

Consequently, the analyst usually carries out double or triple checks using
other techniques (e.g., other colouring agents, other columns, other mobile phases,
etc.).

Attention must also be paid to detection limits and sensitivity. The detection
limit is generally defined as the quantity (or concentration) required to give a signal
equal to three times the standard deviation of the blank. Sensitivity is also defined as
the quantity (or concentration) required to give a certain intensity of colouring
reaction, spot, peak, etc. In the case of too diluted a sample solution or an
insensitive detection method, the reaction or determination tends to produce a
negative result. Consequently, it is important to prepare a sample solution in an
appropriate concentration and to use highly sensitive detection methods for each
component in the sample.

9.2.5. Sampling

It is extremely important to collect representative samples from many types of

shipments at the examination stage and to prepare a test sample for analysis in the
Customs laboratory with the minimum composition change, as described in the
section on "Sampling".

In order to accomplish these procedures safely and consistently, a sampling

plan should be prepared, developed and documented for the various types of goods
traded, covering delivery of the samples to the Customs laboratory and production of
samples for analysis as well as sample storage and disposal. Laboratory staff should
be included in the discussions.

To ensure correct sampling and sample preparation and to avoid unnecessary

repetitive analyses, good communication is necessary between the clearance or field
officers and the laboratory staff.

9.2.6. Audit procedure

A Customs laboratory should include performance and system audits in its

quality assurance programme.

The performance audit is to examine and evaluate the overall analytical

activities of the analysts; it should include worksheet or notebook review, field analyst
work review, the duplication of sample analysis, and intra- and inter-laboratory
comparisons.

The system audit is a field inspection or assessment of the laboratory's control

system and should be well-planned and conducted by a trained audit team in order to
enhance the quality of the laboratory's activities.

Qualified persons, who are familiar with the quality assurance programme and
are skilled scientists, should be selected and trained as auditors.

The following items should be examined and evaluated by the audit team :

- Performance of quality assurance activities.

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 - Confirmation of reliability of analytical methods.
- Sample analysis and analytical reporting procedures.
- Safety and anti-pollution measurement.
- Sample and data handling.
- Management and procurement of laboratory facilities and supplies.
- Staff training and evaluation, etc.

After the audit has been completed, provisional recommendations to enhance

the quality of the laboratory's activities are made by the audit team to the assigned
staff and the laboratory director. The provisional recommendations should be
discussed at a meeting to avoid any problems or misunderstanding.

The audit report should point out imperfections in laboratory activities and
recommend corrections (e.g., changes in laboratory procedures, improvement or
purchase of laboratory facilities, need for staff training, etc.).

A draft report should be prepared as soon as possible and be submitted to the

laboratory for review and checking of its factual accuracy, in advance. After any
corrections have been made to the report, the final version should be submitted to
management and appropriate action should be taken on the basis of the report's
recommendations.

9.2.7. Inter-laboratory comparison

Intra-laboratory checking sometimes does not produce sufficient conclusions

for evaluating and upgrading the Customs laboratory's performance. In such cases,
inter-laboratory comparison may be useful. The main objectives of this are as follows
:

- To develop analytical techniques among laboratories.

- To confirm the reliability of analytical methods.
- To examine the grade of standard materials or chemicals, including reliability.
- To highlight the laboratory's particular capabilities.
- To exchange technical information.
- To investigate optimum analytical methods, such as official analysis methods.
- To facilitate international trade through the acceptance of analytical data.

When carrying out this type of activity, international standards (e.g., ISO 5725,
10011-1, 10011-2, 10011-3, etc.) could be extremely useful.

I/C1/9/8
Chapter 2 : Laboratory equipment, instruments and apparatus

INTRODUCTION

Set out below are tables listing various equipment, instruments and apparatus
needed for a Customs laboratory. The tables are divided into three groups :

- Basic equipment, instruments and apparatus

- Special instruments and apparatus required for HS classification

- Other instruments and apparatus which may be needed in an advanced Customs

laboratory.

The number of items of equipment, instruments or apparatus required depends, of

course, on the number of analysts working in a laboratory. For the purposes of these
tables it has been assumed that a standard Customs laboratory employs 12 analysts.

This Chapter of the Customs Laboratory Guide also contains a section on

instrument maintenance, etc.

Note)

"*" indicates basic equipment or apparatus which is essential to start up a Customs

laboratory. The number of items, given in brackets following the "*", is the minimum
and more will be required depending on the size of the Customs laboratory.

"**" indicates essential instruments to start up a standard Customs laboratory, and

equipment or apparatus used with those instruments. The number of items (the
minimum) required are given in brackets following the "**".

The ability of a developing country's Customs laboratory to purchase instruments,

equipment and apparatus will depend on its resources. Basic items should be
purchased to establish a minimum capability dependent on the types of analyses
required. Additional supplies should only be purchased as workflow dictates or where
experience shows them to be necessary.

° °

I/C2/9
CLG/AS 1-Sep. 2002

1. Basic equipment, instruments and apparatus

1.1. Basic equipment

Equipment Number (for a Remarks

laboratory of
12 chemists)

Chemical experimental table 6 * (1)

Physical experimental table 9 * (1)
Balance table 6 * (1)
Storage cabinet, normal type 3 * (2)
Storage cabinet, safety type 6 * (1)
Fume cupboard 6 * (2)
Air conditioner 1 For infra-red room** (1)
Sink 6 * (2)
Chair, for laboratory 20 * (5)
Office table and chair 12 * (3)
Fire extinguisher 6 * (2)
Emergency shower 2 * (2)
Eyewash station 2 * (1)
Refrigerator 1 For storage of samples, reagents, etc.*
(1)
Alarm 6 * (2)
First-aid box 1 * (1)
First-aid medicines 1 set * (1)
Cylinder 10 H2, O2, N2, He, etc.** (4)
Bookshelf 3 * (2)

I/C2/10.
1.2. Glassware

Glassware Number Remarks

Beaker 10 ml 30
20 ml 30
50 ml 250 * (30)
100 ml 360 * (30)
200 ml 60 * (10)
300 ml 30
500 ml 15 * (2)
1000 ml 6 * (1)
2000 ml 5
Conical beaker 200 ml 60 * (5)
300 ml 30
500 ml 10
1000 ml 5
Tall beaker 100 ml 15 * (5)
200 ml 15
Erlenmeyer flask 10 ml 15
50 ml 150 * (10)
100 ml 250 * (15)
200 ml 150 * (10)
300 ml 30
500 ml 15 * (5)
1000 ml 6 * (1)
2000 ml 5
Filtering flask 300 ml 3 * (1)
Long-neck Kjeldahl flask 200 ml 30 * (3)
Round-bottom flask 50 ml 10
100 ml 20 * (2)
200 ml 10 * (2)
500 ml 10
1000 ml 5
Short-neck Kjeldahl flask 10 ml 20
25 ml 10 * (5)
50 ml 10 * (5)
100 ml 20 * (5)
200 ml 10
500 ml 10
1000 ml 5
Volumetric flask, clear 10 ml 30
25 ml 30
50 ml 30 * (5)
100 ml 90 * (10)
200 ml 15 * (5)
250 ml 15 * (5)
500 ml 9 * (1)
1000 ml 9

I/C2/11
 Glassware Number Remarks
Volumetric flask, amber 50 ml 30
100 ml 30 * (5)
250 ml 30
500 ml 10
Culture dish 30 * (2)
Graduated cylinder 10 ml 15
25 ml 15 * (2)
50 ml 15 * (2)
100 ml 15 * (2)
250 ml 6
500 ml 6
1000 ml 6
Colour comparison 30 ** (5)
Watch glass 60 mm 30 ** (5)
120 mm 30
Centrifuge vessel 10 ** (6)
Dropping bottle with bulb and pipette 15 * (5)
Drying tube, straight 10 * (2)
U bend 10
Reagent bottle, narrow mouth, amber 60 ml 30
250 ml 30 * (10)
500 ml 30
Reagent bottle, wide mouth, plain 30 ml 15
120 ml 15 * (5)
500 ml 15
Reagent bottle, narrow mouth, plain 60 ml 30
250 ml 30 * (10)
500 ml 30
Reagent bottle, wide mouth, amber 30 ml 15
120 ml 15 * (5)
500 ml 30
Specific gravity bottle 6 * (2)
Specimen bottle 200
Test tube 18 mm 1500 * (100)
30 mm 75
Vial, with polyethylene stopper 300
Weighing bottle 30 x 30 mm 30 * (3)
40 x 40 mm 30
Burette, plain 10 ml 6
plain 50 ml 6 * (2)
amber 10 ml 6
amber 50 ml 6

I/C2/12
 Glassware Number Remarks
Measuring pipette 1 ml 30 * (3)
2 ml 30 * (3)
5 ml 30 * (3)
10 ml 30 * (3)
Volumetric pipette 0.5 ml 6
1 ml 60 * (6)
2 ml 60 * (6)
3 ml 30 * (3)
4 ml 4
5 ml 30 * (3)
10 ml 30 * (3)
15 ml 6
20 ml 30 * (3)
25 ml 30 * (3)
30 ml 9
50 ml 15 * (1)
100 ml 15
Komagome pipette 1 ml 12
2 ml 12
5 ml 12 * (2)
10 ml 12
Desiccator, plain 150 mm 12 * (2)
plain 300 mm 3
amber 300 mm 3
Desiccator plate 150 mm 12 * (2)
300 mm 6
Developing vessel (large size) 3 For TLC (thin-layer
chromatography)* (2)
Developing vessel (small size : sample bottle) 5 For TLC* (2)
Capillary, disposable 3,000 For TLC* (100)
Nebulizer, amber 30 For TLC* (3)
Developing vessel 3 For PC (paper
chromatography)
Filtering funnel, long stem
45 mm 15
75 mm 30
Filtering funnel 30 mm 30
75 mm 90 * (10)
120 mm 30
180 mm 15

I/C2/13
 Glassware Number Remarks
Glass funnel, cylindrical type, fused-in fritted glass disc
(30 ml) G0 6
G1 6
G2 15
G3 6
G4 6
G5 6
Separating funnel 50 ml 15
100 ml 30 * (5)
300 ml 15
500 ml 10
1000 ml 6
Aspirator 9 * (2)
Condenser (Liebig) 5 * (2)
Glass tubing 1.2 m 60
Glassware for soxhlet extraction 6 * (2)
Glassware for distillation 6 * (2)
Quartz cuvette (6 pairs) 12 For UV-VIS (Ultraviolet and
visible) spectrophotometer**
(1)
Vessel for quartz cuvette 2 For UV-VIS spectro-
photometer** (1)
Chromatographic column with stopcock 10 For column chromatography*
(3)
Glass wool 1 For GC (gas
chromatography)** (1)
Glass insert 12 For GC** (3)
Glass column 50 cm 10 For GC
1m 10
2m 20 ** (6)
4m 10
Glass syringe 1 ml 6 ** (2)
2 ml 6
5 ml 6
10 ml 6
Stopcock 60
Glass stirring rod 20 * (2)
Cover glass 3,000 For microscopes** (300)
Slide glass 1,500 For microscopes** (100)
Spherical ampoule 10

I/C2/14
1.3. Rubber and plastic ware

Laboratory ware Number Remarks

Beaker, polypropylene 50 ml 15
300 ml 15 * (2)
1000 ml 6
Rubber tube :
Presser, endurable type 30 m For evaporators** (3)
Presser, endurable type
(wire reinforced for hydraulic type) 10 m For analytical equipment

Silicone rubber type 30 m

For gas 10 m For H2, N2, O2, C2H2, Ar(He)

Black or yellow rubber for laboratory use 50 m Diameters should be suitable

for glass tubes
Rubber bulb for measuring pipette 1 ml 30
2 ml 30
5 ml 30 * (3)
10 ml 30
Rubber stopper :
For test tube, small Erlenmeyer flasks and
reagent bottle (narrow mouth) 600 * (6)

For large Erlenmeyer flasks and reagent bottle

(wide mouth) 24
Silicone rubber stopper, small 180
Centrifuge vessel 10 ** (3)
Reagent bottle 50 ml 60
(polyethylene) 500 ml 90
Specimen bottle 300
Washing bottle 500 ml 30 * (2)
Graduated cylinders, polypropylene 10 ml 6
50 ml 6
Measuring pipettes, polyethylene 1 ml 30
5 ml 30
Pipette washer 3
Disposable plastic syringe 5 ml 250 Per year
10 ml 250 Per year
50 ml 250 Per year
Spoon, plastic 12 * (3)
Rubber bulb 12
Disposable gloves 500 Per year* (50)

I/C2/15
 Laboratory ware Number Remarks
Gloves, anti-acid 12
Protection gloves 5
Desiccator of plastics, box-type 3 For TLC* (1)
Septum 26 For GC** (6)
Column case 2 For GC** (1)
Pipette case 3 * (1)
Pipette controller 5 * (2)
Teflon seal tape 10 * (2)
Chemical structures (model) 1 set
Trough 12

I/C2/16
1.4. Other laboratory ware and utensils

Laboratory ware Number Remarks

Evaporating dish, porcelain
20 ml 30
50 ml 30
120 ml 30 * (3)
400 ml 6
Porcelain crucible and lid 10 ml 600
Disposable aluminium 126 Per year
weighing/evaporating dish
Zirconium, vitreous carbon or alkali-resistant sintered
alumina crucible 30 ml 5
Porcelain funnel, Büchner type
55 mm 6
90 mm 6 * (2)
150 mm 3
Cork stopper :
For test tube, small Erlenmeyer flask and reagent bottle
(narrow mouth) 600 * (50)
For large Erlenmeyer flask and reagent bottle (wide
mouth) 50
Cork borer 3 * (1)
Cork press 3 * (1)
Cork ring 100 ml 10 * (1)
200 ml 10
300 ml 10
500 ml 10
Filter paper, for quantitative test 55 mm 1,500 * (100)
90 mm 6,000
150 mm 3,000
Filter paper, for quantitative test Ash content
Quick filtering 90 mm 300 0.09 mg/piece
Ordinary use 90 mm 1,500 0.09 mg/piece
Fine particles 90 mm 3,000 0.09 mg/piece
Ordinary use 90 mm 1,500 0.09 mg/piece
Thimble filter paper 750 For soxhlet extractors* (70)
Litmus paper 10 * (2)
Micro-dispenser 100
Powder paper, small 30,000
large 30,000
Section paper 5 * (1)
Semilogarithmic graph paper 2

I/C2/17
 Laboratory ware Number Remarks
Log-log graph paper 2
Burette clamp, double 5 * (1)
Clamp, small 12
large 24
Clamp holder 20
Clamp for glassware joint 120 * (10)
Clamp for test tube 60 * (6)
Mohr clamp 60 * (6)
Pinchcock clamp 10
Rod or pipe connector 48
Clay triangle 10
Open ring support 50 mm 6
90 mm 6 * (2)
150 mm 3
Test tube holder 10 * (1)
Tripod 15 * (1)
Wire gauge, with asbestos 10 * (1)
Rack for test tube, small 12
large 3
Support, small 12 * (1)
large 12
Support for funnel 12
Support, jack, with precise vertical adjustment 5 * (1)
Support for burette 6 * (1)
Support for colour comparison 3
Support for pipette 6 * (1)
Copper wire 3 * (1)
Nichrome wire 3
Platinum wire 1 * (1)
Burner, Bunsen 12 LPG (Liquid petroleum gas)*
(2)
Deep-blue cobalt glass 3
File 6
Label 10 * (1)
Level gauge 50

I/C2/18
 Laboratory ware Number Remarks
Manometer 5
Test sieve 12
Test tube brush 50 * (5)
Thermometer 0 - 360 6 * (1)
20 - 100 6 * (2)
Precision 0 - 100 6

Hygrometer 3
Mortar and pestle, porcelain
60 mm 6
120 mm 9
210 mm 3
Mortar and pestle, agate 50 mm 3
Mortar and pestle, alumina
120 mm 3
Filter paper, for chromatography For PC
2 x 40 cm 300
40 x 40 cm 150
TLC plate, silica gel 10 x 20 cm 12 p. For TLC
20 x 20 cm 30 p. "p." = pack * (3)
cellulose 20 x 20 cm 6 p.

Capillary column 3 For GC** (2)

Stainless-steel column 6 For GC
Column accessories For GC
for glass column 2 set ** (1)
for capillary column 2 set ** (1)
for stainless-steel column 2 set
Column packing kit 1 For GC** (1)
Capillary column holder 3 For GC** (1)
Micro-syringe 1 µl 9 For GC** (2)
2 µl 6
5 µl 6

Press and evacuable die to prepare KBr pellets 1 set For IR ** (1)
Crystal-polishing kit 1 set For IR ** (1)
Blower, foot-powered 3
Clip 10
Forceps, stainless-steel 120 * (5)
Micro-spatula 60 * (6)
Needle for glass syringe 15

I/C2/19
 Laboratory ware Number Remarks
Spoon, stainless steel 60 * (6)
15
Magnetic spin bar 36 ** (3)
Tongs for crucible 210 mm 15 * (3)
450 mm 3
Carrier for laboratory bottles 5
Safety goggles 15 * (2)
Magnetic stirrer 12 ** (2)
Safety ware 25 * (2)
Driver set 1 * (1)
Glass cutter 1 * (1)
Knife 3
Pliers 2
Saw 3
Micrometer, vernier, etc. 1 To determine thickness
Tool kit 1
Tube cutter 1
Vice 2

I/C2/20
1.5. Basic instruments and apparatus

Instruments Main uses

Fourier transform infra-red (FT-IR) Organic, inorganic chemicals, polymers, narcotics
spectrophotometer *
Gas chromatograph * Organic chemicals, petroleum, food, perfumes
Air compressor ** For GC
Vibrator for column packing ** For GC
UV & VIS spectrophotometer * Quantitative measurement for food, chemicals
Emission spectrophotometer Qualitative analysis of inorganic materials
X-ray diffractometer * Inorganic chemicals, minerals
Atomic absorption spectrophotometer * Measurement for content of metals
Accumulator Quantitative analysis of metal, etc. (electrolytic
method)
Hydrometer (1 set) General purpose
pH meter * General purpose
Photometer Quantitative analysis
Polarograph Quantitative analysis of metal, etc.

Potentiometer Quantitative analysis of metal, etc.

Tester General purpose
Melting-point apparatus * Organic chemicals
Petroleum-oil distillator Petroleum oil
Nitrogen analyser system * Foods
Refractometer General purpose
Surface-tension balance * Surface-active agents
Automatic water distillation or Water purify * Purifying water
Electric muffle furnace * Food, inorganic chemicals, minerals
Electric drying oven * General purpose
Vacuum drying oven * Food, plastics or paint
Direct-reading chemical balance * General purpose
Electronic even balance * General purpose
Constant-temperature water bath *
For physical measurements at 15 °C or 20 °C
Oil bath General purpose
Sand bath * General purpose

I/C2/21
 Instruments Main uses
Optical (polarised light) microscope * Food, minerals
Stereo-microscope * Textiles, minerals
Various kinds of electrodes Quantitative analysis of metal, etc.
Centrifuge * Food, paint, other separation
Homogenizer Foods
Mill General purpose
Oxygen burner General purpose
Rotary evaporator * For concentration or evaporation of organic
solvents
Infra-red lamp Evaporation of solvents
Mixer General purpose
Resistance box General purpose
Stopwatch General purpose
Timer General purpose
UV light ** For TLC
Calculator General purpose
Heavy ion eliminator Elimination of heavy metals from effluent

I/C2/22
 CLG/AS 1-Sep. 2002

2. Special instruments and apparatus required for Harmonized System classification

The following instruments and apparatus are necessary for specific methods of
analyses for determining criteria prescribed by the legal texts or the Explanatory Notes of the
Harmonized System. The kinds of instruments and apparatus which need to be installed
may vary from country to country, depending on the volume of trade in the relevant goods,
etc.

It should be noted that many Customs laboratories are not equipped with all of these
instruments and apparatus, because most of them are expensive and may not be frequently
used. Attention should therefore be paid to the cost and benefits when deciding which kinds
of instruments and apparatus are to be procured.

Special instrument and apparatus HS provision

Polarimeter for sugar analysis (saccharimeter) Note 2 (A)(a) to Chapter 11 and Subheading
Note 1 to Chapter 17
Woven metal wire cloth sieves with apertures of Notes 2 and 3 to Chapter 11
315 micrometres, 500 micrometres, 1.25 mm and
2 mm
Thermometer, fixed in a stopper, for Bellier ENs to headings 15.09 and 15.10
reaction
Pressure gauge and thermostat, for determining Subheading Note 1 to Chapter 22
excess pressure of sparkling wines
Distillation apparatus and hydrometer for alcoholic Note 6 to Chapter 20, Note 1 (f) to Chapter 21,
measurement Note 3 to Chapter 22, headings 22.07 and 22.08
Special steam-distillation apparatus for Subheadings 2529.21 and 2529.22
determining fluoride content
Special muffle furnace, silica crucible and silica lid Subheading Notes 1 and 2 to Chapter 27
for coal analysis
Adiabatic bomb calorimeter Subheading Note 2 to Chapter 27

Vacuum distillation apparatus for petroleum Note 2 to Chapter 27 and Note 3 (a) to Chapter 39
products
Distillation apparatus for petroleum products Note 2 to Chapter 27, Note 3 (a) to Chapter 39,
Subheading Notes 3 and 4 to Chapter 27,
subheading 2707.50 and ENs to headings 29.02
and 29.33
Hydrometer for petroleum EN to heading 27.12
Penetrometer, standard cone, etc. EN to heading 27.12
Apparatus for determining oil content in paraffin Subheading 2712.20
wax
Geiger-counter Note 6 (d) to Chapter 28

I/C2/15.
CLG/AS 1-Sep. 2002

Special instrument and apparatus HS provision

Rotational viscometer and dropping point EN to heading 34.04
measuring apparatus
Devices for measuring minimum burst pressure of Subheading 3917.31
plastic tubes, pipes and hoses
Rubber testing apparatus consisting of Note 4 to Chapter 40
- - vulcanizing apparatus
- - test-piece press
- - tensile test machine, and
- - straining device
Elrepho apparatus or other equivalent brightness Note 5 to Chapter 48
tester
Mullen-type bursting tester Note 5 and Subheading Notes 1, 2, 5 and 6 to
Chapter 48
Tear-testing machine and tensile-testing machine Subheading Note 2 to Chapter 48
for paper
CMT 30 crush-resistance tester Subheading Notes 3 and 4 to Chapter 48
Thermohydrostat for producing the standard General EN to Section XI
atmospheres for the conditioning and testing of
textiles
Tensile-testing machine Note 6 and Subheading Note 1 (a) to Section XI,
and subheadings 5607.21 and 5607.41
Straining device for textiles Subheading Note 1 (a) to Section XI
Devices for determining mass per unit length of Section XI
yarn
Devices for determining mass per unit area of Section XI
textiles
Carbon analyser Subheading 6903.10
Equipment for determining the linear coefficient of Subheadings 7002.32, 7013.32 and 7017.20
expansion of glass
Test sieves having mesh apertures of 63 Subheading Note 1 to Chapter 71, Note 8 (b) to
micrometres, 0.5 mm, 1 mm and 5 mm Section XV, Note 1 (h) to Chapter 72 and
Subheading Note 1 (c) to Chapter 79
Carbon and sulphur analyser Chapter 72
Electrolysis equipment Notes 1 (a) and (b) to Chapter 74
Oxygen analyser Subheading Note 1 to Chapter 75

I/C2/16.
CLG/AS 1-Sep. 2002

3. Other equipment, instruments and apparatus which may be needed in a standard and
advanced Customs laboratory

3.1. Equipment

Equipment Number Remarks

Safe 1 For illicit drugs, etc.
Supervision camera 1 set
Harmful-gas alarm detector >10 For each room
Inflammable-gas alarm detector >5 For H2(GC), etc.
Air cleaner 2
Water pure refinery 1
Crusher 1 For sampling conditioning
Vibratory disk mill 1 For sampling conditioning
Driller 1 For sampling conditioning
Saw for metal 1 For sampling conditioning
Pressure regulator to be used with 1 For sampling conditioning
compressed gases
Apparatus and devices for waste 1
treatment
Fume hoods 6 For GPC (gel-permeation chromatography),
etc.
Clean air bench 1
Air conditioner >3 For IR (infra-red), MS (mass spectrometer),
NMR (nuclear magnetic resonance) rooms,
etc.
Freezer 2 For storage of samples, reagents, reference
materials

I/C2/16.
CLG/AS 1-Sep. 2002

3.2. Glassware

Glassware Number Remarks

Beaker 1 ml 15
3-Neck round-bottom flask 500 ml 10
1000 ml 10
Filtering flask 500 ml 5
1000 ml 5
Flat-bottom flask 100 ml 20
200 ml 10
300 ml 10
500 ml 5
1000 ml 3
Short-neck pear flask 10 ml 15
20 ml 15
50 ml 30
100 ml 20
10
200 ml
Distillation flask 30 For automatic (vacuum)
distillation apparatus
Automatic burette 2
Micropipette 10
Pasteur pipette 25
Evaporating dish 50 ml 10
100 ml 25
200 ml 15

Mini petri dish for culture 50

Test tube with stopper 100
Syringe vial 100
Crimp seal vial 100
Desiccator, with socket on the cover 5
Adapter (reducing) 10
(enlarging) 10
(distilling) 10
(straight type), etc. 10

Condenser (tube) 10
(Alihn) 10
(Graham) 10
(Dimroth) 10
Distilling column 5
Bulb (Kjeldahl), long delivery tube, bent 5

I/C2/15.
CLG/AS 1-Sep. 2002

Glassware Number Remarks

Bulb (Kjeldahl) 10
Sample pipette 10 For MS
Tube for auto-collector 100 For GPC
Sample tube 50 For NMR, per year

I/C2/15.
CLG/AS 1-Sep. 2002

3.3. Other laboratory ware and utensils

Laboratory ware Number Remarks

Safe pipette controller 5
Automatic burette (complete set) 5
High-precision tweezers 3
Colony counter 1
Wire basket 5 For autoclave
Dewar container or vessel 5
Flexible heating ribbon 3
Laboratory shelf 5
Diamond scriber 1
Sealon film 5 Per year
Screw-cap vial 1 ml 300 Per year
2 ml 100 Per year
5 ml 100 Per year
10 ml 50 Per year

Air-tight syringe 5 For GC

Foil for pyrolyser 10 For GC
Column for GC-MS (gas chromatograph/mass 5
spectrometer)
Column accessories for GC-MS 5
Vacuum vial 50
Rubber stopper 100 For seal vial
Crimp cap (aluminium) 100 For seal vial
Plier-type decapper 2 For seal vial
Hand-operated aluminium cap crimper 2 For seal vial
Seal vial 1 ml 100 For GC and HPLC (high
2 ml 50 performance liquid
5 ml 30 chromatography), etc.
10 ml 30

Column accessories for HPLC 10

Column for HPLC 10
Guard-column for HPLC 10

I/C2/15.
CLG/AS 1-Sep. 2002

Laboratory ware Number Remarks

Micro-syringe 2 µl 2 For HPLC
5 µl 5
10 µl 2
25 µl 2
Disposable plastic syringe For HPLC, etc.
10 ml 100 Per year
25 ml 100 Per year
50 ml 100 Per year
Micro-filter for micro-syringe For HPLC
0.10 µm 1000 Per year
0.20 µm 1000
0.45 µm 1000
(water and anti-water types)
Micro-filter 0.10 µm 100 For HPLC
0.20 µm 100 Per year
0.45 µm 100
(water and anti-water types)
Filter holder 2 For HPLC
Sample table 30 For SEM (scanning
electron microscope)
Film 50 For SEM
Printing photographic paper 100 For SEM
Aluminium pan, disposable 100 For thermal analyser
Platinum pan 5 For thermal analyser
Cathode lamp 1 set For AAS (atomic
absorption
spectrometer)
NMR tube rack 3 For NMR
Cap for sample tube 20 For NMR
Diskette 100 For computer

I/C2/15.
CLG/AS 1-Sep. 2002

3.4. Instruments and apparatus

Instruments Main uses

Auto-sampler system for GC Organic chemicals, drugs, essential oils, etc.
Pyrolyser system for GC Polymers
Gas chromatograph/mass spectrometer (GC-MS) Organic chemicals, essential oils, drugs, etc.
Secondary ion mass spectrometer (SIMS, etc.) Organic chemicals, polymers, etc.
High-resonance inductively-coupled-plasma/mass Inorganic materials
spectrometer (ICP-MS)
Liquid chromatograph/mass spectrometer (LC- Organic chemicals, drugs, etc.
MS)
Gas chromatograph/Fourier transform infra-red Organic chemicals, drugs, essential oils, etc.
spectrophotometer (GC-FT-IR)
Super-critical fluid chromatograph Organic chemicals
High-performance liquid chromatograph (HPLC) Organic chemicals, drugs, oils, saccharides, etc.
Ion chromatograph Inorganic chemicals
Fully-automated amino acid analyser Amino acid, foods
Gel-permeation chromatography (GPC) Organic chemicals, polymers
Fourier transform infra-red spectrophotometer General purpose
Raman spectrophotometer Organic and inorganic chemicals
Spectropolarimeter Organic materials
Inductively coupled plasma atomic emission Inorganic materials
spectrometer
Nuclear magnetic resonance spectrometer (NMR) Organic chemicals, polymers, drugs, etc.
X-ray fluorescence spectrometer Inorganic materials
Scanning or transmission electron microscope Inorganic chemicals, starch, ore, etc.
(SEM or TEM)
Vacuum evaporator For SEM or TEM (transmission electron
microscope)
Ion-spattering device For SEM or TEM
Freeze-dry device For SEM or TEM, etc.
Energy dispersive X-ray spectrometer Inorganic materials
Auto-tensiometer Surface-active agents
Automatic vacuum distillation apparatus Oils, polyolefins
Density/specific gravity measuring instrument Oils, organic chemicals, etc.

I/C2/15.
CLG/AS 1-Sep. 2002

Instruments Main uses

Thermal analyser Ore, inorganic chemicals
Capillary electrophoresis apparatus Proteins, etc.
Electrophoresis apparatus Proteins, etc.
Automatic molecular weight apparatus Organic chemicals, polymers
Karl Fisher titrating apparatus Quantitative analysis of water
Kinetic viscosity monitoring system General purpose
Micro-organic element and gas analyser Organic chemicals, polymers
Semi-micro amino nitrogen apparatus (Van Slyke Foods
method)
Surface-area apparatus Clays, etc.
Viscosity measuring system Liquid materials
Densitometer For TLC
Autoclave Enzymes, etc.
Incubator Enzymes, etc.
Automatic titrating apparatus Quantitative analysis
Automatic pipetting machine Quantitative analysis
Chromatography system Chemicals, drugs, lubricating oils, etc.
Coulometric analyser Quantitative analysis of metal, etc.
Electrolytic analyser Quantitative analysis of metal, etc.
Flame spectrophotometer Quantitative analysis of metal, etc.
Circulating aspirator General purpose
Electronic shaker General purpose
High-vacuum pump General purpose
Magnetic stirrer with heater General purpose
Hot plate General purpose
Personal computer General purpose
Ultrasonic cleaner For HPLC, etc.
Ultrasonic pipette cleaner Washing of pipettes, etc.

I/C2/15.
CLG/AS 1-Sep. 2002

4. Instrument maintenance and attention

4.1. Introduction

An inventory record and a service record (which covers information on performance

problems, repairs and cost of repairs, date of service, etc.) and a checklist on each
instrument should be kept by the person in charge, who is assigned by the Director
General.

It is, of course, desirable to ask the suppliers to offer routine maintenance training
as part of the purchase contract. The specially-trained staff should prepare diagrams,
charts or a simple manual for other staff, and should explain the operating techniques to
them. Before using the following instruments, staff should read the manual on each
instrument and thoroughly understand its operation. If an accident occurs, the person in
charge or specially-trained staff should be informed immediately. If the instrument can
not be repaired by staff, a qualified service representative could be asked to repair the
instrument, but this would entail considerable expense after the end of the guarantee
period. To save costs, it is important to identify parts which are likely to need periodic
replacement and hence to maintain a stock of these parts.

It is desirable that the periodic servicing (e.g., an annual check) be carried out on
each instrument by a qualified service representative.

It may sometimes be advisable to operate certain complex and expensive

instruments as a kind of "in-house service" (e.g., saccharide analysis by HPLC, fatty-acid
analysis by GC) on a regular, (e.g., weekly) basis. In this way, the number of people
operating expensive and complex instruments can be limited to a small number of
experienced people. Furthermore, similar samples requiring similar analytical conditions
can be grouped, thus avoiding frequent changes of instrument parameters and parts
such as columns. Both measures will reduce the risk of mishandling and expensive
repairs.

I/C2/15.
CLG/AS 1-Sep. 2002

4.2. Instrument maintenance, etc.

Instrument Parameter Maintenance, etc.

Infra-red Resolution, wave- Resolution, wave-number accuracy and
spectrophotometer number accuracy reproducibility should be checked with a
and reproducibility polystyrene film on a monthly basis.
Beam balance The beam balance should be checked in
air on a monthly basis.
Solvents (CS2, CCl4, Solvents (CS2, CCl4, etc.) should be
etc.) handled in a fume chamber.
KBr/NaCl plate, etc. A KBr/NaCl plate should not be used for
samples including moisture. The frosted
plate should be polished on, for
example, a deerskin dampened with
alcohol. After use, the plates, assembly
cells, fixed pass cells, agate mortars
and pestles, etc., must be cleaned and
stored in a dry desiccator.
Humidity of IR room An infra-red room has to be air-
conditioned to ensure less than 50 %
humidity.
Refrigerator Sample Samples, reagents, etc., should be put
away and unnecessary materials should
be disposed of by a person in charge.
Valuable samples and reagents should
be stored carefully, e.g., these materials
should not be placed near the door.

Temperature Check the temperature of the

refrigerator every day.
Gas chromatograph Gas leak When in use, check for a leak of H2 gas,
etc., with a soap solution. If the check is
positive, immediately close the gas
supply valve.
Changing the column After cooling the oven to room
temperature, change the column
carefully using gloves. Before use,
sufficient carrier gas must flow in the
column. The maximum temperature of
each column should be checked in
advance.

I/C2/16.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Septum Replace dirty septum with a new one
before use.
Glass insert Clean or replace the glass insert every
week, when in use.
Washing of detector Before use and after cooling a detector
to room temperature, wash the detector,
if necessary (acetone is employed, for
example, if silicones and TMS(trimethyl
silyl) - derivatives are injected).
Ignition of H2 gas When in use, confirm ignition of H2 gas.
Temperature of On a quarterly basis, the temperature of
column oven the oven should be checked using a
portable indicating reference pyrometer.
When in use, check the temperature
control system and the overheating
protector. After use, allow carrier gas to
flow in the column for cleaning purposes
until it has been cooled to room
temperature for more than 30 minutes
and all switches are finally turned off.
Gas chromatograph Valve check for gas After use, close each gas supply valve.
supply
X-ray diffractometer Angle check An angle check should be carried out
every month.
X-ray leak Checks for X-ray leaks should be
carried out when in use.
Cooling water Before use, check the water pressure
and flow rate. Clean the water tank
every quarter.
X-ray shutter Before use, close the X-ray shutter.
X-ray tube When changing an X-ray tube, handle it
carefully. Turn up the switch of the X-
ray tube gradually.
Changing of test When the sample is changed, close the
samples X-ray shutter. The body must not be
exposed to X-ray radiation.
X-ray detector X-ray detector is used to judge whether
the body is exposed to X-rays. When
an X-ray diffractometer is in use, the
analyst must always have an X-ray
detector.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Use The Director General must designate
staff to be in charge of the use of the X-
ray diffractometer; only the designated
staff can use this instrument. During
operation, the X-ray protection box
should be completely closed and the
operator should inform other staff that
the X-ray diffractometer is in use.
Mill Crushing During crushing, do not insert fingers
into the body of the mill. The sample
should be taken out after the electronic
power has been switched off.
Washing After use, the cutter and sample vessel
should be cleaned. Be careful not to
drench the motor.
UV & VIS Wave-length Twice a month, the wave-length
spectrophotometer accuracy and re- accuracy and reproducibility should be
producibility checked over the entire UV-visible
range by using standard/reference
materials.
Absorbance Every month, the absorbance accuracy
accuracy and re- and reproducibility should be checked
producibility by using standard /reference materials
scanning from 210 to 450 nm.
Cell Handle cells carefully ; after use, clean
and store them in alcohol.
Solvent Care should be taken to ensure
adequate ventilation; do not leave
organic solvents on the benches.
Light source After stabilization, the measurement
should be started. Eyes should not be
exposed to the light source.
Balance Accuracy Reference weights should be calibrated.
If necessary, ask a qualified service
operator or a specially-trained staff
member to check or repair.
Cleaning Keep the analytical balance clean, to
protect all parts from dust or
contamination.
Emission spectro- Mirror balance Mirror balance should be performed by
photometer a qualified service representative.
Ventilation system Check the ventilation system to ensure
that combustion gas does not leak into
the room.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Electrode support Do not touch the electrode support
during measurement.
Safety system for Inspect the safety system for the high-
high-voltage circuit voltage circuit at regular intervals
(quarterly).
Diffraction grating The door of the body of the instrument
and mirror surface should always be closed. Do not touch
the diffraction grating and mirror
surface.
Photographic film or Photographic film and plates should be
plate handled in a dark room.
Cooling water Cooling water is made to flow through
this instrument when in use.
Light source Eyes should not be exposed to the light
source.
Saccharimeter Calibration and Calibrate and determine linearity with
linearity standard sucrose solutions.
Heating mantle Electrical resistance An electrical resistance box should be
box employed for temperature control.
Use Do not use a heating mantle if the
heating coil is exposed. If water and
solvents are spilt, the heating mantle
must immediately be switched off. Once
adequately dried, the heating mantle
can be used again.
Atomic absorption Gas leak Check for any leakage of the gas to be
spectrophotometer used.
Burner head The burner head should be cleaned
before use or after cooling to room
temperature.
Drain Check that the drain bottle does not
overflow.
Position of burner, Before ignition, check the position of the
knob, etc. burner, the pressure control knob, the
switching lever for the gas supply, etc.
Cathode lamp When changing a cathode lamp, it
should be handled carefully.
Leakage of liquids If leakage of the sample solution is
detected, the packing, connector, etc.,
must be changed after cleaning with
water.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Sensitivity When used, the standard solution is
aspirated into the flame and absorption
should be determined. Sensitivity
should be compared with previous
results.
Detection limit When in use, the standard solution is
aspirated with the flame six times
consecutively. The solution, which gives
a minimum of twice the baseline for
every aspiration, represents the
detection limit concentration. The
detection limit should be compared with
previous results.
Gas valve After use, each gas supply valve must
be closed.
Centrifuge Horizontal The centrifuge is placed horizontally in
the room.
Cleaning Keep the inside of the centrifuge clean.
Balance Equal weights of two sample vessels
including muddy samples/suspension
must be placed opposite one another.
Abnormal sound Revolutions should be gradually
increased. If an abnormal sound is
heard, the centrifuge should
immediately be switched off and
everyone should keep away from the
centrifuge until it has stopped.
Oven Temperature control The temperature in the oven should be
checked with an indicating reference
pyrometer. When in use, check whether
the temperature regulator is working.
In the case of a If the sample includes a large quantity of
sample including organic solvent or water, then the
large amounts of solvent or water is initially evaporated to
organic solvent or dryness on/in a water bath and the dried
water sample is then placed in the oven and
thoroughly dried at an appropriate
temperature.
Vacuum drying oven Between the drying oven and the
vacuum pump, a vacuum trap should be
employed. The air-supply valve should
gradually be opened to bring the
pressure in the oven up to the level of
atmospheric pressure.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Rotary evaporator Motor The motor should be firmly fixed on a
support.
Quantity of sample A sample solution corresponding to half
the quantity of the flask to be used is
added to it and the solvent in the sample
solution is then evaporated.
Sample vessel The sample flask should be fixed to the
evaporator with a clip, so as not to fall
into the water bath.
Water bath Ensure that there is always a certain
level of water in the bath to avoid
heating an empty bath.
Evaporated solvents Evaporated solvents should be collected
into the prescribed disposal bottle.
Homogenizer Cutter Before changing or washing the cutter,
turn off the power.
Vessel A plastic vessel is very convenient to
use.
Use The sample should be cut to a few mm
in size in advance. After use, the cutter
and vessel should be cleaned.
Surface tension balance Plate or ring The ring or plate of platinum or glass
should be handled carefully with forceps
and thoroughly washed before/after use.
Sample dish Sample dishes should be cleaned
before/after use.
Surface- tension The surface tension of water/reference
accuracy materials should be initially determined
and adjusted.
Nitrogen analyser system Decomposition The decomposition procedure should be
procedure carried out in a fume chamber.
Sampling Less than 1 g of a sample is used for
nitrogen analysis.
Heating The sample, which includes a lot of
hydrocarbons, should be carefully
heated to avoid bubbling over. It is
better to wait overnight after adding
concentrated sulphuric acid and to start
heating it the following morning.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Diluting After cooling, the decomposition solution
should be transferred to a volumetric
flask to which water has been added in
advance. The flask should be shaken
frequently to ensure thorough mixing.
Distillation device First check whether the connections are
damaged. If so, they should be
repaired/exchanged. Check that the
distillation line is not tightly closed
before heating.
Alkali solution The alkali solution should be carefully
added to the sample solution.
Washing After distillation, this device should be
washed thoroughly with water and
subsequently with de-ionized water.
Water bath Temperature check When in use, check the temperature of
the water bath by using a thermometer.
Adding water Ensure that there is always a certain
level of water in the bath to avoid
heating an empty bath.
Burner Extinguisher An extinguisher should be fitted beside
the burner.
Rubber tube The rubber tube should be firmly settled.
Check carefully for gas leaks.
Volatile organic Before use, check that there is no
solvents volatile organic solvent around the
burner.
Ignition Before igniting, check that the needle
valve for adjusting the gas supply is
closed. The gas supply valves are
opened and the needle valve for
adjusting the gas supply is then opened
gradually and the burner is ignited.
After ignition, the air and gas supply
should be adjusted.
Valve After use, make sure that all gas supply
valves are closed.
pH meter Accuracy and When in use, pH value should be
linearity calibrated as closely as possible with
commercially prepared buffers.

I/C2/15.
CLG/AS 1-Sep. 2002

Instrument Parameter Maintenance, etc.

Electrode After use, the electrode should be
carefully washed with de-ionized water
and capped with de-ionized water to
prevent it from drying out. Check the
quantity of electrode solution every
quarter and add more solution or
change the solution if necessary.
Melting point apparatus Calibration of Take the melting points of standard
thermometer materials.
Heating bath oil or Do not touch the heating bath oil or the
heating plate heating plate directly.
Soxhlet extraction system Extinguisher An extinguisher should be fitted beside
the fume chamber.
Water bath For long-term use, ensure that there is
always a certain level of water in the
bath to avoid heating an empty bath.
Fume chamber Extraction procedures should be carried
out in the fume chamber.
Temperature of The temperature of the water in the bath
water bath is set according to the boiling point of
the solvent to be used, and there should
be a sufficient flow of cooling water.
Anti-bumper Anti-bumper must be added in a
collecting flask to prevent sudden
bumping.
Cooling and After extraction, the pieces of equipment
evaporation of should be placed on an appropriate
solvent stand and cooled. The collecting flask is
again placed on/in the water bath. The
solvent in the flask is almost entirely
evaporated. The flask is then placed in
an oven, set at an appropriate
temperature, and thoroughly dried.
After use After use, the extraction system should
be switched off and the flow of cooling
water should be stopped. Extraction
tools must be cleaned and dried.

x
x x

I/C2/15.
CLG/AS 1-Sep. 2002

Chapter 3 : Chemical reagents, reference chemicals and materials

CONTENTS

1. Basic chemical reagents

1.1 Inorganic acids of non-metals

1.2 Inorganic bases and hydroxides

1.3 Salts of inorganic acids and metals, and inorganic compounds of precious metals

1.4 Organic solvents

1.5 Indicators

1.6 Drying agents

1.7 Sugars

1.8 Enzymes

1.9 Other

2. Supplies and accessories for GC, HPLC, IR, ICP, AAS, etc.*

2.1 Column chromatography (CC)

2.2 Paper chromatography (PC) and thin-layer chromatograph (TLC)

2.3 Gas chromatography (GC)

2.4 High-performance liquid chromatography (HPLC)

2.5 Gel permeation chromatography (GPC)

2.6 Emission spectrophotometry

2.7 Inductively coupled plasma (ICP) and Atomic absorption spectrophotometry (AAS)

2.8 Infra-red spectrometry analysis

2.9 Mass spectrometry analysis

2.10 Nuclear magnetic resonance (NMR) analysis

2.11 pH meter

I/C3/
CLG/AS 1-Sep. 2002

3. Chemicals for illicit drug analysis*

4. Chemicals for titration analysis*

5. Other organic reagents and materials*

5.1 Organic reagents for inorganic analysis

5.2 Hydrocarbons and their derivatives

5.3 Alcohols, phenols, phenol-alcohols and their derivatives

5.4 Ethers, ether-alcohols, ether-phenols and their derivatives

5.5 Aldehyde-function compounds

5.6 Ketone-function compounds

5.7 Carboxylic acids and their anhydrides, halides and their derivatives

5.8 Nitrogen-function compounds

5.9 Heterocyclic compounds

5.10 Vitamins

5.11 Other sugars

5.12 Starches

5.13 Vegetable oils

5.14 Waxes

5.15 Dyes

5.16 Essential oils

5.17 Textiles

5.18 Other

6. Other inorganic reagents and materials*

6.1 Mineral products

6.2 Other inorganic acids of non-metals

6.3 Other salts of inorganic acids and metals, and inorganic compounds of precious
metals
6.4 Other inorganic oxygen compounds

I/C3/
CLG/AS 1-Sep. 2002

I/C3/
 CLG/AS 1 - Sep. 2002

6.5 Base metals

6.6 Other

Notes 1 : Lists, which are marked by "*", would not include chemicals already listed in "1.
Basic chemical reagents".

2: "RM" means "Reference material". In order to save costs, known and well
documented samples should be stored as reference materials.

3: "RM(LH25.28)" and "RMs(LSXI)" mean Reference chemical (Legal text,

heading 25.28) and Reference chemicals (Legal text, Section XI), respectively.
"RM(ENC17N1b)" and "RM(ENC16G) mean Reference material (Explanatory
Note, Chapter 17, Note 1-(b)) and Reference material (Explanatory Note, Chapter
16, General), respectively.

4: Most goods classified in Chapters 28 and 29 are not listed as reference

chemicals. If necessary, these reference chemicals should be prepared
beforehand for use in experiments to determine, for example, whether unknown
samples are separate chemical elements, separate chemically-defined
compounds or separate chemically-defined organic compounds.

5: Since the purchase of chemical reagents and reference materials is dependent on

the resources available, it is desirable for a Customs laboratory to purchase the
basic reagents and materials to establish a minimum capability, and expand as
workflow increases or experience shows necessary.

I/C3/3.
 List of chemical reagents, reference chemicals
and materials for Customs laboratories

Reagent Use No.

Chloric acid 1.1
Hydrogen fluoride (Hydrofluoric acid) 1.1
Hydrogen chloride (Hydrochloric acid) 1.1
Nitric acid, fuming (Sp. Gr. 1.50) 1.1
Nitric acid (SG. 1.42) 1.1
Phosphoric acid 1.1
Phosphorous acid 1.1
Sulphuric acid, fuming (60 %) 1.1
Sulphuric acid 1.1
Ammonium hydroxide 1.2
Barium hydroxide Deproteinising, etc. 1.2
Potassium hydroxide 1.2
Sodium hydroxide 1.2
Ammonium chloride Buffer, etc. 1.3
Ammonium molybdate tetrahydrate 1.3
Ammonium nitrate 1.3
-
Barium chloride dihydrate SO4 , etc. 1.3
Calcium carbonate 1.3
Cupric chloride dihydrate 1.3
Cupric sulphate pentahydrate Fehling's solution A, 1.3
crude protein, etc.

Cuprous chloride 1.3

Dipotassium carbonate anhydrous 1.3
Dipotassium sulphate Crude protein, etc. 1.3
Disodium carbonate monohydrate Alkaline solution, etc. 1.3
Disodium sulphate anhydrous 1.3
Ferric chloride Drugs, etc 1.3
Ferrous chloride tetrahydrate 1.3
Ferrous sulphate heptahydrate 1.3
Platinic chloride Drugs, etc. 1.3

I/C3/4.
 Reagent Use No.
Potassium iodide Illicit drugs, Hanes A, 1.3
dextrose, etc.

Potassium permanganate 1.3

Potassium dichromate 1.3
-
Silver nitrate Drugs, Cl , etc. 1.3
Sodium chloride 1.3
Sodium hydrogencarbonate 1.3
Sodium nitrate 1.3
Sodium sulphite 1.3
Sodium thiosulphate 1.3
Tetrapotassium hexacyanoferrate trihydrate 1.3
Tripotassium hexacyanoferrate Hanes A, etc. 1.3
Trisodium orthophosphate 1.3
1,1,1-Trichloroethane 1.4
1,2-Dichloroethane 1.4
Acetone Oils, etc. 1.4
Acetonitrile 1.4
Benzene Oils, etc. 1.4
Butanone (Methyl ethyl ketone) 1.4
Carbon tetrachloride 1.4
Chloroform 1.4
Cyclohexane 1.4
Dichloromethane Solvent 1.4
Diethyl ether 1.4
Ethanol (Conc. 99.5 % or more by weight) 1.4
Ethyl acetate Alcoholic beverages 1.4
Glycerine 1.4
Methanol 1.4
n-Hexane Squalene, etc. 1.4
n-Pentane 1.4
Petroleum ether Lubricant oils, etc. 1.4
Phenol RM(EN29.07) 1.9

I/C3/5.
CLG/AS 1-Sep. 2002

Reagent Use No.

Propan-1-ol (n-Propanol) Rum, etc. 1.4
Propan-2-ol (2-Propanol) Alcoholic beverages 1.4
Pyridine 1.4
Tetrahydrofuran 1.4
Trichloroethylene 1.4
Toluene RM(EN29.02) 1.4
Xylene RM(EN29.02) 1.4
2,6-Dichloroindophenol sodium 1.5
Alizarin Red 1.5
Alizarin Yellow 1.5
Bromocresol Purple 1.5
Bromocresol Green 1.5
Bromophenol Blue 1.5
Bromothymol Blue 1.5
C.I. acid green 1 (Naphthol Green B) 1.5
C.I. direct red 28 (Congo Red) 1.5
Calmagite 1.5
Chloramine T 1.5
Chlorophenol Red 1.5
Cresol Red 1.5
EBT (Eriochrome Black T) 1.5
Eosin Y 1.5
Epichlorohydrin 1.5
Indigo carmine 1.5
Indole 1.5
Litmus 1.5
Metacresol Purple 1.5
Methyl Orange 1.5
Methyl Red 1.5
Methyl thymol Blue 1.5
Methyl Violet 1.5
Methyl Yellow 1.5

I/C3/6.
 Reagent Use No.
Nessler's reagent 1.5
Neutral Red 1.5
Ninhydrin Ninhydrin spray 1.5
o-Cresolphthalein 1.5
PAN (pyridylazonaphthol) 1.5
Phenol Red (Phenolsulphonephthalein) 1.5
Phenolphthalein 1.5
Sodium nitroprusside Simon's reagent, 1.5
nitrogen, etc.

Starch, soluble Sucrose, etc. 1.5

Thymol Blue 1.5
Thymolphthalein 1.5
Xylenol Orange 1.5
Calcium chloride (CaCl2) 1.6
Calcium oxide (CaO) 1.6
Calcium sulphate (CaSO4) 1.6
Disodium sulphate (Na2SO4) 1.6
Silicone dioxide (SiO2) 1.6
Sodium (Na) 1.6
Fructose RM(LC17N1b) 1.7
Glucose RM(LC17N1b) 1.7
Lactose, monohydrate RM(LC17N1b) 1.7
Maltose, monohydrate RM(LC17N1b) 1.7
Sucrose RM(LC17N1b) 1.7

β-Galactosidase 1.8

Glucoamylase (α-1,4-Glucan glucohydrase) Starch, etc. 1.8

Invertase Sucrose 1.8

Acetic acid Buffer, etc. 1.9
Boiling tips 1.9
Copper wire Halogens, etc. 1.9
Dimethylsulfoxide 1.9
Dimethyl formamide Textiles, etc. 1.9

I/C3/7.
CLG/AS 1 - Sep. 2002

Reagent Use No.

Hydrogen peroxide (Conc. approx. 30 %) Fibres, etc. 1.9
Trifluoro acetic acid 1.9
Aluminium oxide (calcined alumina),(100-200 mesh) Lubricant oils, 2.1
preparations, etc.

Aluminium oxide (calcined alumina), acidic (100-200 mesh) Lubricant oils, 2.1
preparations, etc.

Aluminium oxide (calcined alumina), basic (100-200 mesh) Lubricant oils, 2.1
preparations, etc.

Celite Vitamin E, etc. 2.1

Ion-exchangers Mixtures, etc. 2.1
Silicon dioxide (activated silica gel) (100-200 mesh) Lubricant oils, organic 2.1
preparations, etc.

Tanning extracts of vegetable origin RMs(LH32.01) 2.2

Anthracene RM(EN29.02) 2.3
Benzene (purity 99 % (m/m) minimum) RM(EN29.02) 2.3
m-Cresol RM(EN29.07) 2.3
o-Cresol RM(EN29.07) 2.3
p-Cresol RM(EN29.07) 2.3
Xylenol RM(EN29.07) 2.3
2-Ethyl-2-picoline RM(EN29.33) 2.3
2-Vinylpyridine RM(EN29.33) 2.3
Methylpyridine RM(EN29.33) 2.3
Pyridine RM(EN29.33) 2.3
Linoleic acid RM(ENH29.16) 2.3
Ethanol RM(LC20N6) 2.3
1,2,4-Trimethylbenzene RM(LC27N2) 2.3
Cumene (Isopropylbenzene) RM(LC27N2) 2.3
Ethylbenzene (purity 99 % (m/m) minimum) RM(LC27N2) 2.3
n-Decane (purity 99 % (m/m) minimum) RM(LC27N2) 2.3
Naphthalene RM(LC27N2) 2.3
Squalane RM(LH15.04) 2.3
Squalene RM(LH15.04) 2.3
n-Dotriacontane RM(LH15.10) 2.3
D-Glucitol (Sorbitol) RM(LH29.05) 2.3

I/C3/8.
 Reagent Use No.
Mannitol RM(LH29.05) 2.3
Palmitic acid RM(LH29.15) 2.3
Oleic acid RM(LH29.16) 2.3
Stearic acid RM(LH29.16) 2.3
Alcohol kit RMs 2.3
Fatty acid kit RMs 2.3
Hydrocarbon kit RMs 2.3
Petroleum gases RMs 2.3
Butter RM(LH04.05) 2.3
Lard RM(LH15.01) 2.3
10 % Sucrose diacetate hexabutylate (Chromosorb GAW DMCS, 80- 2.3
100 mesh)
2 % Silicone OV-101 (Chromosorb GAW DMCS, 80-100 mesh) 2.3
2 % Silicone OV-1 (Gaschrom Q, 100-200 mesh) 2.3
2 % Silicone OV-17 (Chromosorb GAW DMCS, 80-100 mesh) 2.3
20 % DEGS (Chromosorb GAW DMCS, 80-100 mesh) 2.3
3 % Silicone SE-30 (Chromosorb GAW DMCS, 80-100 mesh) 2.3
3 % Dexil 300 GC (Chromosorb GAW DMCS, 80-100 mesh) 2.3
5 % PEG (polyethylene glycol) (Chromosorb GAW DMCS, 80-100 2.3
mesh)
PEG 20M (capillary column) 2.3
Silicone OV-101 (capillary column) 2.3
BSA (N,O-bis(trimethylsilyl)acetamide) Narcotic drugs, etc. 2.3
Esterification reagents (BF3-methanol (12 %, W/W), etc.) Vegetable oils, fatty 2.3
acids, etc.

Trifluoroacetic anhydride Acetylation 2.3

Trimethylchlorosilane (TMCS) Trimethylsilicification 2.3
Trimethylsilicification (TMS) reagent Trimethylsilicification 2.3
1,4-Dioxane (HPLC grade) 2.4
Acetone (HPLC grade) 2.4
Acetonitrile (HPLC grade) 2.4
Benzene (HPLC grade) 2.4
Dichloromethane (HPLC grade) 2.4

I/C3/9.
CLG/AS 1-Sep. 2002

Reagent Use No.

Diethyl ether (HPLC grade) 2.4
Ethyl acetate (HPLC grade) 2.4
Hexane (HPLC grade) 2.4
Methanol (HPLC grade) 2.4
N,N-Dimethylformamide (HPLC grade) 2.4
Water (HPLC grade) 2.4
Piperine RM(ENC16G) 2.4
Caffeine RM(LC19N3) 2.4
Theobromine RM(LC19N3) 2.4
Polyethylene glycol (the average molecular weight : 200, 300, 500, RM 2.5
1,000, 2,000 etc.)
Polystyrene (the average molecular weight : 200, 300, 500, 1,000, 2,000 RM 2.5
etc.)
Carbon bars Support 2.6
Iron bar (Standard) RM 2.6
Atomic absorption (AAS) standards (Ag, Al, As, Au, B, Be, Bi, Ca, Cd, RMs(LSXI) 2.7
Co, Cr, Cu, Fe, Ir, K, Mg, Mn, Mo, Na, Nb, Ni, P, Pa, Pb, Pt, Rh, Ru, Se,
Sn, Te, Ti, V, W, Zn, Zr) 1000 ppm
Inductively coupled plasma (ICP) standards (Ag, Al, As, Au, B, Be, Bi, RMs(LSXI) 2.7
Ca, Cd, Co, Cr, Cu, Fe, Ir, K, Mg, Mn, Mo, Na, Nb, Ni, P, Pa, Pb, Pt, Rh,
Ru, Se, Sn, Te, Ti, V, W, Zn, Zr) 10,000µg/ml
KRS-5 cell 2.8
Liquid paraffin 2.8
Potassium bromide (KBr) powder or die (spectrophotometric grade) 2.8
Potassium bromide (KBr) cell 2.8
Potassium bromide (KBr) salt plate 2.8
Sodium chloride (NaCl) cell 2.8
Sodium chloride (NaCl) salt plate 2.8
AgBr plates for wet or aqueous samples (1 set) 2.8
AgCl plates 2.8
Polyethylene RM(LH39.01) 2.8
Polyisobutylene RM(LH39.02) 2.8
Polypropylene RM(LH39.02) 2.8
Poly(vinyl chloride) RM(LH39.04) 2.8

I/C3/10.
 CLG/AS 1 - Sep. 2002

Reagent Use No.

Poly(vinyl acetate) RM(LH39.05) 2.8
Poly(vinyl alcohol) RM(LH39.05) 2.8
Poly(methyl methacrylate) RM(LH39.06) 2.8
Poly(ethylene terephthalate) RM(LH39.07) 2.8
Polyacetals RMs(LH39.07) 2.8
Silicones RMs(LH39.10) 2.8
Standard substances for mass calibration RM 2.9
Acetone-d6 2.10
Benzene-d6 2.10
Chloroform-d 2.10
Deuterium oxide 2.10
Dimethyl-d6 sulphoxide 2.10
Methyl-d3 alcohol-d 2.10
Tetramethylsilane (TMS) RM 2.10

Buffer solution with pH 6.88 at 20 °C pH meter 2.11

Buffer solution with pH 3.57 at 20 °C pH meter 2.11

Buffer solution with pH 4.00 at 20 °C pH meter 2.11

Buffer solution with pH 5.00 at 20 °C pH meter 2.11

2,4-Dinitrophenylhydrazine 3
2,6-Dibromoquinone-4-chloroimide 3
2,6-Dichloroquinone-4-chloroimide 3
4-Dimethylaminobenzaldehyde Psychotropic 3
substances, etc.

Ammonium vanadate Mandelin's reagent 3

Aurous chloride Psychotropic 3
substances, etc.

Bismuth subnitrate Dragendorff spray 3

Cadmium potassium iodide Marme reagent 3
Cadmium iodide Marme reagent 3
Cobaltous thiocyanate Scott reagent 3
Cobaltous acetate tetrahydrate Dille-Koppanyi reagent 3
Ethanal (acetoaldehyde) Dragendorff spray 3
Fast Blue B (di-6-anisidinetetrazolium chloride) Fast Blue B solution 3

I/C3/11.
 Reagent Use No.
Fast Blue BB salt (4-Benzamide-2,5-diethoxybenzene diazonium, zinc Marijuana, etc. 3
chloride salt)
Isopropylamine Dille-Koppanyi reagent 3
Lithium sulphate 3
Magenta I (Fuchsine, C.I. basic violet 2) 3
Mercuric chloride Mayer's reagent 3
Methanal (formaldehyde conc. approx. 37 %) Marquis reagent 3
Methylrosaniline chloride Narcotic drugs 3
Molybdic acid (or sodium molybdate as an alternative) Frohde's reagent 3
p-Dimethylaminobenzaldehyde Ghamrawy reagent 3
p-Dinitrobenzene Zimmermann reagent 3
p-Nitroaniline Psychotropic 3
substances, etc.

Picric acid Psychotropic 3

substances, etc.

Platinum chloride (chloroplatinic acid) Narcotic drugs 3

Potassium 1,2-naphthoquinone-4-sulphonate Psychotropic 3
substances, etc.

Reinecke salt monohydrate (Ammonium 3

tetrathiocyanodiammonochromate)
Selenious acid Mecke's reagent 3
Tetraethylammonium hydroxide 3
Trisodium hexacyanoferrate Psychotropic 3
substances, etc.

Vanillin Duquenois reagent 3

Standards narcotic drugs and psychotropic substances (morphine RMs 3
sulphate, morphine hydrochloride, codeine phosphate, amfetamine
hydrochloride, metamfetamine hydrochloride, etc.)
Cannabis RM 3
Opium RM 3
Ammonium thiocyanate (standard solution) 4
Ammonium ferrous sulphate (Mohr's salt) (standard solution) 4
Hydrogen chloride (Hydrochloric acid) (standard solution) 4
Iodine (standard solution) 4
Karl Fischer reagents 4
Nitric acid (standard solution) 4

I/C3/12.
 Reagent Use No.
Oxalic acid (standard solution) 4
Potassium cyanide (standard solution) 4
Potassium dichromate (standard solution) 4
Potassium hydroxide (standard solution) 4
Potassium iodate (standard solution) 4
Potassium permanganate (standard solution) 4
Silver nitrate (standard solution) 4
Sodium chloride (standard solution) 4
Sodium hydroxide (standard solution) 4
Sodium thiosulphate (standard solution) Sucrose, etc. 4
Succinic acid (standard solution) 4
Sulphuric acid (standard solution) 4
Acetic acid RM(LC22N1d), Hanes 4
A, etc.

Copper phosphide RM(LC28N7) 4

Boric acid RM(LH25.28) 4
Calcium fluoride RM(LH25.29) 4
5-[p-(Dimethylamino)benzylidene]rhodanine Ag, Au 5.1
Alizarin (1,2-Dihydroxyanthraquinone) Al, In, Th, Zr, F 5.1
Aluminon Al 5.1
2-
Curcumin (C.I. natural yellow) B, B2O4 , Be 5.1
3,5,7,2',4'-Pentahydroxyflavone (Morin) Be, Ga, In 5.1
Thiourea Bi, Se 5.1
- 3-
Fluorescein Br ,BrO 5.1
2-
2,7-Dihydroxynaphthalene C2O4 5.1
Glyoxal bis(2-hydroxyanil) Ca 5.1
2,2'-Dipyridyl Cd, Fe(II) 5.1
- -
Aniline Cl , ClO3 5.1
-
Diphenylcarbazide Cl 5.1
Nitroso-R-salt Co 5.1
2-
Methylene Blue Cr(III), Mo, Ta, CrO4 5.1
- -
Cl , ClO4

Disodium chromotropate (Chromotropic acid, disodium salt) Cr(VI), Ti 5.1

I/C3/13.
 Reagent Use No.
Naphthol Yellow S Cs, Rb, K 5.1

Cupron (α-Benzoinoxime) Cu 5.1

Rubeanic acid (Dithiooxamide) Cu, Ru 5.1

1,10-Phenanthroline Fe(II) 5.1
Mannitol Ge 5.1
Quinalizarin Ge 5.1
Diphenylcarbazone Hg(I), Hg(II) 5.1
Leucomalachite Green Ir 5.1
1-Amino-4-hydroxyanthraquinone Li 5.1
Magneson (4-(4-nitrophenylazo)resorcinol) Mg 5.1
Hydroxylamine hydrochloride Mn, drugs, etc. 5.1
Tannic acid Nb, Ta 5.1
Diethylglyoxime Ni, Pa, Re 5.1
3-
α-Naphthylamine NO 5.1
3-
Sulphanilic acid NO 5.1
4-Nitrosodiphenylamine Pa 5.1
Diphenylthiocarbazone Pb, Zn 5.1
4-Nitrosodimethylaniline Pt, Rh 5.1
Resorcinol Pt 5.1
Rhodamine B Sb, Ga 5.1
Cochineal Sc 5.1
N,N'-Diphenylbenzidine Se 5.1
Disodium rhodizonate (Rhodizonic acid, disodium salt) Sr 5.1
+
Thymol Ti, NH4 5.1
Oxine (8-hydroxyquinoline) U, V 5.1
Malachite Green W, Ce 5.1
2,6-Diethylaniline Zn 5.1
Benzyl chloride 5.2
Ligroin SEM 5.2
Nitrobenzene Textiles, etc. 5.2
Paraffin 5.2
Styrene Solvent 5.2

I/C3/14.
 Reagent Use No.
α-Naphthol 5.3

β-Naphthol 5.3

2-Chloroethanol 5.3
2,4-Dinitrophenol 5.3
Benzyl alcohol Perfume 5.3
Butan-1-ol (n-Butanol) Ethanol (IS) 5.3
Butan-2-ol (2-butanol) Alcoholic beverages 5.3
Catechol 5.3
Chloral hydrate Microscope 5.3
Cyclohexanol Solvent 5.3
Ethylene glycol Solvent 5.3
Hydroquinone (p-Dihydroxybenzene) 5.3
Isoamyl alcohol Rum, etc. 5.3
Isobutanol Alcoholic beverages 5.3
Pentanol (Amyl alcohol) Rum, etc. 5.3
Pyrocatechol Tannins 5.3
Pyrogallol Vitamin E, etc. 5.3
Resorcinol Tannins 5.3
2,2'-Oxydiethanol (diethylene glycol) Solvent 5.4
Anisole Perfume 5.4
Benzaldehyde Perfume 5.5
Anthraquinone Oils, etc. 5.6
Anthrone Colouring agent 5.6
Cyclohexanone Solvent 5.6
Hexan-2-on (Butyl methyl ketone) Solvent 5.6
Adipic acid RM 5.7
Citric acid, monohydrate RM, drugs, etc. 5.7
Lactic acid RM 5.7
Maleic acid RM 5.7
Malic acid RM 5.7
Oxalic acid, dihydrate RM 5.7
Succinic acid RM 5.7

I/C3/15.
 Reagent Use No.
Tartaric acid RM 5.7
Acetic anhydride Acetylation 5.7
Cinnamic acid Perfume 5.7
Ethyl formate Solvent 5.7
Formic acid (Conc. 99 % or more by weight) 5.7
Mercurous acetate Iodine value, etc. 5.7
Methyl salicylate Perfume 5.7
Potassium sodium tartrate Fehling's solution B 5.7
Trichloroacetic acid Iodine value, etc. 5.7
Trifluoroacetic acid Acetylation 5.7
Glycine RM (amino acid) 5.8
L-Alanine RM (amino acid) 5.8
L-Arginine, HCl RM (amino acid) 5.8
L-Aspartic acid RM (amino acid) 5.8
L-Cysteine, HCl RM (amino acid) 5.8
L-Glutamic acid RM (amino acid) 5.8
L-Histidine, HCl RM (amino acid) 5.8
L-Isoleucine RM (amino acid) 5.8
L-Leucine RM (amino acid) 5.8
L-Lysine, HCl RM (amino acid) 5.8
L-Methionine RM (amino acid) 5.8
L-Ornithine, HCl RM (amino acid) 5.8
L-Phenylalanine RM (amino acid) 5.8
L-Proline RM (amino acid) 5.8
L-Serine RM (amino acid) 5.8
L-Threonine RM (amino acid) 5.8
L-Tryptophan RM (amino acid) 5.8
L-Tyrosine RM (amino acid) 5.8
L-Valine RM (amino acid) 5.8
Dinitrophenylhydrazine Drugs, etc. 5.8
Ethylenediaminetetraacetic acid (EDTA) Standard 5.8
L- or DL-Ascorbic acid (Vitamin C) RM 5.10

I/C3/16.
 CLG/AS 1 - Sep. 2002

Reagent Use No.

Niacin (Nicotinic acid) RM 5.10
Nicotinamide RM 5.10
L- or DL- Panththenic acid RM 5.10
Pyridoxine (Vitamin B6) RM 5.10
Riboflavin (Vitamin B2) RM 5.10
Thiamine (Vitamin B1) RM 5.10
Vitamin A RM 5.10
Vitamin D2 RM 5.10
Vitamin E RM 5.10
Galactose RM(LH29.40) 5.11
Mannose RM(LH29.40) 5.11
Xylose RM(LH29.40) 5.11
Starch (cassava) RM(LH11.08) 5.12
Starch (corn) RM(LH11.08) 5.12
Starch (potato) RM(LH11.08) 5.12
Starch (wheat) RM(LH11.08) 5.12
Soya-bean oil RM(LH15.07) 5.13
Peanut oil (arachis, groundnut) RM(LH15.08) 5.13
Olive oil RM(LH15.09) 5.13
Palm kernel oil RM(LH15.13) 5.13
Cotton-seed oil RM(LH15.12) 5.13
Safflower oil RM(LH15.12) 5.13
Sunflower-seed oil RM(LH15.12) 5.13
Babassu oil RM(LH15.13) 5.13
Coconut oil RM(LH15.13) 5.13
Palm oil RM(LH15.11) 5.13
Colza oil RM(LH15.14) 5.13
Mustard oil RM(LH15.14) 5.13
Rape oil RM(LH15.14) 5.13
Castor oil RM(LH15.15) 5.13
Corn oil RM(LH15.15) 5.13
Jojoba oil RM(LH15.15) 5.13

I/C3/17.
CLG/AS 1 - Sep. 2002

Reagent Use No.

Linseed oil RM(LH15.15) 5.13
Sesame oil RM(LH15.15) 5.13
Tung oil RM(LH15.15) 5.13
Vegetable waxes RMs(LH15.21) 5.14
Mineral waxes RMs(LH27.12) 5.14
Acid dyes RMs(LH32.04) 5.15
Basic dyes RMs(LH32.04) 5.15
Direct dyes RMs(LH32.04) 5.15
Disperse dyes RMs(LH32.04) 5.15
Reactive dyes RMs(LH32.04) 5.15
Vat dyes RMs(LH32.04) 5.15
Bergamot oil RM(LH33.01) 5.16
Geranium oil RM(LH33.01) 5.16
Ground-nut oil RM(LH33.01) 5.16
Jasmine oil RM(LH33.01) 5.16
Lavender oil RM(LH33.01) 5.16
Lemon oil RM(LH33.01) 5.16
Lime oil RM(LH33.01) 5.16
Orange oil RM(LH33.01) 5.16
Peppermint oil RM(LH33.01) 5.16
Cellulose acetate (yarn) RM(ENC54) 5.17
Nylon (yarn) RM(ENC54) 5.17
Polyester (yarn) RM(ENC54) 5.17
Polyethylene (yarn) RM(ENC54) 5.17
Polypropylene (yarn) RM(ENC54) 5.17
Silk RM(LC50) 5.17
Wool RM(LC51) 5.17
Cotton RM(LC52) 5.17
Flax RM(LH53.01) 5.17
Hemp RM(LH53.02) 5.17
Jute RM(LH53.03) 5.17
Sisal RM(LH53.04) 5.17

I/C3/18.
 CLG/AS 1 - Sep. 2002

Reagent Use No.

Rayon RM(LH54.03) 5.17
Acrylic fibres RMs(ENC54) 5.17
Modacrylic fibres RMs(ENC54) 5.17
Urea General use 5.18
Soaps (sodium stearate, etc.) RMs(LH34.01, 5.18
LH34.02)

Anionic surface-active agents (sodium alkylbenzene sulphonate, etc.) RMs(LH34.01, 5.18

LH34.02), HPLC, etc.

Cationic surface-active agents (cetyl trimethylammonium chloride, etc.) RMs(LH34.01, 5.18

LH34.02), HPLC, etc.

Non-ionic surface-active agents (polyoxyethylene lauryl alcohol ether) RMs(LH34.01, 5.18

LH34.02)

Agar-agar RM(LH13.02) 5.18

Pine oil RM(LH38.05) 5.18
Bovine leather RM(LH41.01) 5.18
Turpentine oils RMs(LH38.05) 5.18
Rosin and resin acids RMs(LH38.06) 5.18
Sublimed sulphur RM(LH25.03) 6.1
Quartz RM(LH25.06) 6.1
Quartzite RM(LH25.06) 6.1
Kaolin RM(LH25.07) 6.1
Andalusite RM(LH25.08) 6.1
Bentonite RM(LH25.08) 6.1
Chamotte RM(LH25.08) 6.1
Decolourising earths RM(LH25.08) 6.1
Dinas earth RM(LH25.08) 6.1
Fire-clay RM(LH25.08) 6.1
Fuller's earth RM(LH25.08) 6.1
Kyanite RM(LH25.08) 6.1
Mullite RM(LH25.08) 6.1
Silimanite RM(LH25.08) 6.1
Chalk RM(LH25.09) 6.1
Barytes RM(LH25.11) 6.1
Witherite RM(LH25.11) 6.1

I/C3/19.
CLG/AS 1 - Sep. 2002

Reagent Use No.

Siliceous fossil meals RM(LH25.12) 6.1
Corundum RM(LH25.13) 6.1
Emery RM(LH25.13) 6.1
Pumice stone RM(LH25.13) 6.1
Slate RM(LH25.14) 6.1
Ecaussine RM(LH25.15) 6.1
Marble RM(LH25.15) 6.1
Travertine RM(LH25.15) 6.1
Basalt RM(LH25.16) 6.1
Granite RM(LH25.16) 6.1
Porphyry RM(LH25.16) 6.1
Sandstone RM(LH25.16) 6.1
Dolomite RM(LH25.18) 6.1
Gypsum RM(LH25.20) 6.1
Limestone RM(LH25.21) 6.1
Hydraulic lime RM(LH25.22) 6.1
Quicklime RM(LH25.22) 6.1
Slaked lime RM(LH25.22) 6.1
Soda asbestos RM(LH25.24) 6.1
Mica RM(LH25.25) 6.1
Steatite RM(LH25.26) 6.1
Chiolite RM(ENH25.30) 6.1
Cryolite RM(ENH25.30) 6.1
Felspar RM(LH25.29) 6.1
Fluorspar RM(LH25.29) 6.1
Leucite RM(LH25.29) 6.1
Nepheline syenite RM(LH25.29) 6.1
Nepheline RM(LH25.29) 6.1
Chlorite RM(LH25.30) 6.1
Kieserite RM(LH25.30) 6.1
Perlite RM(LH25.30) 6.1
Vermiculite RM(LH25.30) 6.1

I/C3/20.
 CLG/AS 1 - Sep. 2002

Reagent Use No.

Earth colours RM(LC25N2b) 6.1
Ores RMs(LC26) 6.1
Hydrogen bromide Bromination 6.2
Hydrogen iodide Iodination 6.2
Ammonium cobaltous thiocyanate General use 6.3
Barium carbonate General use 6.3
Calcium chloride dihydrate General use 6.3
Chloroauric acid Drugs, etc. 6.3
Cupric sulphate, anhydrous General use 6.3
Disodium hydrogenorthophosphate Drugs, etc. 6.3
Disodium sulphate decahydrate General use 6.3
Disodium tetraborate decahydrate (Borax) General use 6.3
Magnesium chloride hexahydrate General use 6.3
Mercuric chloride General use 6.3
Potassium bromate General use 6.3
Potassium bromide General use 6.3
Potassium chloride General use 6.3
Potassium chromate As an indicator, etc. 6.3
Potassium cyanide General use 6.3
Potassium fluoride As an indicator, etc. 6.3
Potassium hydrogencarbonate General use 6.3
Potassium iodate General use 6.3
Potassium nitrate General use 6.3
Potassium nitrite General use 6.3
Sodium bromide General use 6.3
Sodium cyanide General use 6.3
Sodium hypochlorite Fibres, etc. 6.3
Sodium nitrite General use 6.3
Sodium phosphotungstate Starch, etc. 6.3
Stannic chloride General use 6.3
Zinc sulphate Starch, Hanes A, 6.3
deproteinizing, etc.

Reagent Use No.

I/C3/21.
CLG/AS 1 - Sep. 2002

Zinc chloride Fibre, etc. 6.3

Calcium hydroxide General use 6.4
Cupric oxide General use 6.4
Cadmium (high purity) RM 6.5
Iron, reduced RM 6.5
Magnesium powder (high purity) RM 6.5
Manganese (high purity) RM 6.5
Iron powder (high purity) RM(LC72) 6.5
Copper (high purity) RM(LC74) 6.5
Nickel (high purity) RM(LC75) 6.5
Aluminium (high purity) RM(LC76) 6.5
Lead (high purity) RM(LC78) 6.5
Zinc powder (high purity) RM(LC79) 6.5
Tin (high purity) RM(LC80) 6.5
Bromine Drugs, etc. 6.6
Carbon disulphide Solvent 6.6
Charcoal, activated, powder General use 6.6
Glass wool General use 6.6
Iodine Iodine, etc. 6.6
Platinum wire General use 6.6

* * *

I/C3/22.
 CLG/AS 1 - Sep. 2002

Chapter 4 : Technical literature and reference books

CONTENTS

1: General technical references

2: Polymer references

3: Textile references

4: Paper references

5: Wood references

6: Food references

7: Pharmaceutical and cosmetic references

8: Mineral and metal references

9: Spectral references

10 : Chromatography references

11 : Other references

I/C4/1
CLG/AS 1 - Sep. 2002

Title Author Publisher

1 Analytical Chemistry, 4th Edition Gary D. Christian John Wiley & Sons, Inc.
1 ASTM (American Society for Testing and ASTM
Materials) standards
1 BSI (British Standards Institute) standards BSI
1 Chemical and Process Technology D.M. Considine McGraw-Hill
Encyclopedia
1 Colour Index The Society of Dyes and Colour
Colourists

1 Concise Etymological Dictionary of S.C. Bevan Applied Science Publishers

Chemistry
1 Concise Encyclopedia of Biochemistry T. Scott de Gruyter
1 Dictionary of Scientific and Technical Terms S.P. Parker McGraw-Hill
1 Dictionary of Organic Compounds Chapman and Halls
1 Encyclopedia of Industrial Chemical Analysis F.D. Snell Interscience
1 Encyclopedia of Chemical Technology Kirk-Othmer John Wiley & Sons, Inc.
1 Encyclopedia of Science and Technology McGraw-Hill
1 General Chemistry in the Laboratory, 2nd J.L. Roberts Jr., Freeman
Edition et al.
1 Handbook of Chemistry Adolph Lange McGraw-Hill
1 Hawley's Condensed Chemical Dictionary G.G. Hawley Van Nostrand Reinhold
Company
1 ISO (International Organization for ISO
Standardization) standards
1 IUPAC (International Union of Pure and Butterworths
Applied Chemistry) standards
1 IUPAC Nomenclature of Organic Chemistry Butterworths
1 IUPAC Nomenclature of Inorganic Chemistry Butterworths
1 Molecular Biology and Biotechnology 2nd J.M. Walker & Royal Society of Chemistry
E.B. Gingold
Edition 1988
1 Official Method of Analysis, Association of Association of Official Analytical
Chemists, Inc.
Official Analytical Chemists (AOAC)
1 Official Methods of Chemical Analysis Association of Official
Analytical Chemists
1 Quality Assurance Principles for Analytical Frederick M. AOAC
Laboratory Garfield

I/C4/2
 CLG/AS 1 - Sep. 2002

Title Author Publisher

1 Standard Methods of Chemical Analysis Frank J. Welcher Robert E. Kringer Publishing

Co.
1 The Merck Index, 11th Edition Merck & Co., Inc.
2 Encyclopedia of Polymer Science and H.F. Mark John Wiley & Sons, Inc.
Technology
2 Encyclopedia of Polymer Science and John Wiley & Sons, Inc.
Engineering, 2nd Edition (1987)
2 Handbook of Common Polymers Rolf and Scott
2 Identification and Analysis of Plastics Illife Books
2 Modern Plastics Encyclopedia McGraw-Hill
2 Plastic Additives & Modifiers Handbook Jesse Van Nostrand Reinhold
Edenbaum Company
2 Plastics Analysis Guide, Chemicals and A. Krause, etc. Hanser Publishers
Instrumental Methods
3 Fairchild's Dictionary of Textiles, 6th Edition I.B. Wingate Fairchild Publications
3 Guide to The Identification of Animal Fibres, H.M. Appleyard WIRA
2nd Edition, 1978
3 Identification of Textile Materials, 9th Edition The Textile Institute
3 Identification of Vegetable Fibres, 1982 D. Catling & Chapman and Hall
J. Grayson
3 Introductory to Textile Science Marjory L. Holt, Rinehart and Winston
Joseph
3 Textile Terms and Definitions, 1981 The Textile Institute
4 Analysis of Paper, 2nd Edition B.L. Browning Mercel Dekker, Inc.
4 Handbook of Pulp and Paper Technology, Kenneth W. Britt Van Nostrand Reinhold
2nd Edition Company
4 The Dictionary of Paper, 4th Edition, 1980 American Paper Institute
5 The Practical Identification of Wood Pulp R.A. Parham, TAPPI Press
Fibres R.L. Gray
5 Wood Structure and Identification, 2nd H.A. Core, Syracuse University Press
Edition, Syracuse Wood Science Series 6, W.A. Cote,
1979 A.C. Day
6 Bailey's Industrial Fat and Oil Products John Wiley & Sons, Inc.
6 Chocolate, Cocoa and Confectionery Bernard W. Van Nostrand Reinold
Science & Technology 3rd Edition (1989) Minifie
6 Encyclopedia of Food Science Food Technology and
Nutrition

I/C4/1
 CLG/AS 1 - Sep. 2002

Title Author Publisher

6 Food Composition and Nutrition Tables (in Wissenschaftliche

three languages) Verlagsgsesellschaft GmbH
7 Analysis of Drug Manual Drug Enforcement
Administration in USA
7 Basic Tests for Pharmaceutical Dosage WHO
Forms
7 Basic Tests for Pharmaceutical Substances WHO
7 Clarke's Isolation and Identification of Drugs The Pharmaceutical Press
7 Clandestine Manufacture of Substances UNDCP
under International Control
7 Cosmetic Bench Reference Allured Publishing Corp.
7 CTFA International Cosmetic Ingredients Nikitakis, The Cosmetic Toiletry and Fragrance
Association
Dictionary J.M.MC.Ewen,
G.N. Eds
7 Dictionary of Drugs Chapman and Halls
7 European Pharmacopoeia Maisonneuve S.A.
7 Flavour and Fragrance Materials Allured Publishging Corp.
7 Flavour Science and Technology, 1990 Y. Bessière and A.F. John Wiley & Sons, Inc.
Thomas

7 Glossary of Terms for Quality Assurance and UNDCP

Good Laboratory Practices
7 Instrumental Data for Drug Analysis Elsevier
7 Multilingual Dictionary of Narcotic Drugs and The United Nations
Psychotropic Substances under International
Control
7 Perfume and Flavor Chemicals S. Arctander Allured Publishing
7 Perfume and Flavor materials of Natural S. Arctander Allured Publishing
Origin
7 US Pharmacopoeia United States Pharmaceutical
Convention

7 USP Dictionary of USAN and International United States Pharmaceutical

Convention
Drugs Names
7 Good laboratories practices in governmental WHO
drug control laboratories and Training
programme in drug analysis
7 Validation of analyical procedures used in the WHO
examination of pharmaceutical materials
8 A Concise Introduction to Ceramics (1991) George C. Van Nostrand Reinhold
Phillips

I/C4/1
 CLG/AS 1 - Sep. 2002

Title Author Publisher

8 Industrial Minerals and Rocks, 6th Edition Society of Mining, Metallurgy and
Exploration, Inc.

8 Metals Handbook American Society for Metals

9 An Infra-red Spectroscopy Atlas for the Infra-red Spectroscopy Committee of the
Chicago Society for Coating Technology,
Coatings Industry, 2nd Edition pub.

9 Atlas of Polymer and Plastic Analysis Deiter O. Hanser Publishers

Hummel
9 Infra-red Spectra Handbook of Common Sadtler Research
Organic Solvents Laboratories
9 The Infra-red Spectra Atlas of Monomer and Sadtler Research
Polymer Laboratories
9 The Infra-red Spectra Atlas of Surface Active Sadtler Research
Agents Laboratories
9 The Infra-red Spectra Handbook of Mineral Sadtler Research
and Clays Laboratories
9 The Infra-red Spectra Handbook of Inorganic Sadtler Research
Compounds Laboratories
9 UV and IR Spectra of Pharmaceutical Association of Official Analytical
Chemists
Compounds
10 Chromatographic Science Series (Vol.II) K.H. Altgelt and Marcel Dekker, Inc.
T.H. Gouw

10 Chromatography : Concept and Contrasts James M. Miller John Wiley & Sons, Inc.
10 Handbook of Analytical Derivatization Daniel R. Knapp John Wiley & Sons, Inc.
Reactions
10 Handbook of Chromatography General Data G. Zweig and CRM Press
and Principles J. Sherma
10 High Performance Liquid Chromatography Csaba Horvath Academic Press
10 Modern Practice of Gas Chromatography, Robert L. Grob John Wiley & Sons, Inc.
2nd Edition
10 Practice of High-Performance Liquid H. Engelhardt Springer-Verlag
Chromatography, 1986
10 Practice of Thin-Layer Chromatography J.C. Touchstone John Wiley & Sons, Inc.
10 Quantitative Analysis Using E. Katz John Wiley & Sons, Inc.
Chromatographic Techniques, 1987
10 The Analysis of Gases by Chromatography C.J. Cowper and Pergamon Press
A.J. DeRose

10 Thin-Layer Chromatography, 2nd Edition Bernard Fried and Marcel Dekker, Inc.
Joseph Sherma

11 Enzyme Handbook, Supplement I, 1974 T.E. Barman Springer-Verlag

I/C4/1
 CLG/AS 1 - Sep. 2002

Title Author Publisher

11 Handbook of Adhesives Irving Shiest Van Nostrand Reinhold

Company
11 Handbook of Industrial Chemical Additives, Michael Ash VCH Publishers
1991
11 Industrial Chemical Thesaurus, 1992 Michael Ash VCH Publishers
11 MC Cutcheon's Functional Materials, 1994 MC Cutcheon's Division MC Publishing Co.
11 MC Cutcheon's Emulsifiers and Detergents, MC Cutcheon's Division MC Publishing Co.
1994
11 Paint Handbook Guy E. McGraw-Hill
Weismantel
11 Refractory Materials Chemical Technology G.B. Rothenberg Noyes Data Corporation
Review No. 76 (1976)
11 Rubber Worl Magazine's 1995 Blue book Lippincot & Peto Inc.
11 The Pesticide Manual 9th Edition CH R. Worthing The British Crop Protection
Council

x
x x

I/C4/1