Operator’s Manual

Spectroil M/F-W
Fuel Analysis Spectrometer

“…for rapid on-site trace metal analysis of liquid fuels used

in liquid-fired gas turbines and diesel engines”

160 Ayer Road Littleton, MA 01460 U.S.A. • Tel. 978.486.0123 • Fax 978.486.0030
email: [email protected] • web page: www.spectroinc.com

Manual Part No. M96116

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE) Operator’s Manual  |  i

Table of Contents
1.0 GENERAL OPERATING REQUIREMENTS ................................................................. 1
1.1 Power Application and Systematic Power Removal............................................................. 1
1.2 Rod Electrode Sharpening ................................................................................................. 3
1.3 Installing the Disc Electrode............................................................................................... 4
1.4 Installing the Rod Electrode and Setting the Gap............................................................... 4
1.5 Installing and Positioning the Sample Holder and Cover.................................................... 5
1.6 Cleaning the Sample Stand . .............................................................................................. 7
1.6.1 Cleaning After Each Burn Cycle ........................................................................................ 7
1.6.2 Cleaning After Each Operating Shift .................................................................................... 7
1.6.3 Cleaning the Quartz Window . .......................................................................................... 8
1.6.4 Cleaning Solutions ............................................................................................................ 8
1.7 Paper Tissue for Operating and Paper Towels for Cleaning ............................................... 8
1.8 Waste Oil Disposal Container ........................................................................................... 8

2.0 DAILY OPERATION ....................................................................................................... 9

2.1 Daily Routine Prior to Use ................................................................................................ 9
2.2 Warm-Up Procedure . ........................................................................................................ 9
2.3 Routine Fuel Sample Analysis . ........................................................................................ 11
2.3.1 Routine Fuel Sample Analysis of Undiluted Samples........................................................ 11
2.3.2 Sample Preparation for #6 Residual Fuels......................................................................... 13
2.3.2.1 Pre-Dilution Sample Heating .......................................................................................... 13
2.3.2.2 Sample Dilution of # 6 Residual Fuel............................................................................... 14
2.4 Daily Standardization Check ........................................................................................... 15
2.5 Complete Standardization ............................................................................................... 16
2.6 Daily Routine Prior to Securing ...................................................................................... 19
2.7 Optical Profiling . ............................................................................................................ 20
2.8 Sample Identification (I.D.)............................................................................................. 21
2.8.1 Setup of the Sample I.D................................................................................................... 21
2.8.2 Using Sample ID.’s........................................................................................................... 21
2.9 Sulfur Analysis.................................................................................................................. 22
2.9.1 Set-up for Sulfur Analysis................................................................................................. 22
2.9.2 Profiling the sulfur Optic................................................................................................. 24
2.9.3 Standardization of the Sulfur Optic.................................................................................. 24
2.9.3 Verification....................................................................................................................... 25
2.9.4 Clean Up and Final Checks.............................................................................................. 25
2.10 Water Analysis.................................................................................................................. 25
2.10.1 Water Program Standardization........................................................................................ 26
2.10.2 Verification....................................................................................................................... 27
2.10.3 Routine Water Sample Analysis........................................................................................ 27

3.0 OPERATOR MAINTENANCE...................................................................................... 28

3.1 Daily Operator Maintenance............................................................................................ 28
3.2 Scheduled Periodic Maintenance...................................................................................... 28
3.3 Procedure to Replace Electrode Sharpener Cutter Blade, M90102.................................... 38

4.0 PERFORMING CALIBRATION CURVE VERIFICATION ......................................... 33

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ii  |  Table of Contents

4.1 Repeatability Testing . ..................................................................................................... 33

4.2 Accuracy . ........................................................................................................................ 34
4.3 Factors Affecting Repeatability and Accuracy.................................................................... 34
4.4 Disc Electrode Offset Procedure....................................................................................... 35

5.0 BACKUP OF COMPLETE OilM SOFTWARE.............................................................. 37

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Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE) Operator’s Manual  |  iii

List of Effective Pages

Summary of Spectroil Modifications

Modification Description
Mod 0 Original CID version of Spectroil M
Mod 1 Upgrade with SFTM port and frequency adjustment potentiometer
Mod 2 Addition of solid state excitation ignition module and SFTM port
Mod 3 Upgrade to combined solid state source
OilMWindows Upgrade to Windows hardware and software
Mod 4 Upgrade to panel PC hardware and Windows XP
Mod 5 CE version of the Spectroil M
Mod 6 CCD Optic and New Software v. 5, starting w/serial number 6001
Mod 7 C.E. version of Mod. 6

Summary of OilMWindows Modification 6 Hardware and Software Manual Versions

Change Version Date Description

First Issue 3.0 7/1/07 Complete update of Mod. 5 version 2.5 manual to include CCD
optic & updated software.
Change 1 3.1 10/24/07 Update for CE version, Mod. 7, changes. Addition of optic
removal procedure. Grammatical corrections
Change 2 3.2 10/31/07 More updates to Chapter 2 for CE certification.
Change 3 3.3 2/23/08 Created separate M/F-W Operator’s Manual, updated accuracy
table, included sample ID, operator’s maintenance, sulfur analy-
sis and residual sample preparation.
Change 4 3.4 4/15/08 Added NOx water analysis procedure.
Change 5 3.4.1 12/23/09 Corrected Figure 2-1.

23 December 2009 / v.3.4.1

iv  |  List of Effective Pages

Total Number of pages in this manual is 46 consisting of the following:

Section Page Numbers

Cover 2
Table of Contents i - ii
List of Effective Pages iii - vi
Chapters 1 - 5 1 - 38

WARNING!!!
High Voltages are Present During the Operation of the
Spectroil M!

Observe all Safety Precautions!

Turn OFF the Main Power Switch and unplug the

SPECTROIL M before any work is performed.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE) Operator’s Manual  |  v

Definitions

The following definitions apply to specific instructions throughout this manual.

WARNING!!!
An operating procedure or practice that may cause injury if not carefully observed or
followed.

CAUTION!!!
An operating procedure or practice that may cause damage to the LNF if not carefully
observed or followed

NOTE!!!
An operating procedure or practice that is essential to emphasize

Software CAUTION!!!
The Spectroil M computer is capable of running multiple software
applications and/or operating systems. However, as designed, the
computer processor is dedicated to the operation and control func-
tions of the Spectroil M. Do not attempt to add any software or al-
ter the original factory installed software without checking first with
the Spectro Inc. Service Department.

23 December 2009 / v.3.4.1

vi  |  List of Effective Pages

Note on Oil Standards

The Spectroil M series of spectrometers can be calibrated for military or commercial
applications. As a rule, the Spectroil M/N-W is calibrated and standardized with D-19,
D-12 and D-3 series of standards, and the Spectroil M/C-W with V-21 or S-21 series
of calibration standards.

Although this manual frequently refers to the military “D” series of standards, the op-
erator procedures are identical for all types of Spectroil M spectrometers. Commercial
customers should substitute their equivalent “V” or “S” series of standards throughout
this manual.

WARRANTY
The warranty period of the Spectroil M family of spectrometers is twelve (12)
months from date of installation or fifteen (15) months from date of shipment,
whichever occurs first. Spectro warrants the Spectroil under conditions of opera-
tion against defects of materials and workmanship. All defective material will be
replaced providing damage was not caused by improper use. Warranty applies to
parts and labor only.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  1

1.0 GENERAL OPERATING

Spectroil M/F-W REQUIREMENTS

Fuel Analysis Spectrometer This manual provides the Spectroil M/F-W opera-
tor with routine instructions on how to set-up the
spectrometer, analyze fuel samples, and perform
routine maintenance. The instructions apply to
the Spectroil M/F-W Fuel Analysis Spectrom-

Operator’s eter with Mod. 6 (CCD optic) and Mod. 7 (C.E.

hardware).

Manual 1.1 Power Application and Systematic Power

Removal

The Spectroil M/F-W consists of the excitation,

optics and readout subassemblies. Each subas-
sembly requires specific voltages to perform as a
system. These voltages are generated within each
subassembly and originate from the main pow-
er distribution assembly. Main power for these
subassemblies is fused with a 10 ampere circuit
breaker CB1 which is mounted on the Power
Connection Plate located on the right side near
the back of the instrument. Power should not be
applied to the instrument unless all specifications
for input power requirements have been met.

To apply power to the instrument, place circuit

breaker CB1 in the upright ON position, Figure 1-1.

Once power is applied to the instrument, two

events occur. First, an internal controller will

Circuit Breaker, CB1

Main Input Power

Connection

Electrode Sharpener
Power Connection

Figure 1-1, Right Side View Showing Circuit Breaker

CB1

23 December 2009 / v.3.4.1

2  |  Operator’s Manual

initialize and automatically load the application. maximum instrument stability. When not in
Simultaneously, the readout system will load use, the MODE switch should be placed in the
Windows XP® and start up the instrument’s appli- STANDBY position.
cation program called OILMWindows®. The in-
strument will boot directly to the Analysis Screen, To completely turn off the Spectroil M/F-W, first
Figure 1-2. shut down the OILMWindows software and then
remove power from the instrument.
If the system fails to establish communication, a
screen similar to Figure 1-3 appears to select the CAUTION: Utilizing the Windows XP® oper-
Correct Configuration File Path. This will hap- ating system dictates a specific series of steps to
pen if the system cannot find a file in case it hasbe performed in the process of shutting down
been moved, updated or is corrupted. Refer to the Spectroil M/F-W. If power is accidentally re-
the Maintenance Manual Section 2.4.4.6 for as- moved from the Spectroil M/F-W spectrometer
sistance to diagnose and correct this condition. or the circuit breaker CB1 is shut off while the
readout system is running Windows XP® or the
Next, move the MODE switch to the OPERATE OILMWindows® application, an orderly shut-
position and power will be applied to the excita- down would not be performed and as a result,
tion source and electrode sharpener. A noticeable the Windows XP® operating system must perform
increase in fan activity will be observed; this is hardware and software diagnostics when power is
normal. reapplied.

At this point, the instrument is ready to begin To prevent this from happening, always follow the
operation. Some time will be needed before the next steps to shut down the Spectroil M/F-W.
instrument stabilizes after power is applied. It is
recommended that the main power remain on 1. Shut down the OILMWindows® applica-
when the instrument is not in use to maintain tion by left clicking the close box (box with
an “X”)in the upper right corner of the
OILMWindows® header, or choose File/Exit
from the pull down menu options. This
will return the software to the Windows XP®
desktop.

2. Left click the START menu and select Shut

Down. A dialog will appear asking what do
you what the computer to do. The options
are, Standby, Restart, or Shutdown.

3. Highlight the Shutdown radio button and

Figure 1-2, Analysis Screen
select OK.

4. The Windows XP® logo will appear with the

instruction that it is shutting down.

5. After the logo disappears a message “It’s now

safe to turn off your computer “ will appear.
Figure 1-3, Error Message if Communications Cannot be
Established 6. It is now safe to place the main circuit break-

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  3

er CB1 in the down position to remove all base of the electrode sharpener. The sound of the
power from the instrument. electric motor should be heard and a slight vibra-
tion should be felt through the motor. The mo-
If, by accident, power was removed from the in- tor will continue to run on a self-timed cycle for
strument, a series of diagnostics will automati- approximately 3 to 5 minutes. Insert the rod into
cally be performed when power is reapplied. It is the rotating electrode guide hole until it comes
extremely important to allow these diagnostics to in contact with the cutter blade. Apply inward
complete in their entirety before loading any ap- pressure until approximately 1/8 to 3/16 inch (3
plication software. If problems are experienced to 5 mm) is cut from the end of the rod. Slightly
during the process of running these diagnos- decrease the inward pressure on the rod electrode,
tics, contact the technical service department of but still maintain its contact with the cutter blade.
Spectro Incorporated for instructions on how to This will polish the rod electrode tip.
recover and proceed with normal operation.
Remove the rod electrode and visually inspect
To restore power to the instrument, follow the in- the tip. It should have a clean cut with no ap-
structions given above. parent chipping around the circumference of the
rod. The surface should be very smooth and have
a polished mirrored looking surface. If the qual-
1.2 Rod Electrode Sharpening ity of the surface is not as described, insert the
rod into the sharpener and repeat the cutting and
The rod electrode, along with the disc electrode, polishing procedure. Remove the rod, inspect
form the analytical gap through which the oil or the surface quality and if acceptable, place the
fuel sample are passed for analysis. An alternat- rod electrode into the original box for storage un-
ing current discharge will occur between the disc til ready for use. To prevent contamination of a
and rod electrode and vaporize the sample and the sharpened rod electrode, do not touch the tip or
metallic components in it. This is the basis of the edge of the tip of the sharpened electrode with the
arc emission technique. fingers or metallic surfaces or anything but a fresh,
clean laboratory grade paper towel. Do not use a
The preparation of the tip of the rod electrode rod electrode for analysis if the surface appears to
plays a significant role in obtaining repeatable an- have been damaged. Refer to Section 7.6.5.1 for
alytical data. The rod electrode must be cleaned the procedure to change/rotate the cutter blade.
prior to inserting it into the electrode sharpener.
T his is accomplished by taking a clean paper NOTE: The electrode sharpener can be a potential
towel and removing the components of the burn source of contamination that can result in degraded
residue from the previous analysis. Remove all accuracy. The electrode sharpener must be emptied
residue from the tip and sides of the electrode by and cleaned frequently.
rotating the rod in the paper towel while applying
pressure with the fingers of the opposite hand. The rod electrode sharpener has a graphite collec-
tor barrel assembly which is secured to the motor
NOTE: The paper towel should be laboratory grade mount and face plate by a rubber o-ring. After
and free of silicon. Do not use household grade approximately 250 sharpenings, this graphite col-
paper towels. lector will need to be emptied. To remove this
barrel assembly, locate the sharpener over a waste
With the spectrometer on, turn the MODE basket with the collector barrel pointing down-
switch to OPERATE. This applies power to J2, ward. Grasp the barrel with the opposite hand
the electrode sharpener power connector. Mo- and rotate it while pulling it away from the motor
mentarily press the power switch located on the mount and face plate. Once the o-ring disengages

23 December 2009 / v.3.4.1

4  |  Operator’s Manual

from the collector barrel, it will be easy to sepa- See Section 1.7 for a description of the laboratory
rate and empty. grade paper towel. Pour out a few disc electrodes
onto a clean laboratory grade paper towel. Take
While the collector barrel assembly is removed, a laboratory grade paper towel and double it to
check the rod electrode cutter head and blade. be sure that no contamination from the fingers
There should not be an accumulation of oil or will be absorbed into the disc. If large size paper
carbon in this area. If an oily residue is present, towels are used, they should be cut with scissors
this is an indication that the rod electrodes are not into two inch squares to facilitate easy handling.
being adequately cleaned before insertion into Place the towel over the disc electrodes, and with
the electrode sharpener. To clean this assembly, the forefinger and thumb, grab one disc from the
remove the cutter blade and use general purpose pile and place the disc on the shaft, Figure 1-4.
spray and wipe detergent. Reassemble the cutter With firm pressure, push the disc electrode onto
blade and the graphite collector barrel assembly. the shaft until it comes to rest against the index
shoulder of the shaft. If the disc electrode does
The cutter blade, part number M90102, for the not offer some resistance to the shaft as it is be-
rod electrode sharpener is a three-sided tungsten ing inserted, remove and discard this electrode
cutter tool commonly used in machining opera- because the inner diameter has not been made to
tions. One side is capable of approximately 1000 the tolerances specified.
sharpenings. The edge of a cutter is worn when
the initial cut of the electrode requires an abnor- CAUTION: The disc electrode shaft is designed
mal amount of inward pressure, and/or a smooth to be replaced by the operator using a small
reflective surface cannot be achieved on the tip jeweler’s screwdriver. The shaft has right hand
of the rod electrode. Refer to Section 3 for the threads for tightening it into the commutator.
procedure to replace the cutter blade. When pushing the disc electrode on the shaft, do
not apply counter-clockwise rotation on the disc
The electrode sharpener power is on a timing electrode as this may cause the disc electrode shaft
circuit and will turn off after approximately 3 to to loosen.
5 minutes. The electrode sharpener can also be
turned off by placing the MODE switch in the NOTE: Loose disc electrodes will produce errone-
STANDBY position. ous results. If the disc electrode is too loose, arcing
will occur between the inner diameter of the disc
and the outer diameter of the shaft.
1.3 Installing the Disc Electrode
CAUTION: The disc electrode may be very hot
The disc electrode is the most significant contrib- to the touch.
utor to the accuracy and repeatability of the in-
strument. They are manufactured and then puri- Use a towel to remove a disc electrode from the
fied to strict specifications to ensure that they do shaft after an analysis, and to wipe away any oil
not contain unacceptable levels of trace element which may have spilled over from the burn.
contamination for the elements of interest. The
care taken to properly install the disc on the shaft
will help to ensure that excitation parameters will 1.4 Installing the Rod Electrode and Setting
be kept as constant as possible, thus resulting in the Gap
repeatable analytical data.
The rod electrode is installed after the disc elec-
To install the disc electrode on the shaft, a labo- trode is already in place. To install the rod elec-
ratory grade disposable towel is recommended. trode, take the rod in the fingers of the right hand

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  5

Rod Electrode

Rod Electrode Clamp

Analytical Gap Setting Knob
Lever

Protective Quartz Sample Stand

Window Sensors

Oil Sample Holder

DiscElectrode

Sample Table
Positioning

Figure 1-4, Sample Stand and Controls for Routine Operation

and with the left hand apply inward pressure to lever begins to return to the lowered position, the
the round black rod electrode clamp knob, Figure rod electrode holder and slide mechanism begins
1-4. This will open the clamp door approximately to raise upward along the vertical axis until it is
3/8 inch (9.5 mm). stopped by the analytical gap adjustment screw.
This time the rod electrode, which is clamped in
Insert the rod electrode into the vertical “v” shaped the rod electrode holder and slide mechanism,
channel until the sharpened tip can be seen pro- will travel upward with the slide mechanism. An
truding from the bottom of the rod holder and analytical gap distance of 0.090 inches has now
gap setting device. Release the rod clamp knob been precisely set.
and the rod electrode will be pinched between
the back of the rod clamp knob and the centering NOTE: Care must be taken not to touch the brass
“v” channel. Press and then release the rod clamp block with the tip of the carbon rod in order to
knob again and the rod electrode will drop by avoid false copper readings.
gravity and come to rest on the disc electrode.
The analytical gap distance has been set during
Raise the analytical gap setting lever. This ac- factory calibration and should not be readjusted
tion will drive the rod electrode holder and slide during routine operation.
mechanism downward along the vertical axis. As
the slide mechanism moves downward, the rod
electrode remains in the installed position, be- 1.5 Installing and Positioning the Sample
cause there is zero clearance between the disc and Holder and Cover
rod electrodes. The analytical gap setting lever
will reach the end of its travel when it is raised The Spectroil M/F-W can accommodate several
to the full upward position. Return the analytical different types of sample holders and a sample
gap setting lever to the lowered position. As the holder cover. The following paragraphs describe

23 December 2009 / v.3.4.1

6  |  Operator’s Manual

the procedure to install disposable and reusable

sample holders and the sample holder cover.

Disposable sample holder require the use of an

adopter, Figure 1-5a. The adopter with the sam-
ple is placed in the slot at the top of the sample
table.

The sample table also has a special cutout and

groove to hold the reusable sample holder in
place and to align it properly for the analysis, Fig-
ure 1-5b. The reusable sample holder should be
cleaned with an ultrasonic bath and an environ-
mentally acceptable cleaning solution.

When performing fluid analysis, an important

Figure 1-5b, Sample Stand with Reusable Sample
consideration which has an effect on the repro- Holder in Place
ducibility of the analysis is the quantity of the to retard the flame and to minimize smoke which
sample introduced into the analytical gap. This will attenuate signal fuel. The cover works with
parameter is one for which the instrument cannot the disposable and reusable sample holders, Fig-
adjust. Proper level of oil in the sample holder is, ure 1-6a and Figure 1-6b.
therefore, part of any good operator technique.
Standards and samples are analyzed either in dis- The following sample stand preparation sequence
posable plastic sample holders or a reusable sam- should be followed to analyze samples that require
ple holder. In either case, it is recommended that the sample holder cover:
the sample holder be filled level with the top.
1. Install the disc electrode, Section 1.3
Sample holder covers are required when flamma-
ble fuel samples are analyzed. Since these samples 2. Install and position the reusable sample
might ignite during the analysis, a cover is used holder, Figure 1-5b. Raise the sample holder
in position and with a disposable pipette, fill

Figure 1-5a, Sample Stand with Disposable Sample Figure 1-6a, Sample Stand with Disposable Sample
Holder in Place Holder and Cover in Place

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  7

analytical gap. If this occurs, the high voltage will

not discharge across the analytical gap, but will
discharge along the lower resistance path causing
damage to the sample stand components.

To prevent arc-over, it is recommended that the

operator perform the simple cleaning procedures
outlined below.

WARNING
PROLONGED CONTACT WITH SOME SOL-
VENTS AND OILS MAY CAUSE CANCER!
Figure 1-6b, Sample Stand with Reusable Sample
Holder and Cover in Place
the sample holder with the fuel sample. Do
WARNING
not overfill the sample holder.
DO NOT USE ANY CHLORINATED SOL-
VENTS INTERNALLY OR EXTERNALLY ON
3. Place the cover over the reusable sample
THE INSTRUMENT!
holder and disc electrode. Note that the
cover only fits in one direction and has a
CAUTION: All chemicals should be used in ac-
cutout for the disc electrode shaft.
cordance with good laboratory practice. Proper
ventilation is required when using any solvent.
4. Install the rod electrode and set the gap, Sec-
Skin contact and prolonged exposure to fumes
tion 1.4.
produced by any solvent may be hazardous.
The sample is now ready for analysis.
1.6.1 Cleaning After Each Burn Cycle
Take the paper towel used to remove the disc elec-
When the analysis is complete, open the sample
trode from the shaft and clean the shaft, the sam-
stand door, remove the rod electrode, remove the
ple table, and the sample plate area between the
cover, lower the sample table, remove the sample,
disc electrode shaft and the rod electrode clamp.
and remove the disc electrode. The sample stand
is now ready for the next analysis.
1.6.2 Cleaning After Each Operating Shift
After 8 hours of operation, the complete sample
stand area must be wiped clean of the oil film
1.6 Cleaning the Sample Stand
buildup created by the burn cycles. If performed
routinely, the sample stand can be cleaned simply
The Spectroil M/F-W incorporates the rotat-
with paper towels and moderate rubbing. How-
ing disc arc emission technique for excitation of
ever, if this procedure is performed sporadically
the fluid sample. This technique produces a fine
or inadequately, an oil dispersant may be required
carbon residue which, when combined with oil
to remove the buildup. A general purpose foam
droplets, produces an oil coating over the sample
type spray detergent is recommended to dissolve
stand and door area. If allowed to accumulate, this
the oil film buildup. A spray detergent is capable
coating will collect the carbon particles and even-
of contacting those areas which are hard to reach.
tually produce a lower resistance path than the
Remove all detergent by wiping dry with paper
towel.
23 December 2009 / v.3.4.1
8  |  Operator’s Manual

1.6.3 Cleaning the Quartz Window 1.7 Paper Tissue for Operating and Paper
The quartz window that protects the lens and fi- Towels for Cleaning
ber optic must be cleaned frequently depending
upon the type of fluid being analyzed. In general, Disposable paper tissues and towels are recom-
this should be done at least every 5 burn cycles. mended for use in the daily operation of the
To clean the protective quartz window, take a Spectroil M/F-W. The type of paper tissue used to
clean, soft, disposable laboratory tissue and wet handle the disc electrodes is very important. Most
one corner of the towel with isopropyl rubbing household tissue paper is treated with certain ele-
alcohol or ammonia based window cleaner. With ments to make it softer or more absorbent. If used
the forefinger, rub the wetted portion of the pa- to handle the disc electrodes, these elements will
per towel along the surface of the window while contaminate the electrodes and produce erratic
applying moderate clockwise pressure on the results, especially for silicon. Therefore, it is rec-
window. This will disperse the oil film. Now take ommended that a laboratory grade paper tissue be
the dry portion of the paper towel and repeat this used for this operation.
procedure until no oil can be seen on the tissue
paper. A cotton swab can also be used for this Paper towels are useful to clean the sample stand
purpose. A diluted solution of ammonia and wa- components and wipe spills which occur during
ter may be used. routine operation. The type of paper towel used
for this function is not critical. Typical household
CAUTION: The lens protected by the window towels or C-fold janitorial towels work best for
does not require cleaning and should only be this function because of their absorbent character-
disassembled by a qualified engineer. istics.

CAUTION: Do not use solvents to clean this

window as they may selectively block or attenu- 1.8 Waste Oil Disposal Container
ate the passage of light necessary to determine A waste oil container for oil analysis applications
the presence and concentration of the elements in is required to properly dispose of the remaining oil
the oil samples. sample after the analysis cycle. It is recommended
that this waste oil container be in the form of a
1.6.4 Cleaning Solutions rectangular pan approximately 6 inches long, 4
The Spectroil M/F-W is designed to analyze pe- inches wide, and 1 inch deep, with a screened cov-
troleum and synthetic base products. In opera- er to permit the remaining oil to drain through the
tion, the handling and actual analysis of these screen. If a drain tube is installed on the bottom of
products create spillage and often leave an oily the waste oil container, the waste oil container can
film on the instrument. In general, these spills continuously empty into a large capacity reservoir
can be adequately cleaned simply by wiping the for proper disposal. Good laboratory procedures
surface with paper towels. There are occasions, should be exercised in the disposition of all waste
however, where the petroleum/synthetic product oils.
may require a detergent to dissolve the petroleum
base. For these occasions and for routine clean-
ing, a general purpose spray and wipe detergent
is recommended for internal and external instru-
ment components.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  9

tissue.
2.0 DAILY OPERATION
3. Turn printer ON and check to see that suf-
This section details those procedures that will be ficient paper is available. If the printer has an
routinely used in the day-to-day operation of the ON LINE light, it should be illuminated.
Spectroil MF-LD. The operator must be familiar
with the general operating requirements described 4. Ensure that an ample supply of sample hold-
in Section 1.0. A flow chart of the normal daily ers, sharpened electrodes and discs are on
routines is shown on the next page in Figure 2-1. hand.
For convenience, the parentheses after each step
in the chart refer to the corresponding sections in 5. Select standards for daily use and shake vig-
this chapter. The various procedures are explained orously for at least 30 seconds.
in brief, easy to follow step-by-step instructions.
6. Have an oil waste container on hand (Sec-
The spectroil M/F-W may be equipped with the tion 1.8).
optional sulfur capability. The procedure to ana-
lyze samples for sulfur is described in Section 2.9 7. Have cotton swabs, contaminant free tissue
of this manual. paper and paper towels on hand (Section
1.7).

2.1 Daily Routine Prior to Use

2.2 Warm-Up Procedure
1. Place the MODE switch on the operator’s
control panel to the OPERATE position, If the Spectroil M/F-W has been idle for several
Figure 2-2. Power will be applied to the hours, it may be necessary to conduct a series of
electrode sharpener and exhaust fans when burns to introduce light into the optics and to al-
MODE switch is in the OPERATE posi- low the electronics to become warm. This warm-
tion. up exercise can be conducted with any oil sample
or standard and can use electrodes which have
2. Verify positive action from the sample stand been burned before. It is recommended that at
exhaust system. With the sample stand door least three warm-up burns be conducted.
open, hold a piece of tissue paper up to the
exhaust filter. It should be sucked up and 1. Analyze or “burn” three or four samples (do
held in place against the filter. Remove the not burn the same sample more than twice
to prevent sample ignition) in accordance
with the instructions given in Section 2.3
Routine Sample Analysis.

NOTE: For the warm-up cycle only, the same disc

and rod electrodes can be utilized for up to four
consecutive burns but the electrodes have to be re-
gapped after each one.

2. The results produced by the warm-up burns

are of no use. Press function key 6 (F6)AV-
ERAGE . This prepares the screen for the
next analysis at which time the three warm-
Figure 2-2, Control Panel
up burns will be cleared.
23 December 2009 / v.3.4.1
10  |  Operator’s Manual

Daily Routine Prior to Use, (2.1)

Warm-Up Procedure, (2.2)

Daily
Daily Cleaning
Standardization Routine Sample
Check, (2.4)
OK Analysis, (2.3)
Prior to Securing,
(2.6)

Not OK
Standardization, (2.5)

Daily
Standardization
Check, (2.4)
OK

Not OK

Optical Profile Check, (2.7)

Electrode Offset Procedure, (4.3)

Standardization, (2.5)

Daily
Standardization
Check, (2.4) OK

Not OK

Acceptable
Accuracy Test, OK
(4.2)

Contact Spectro
Not OK Incorporated

Figure 2-1, Daily Operating Procedure Flow Chart

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  11

2.3 Routine Fuel Sample Analysis 2.3.1 Routine Fuel Sample Analysis of
Undiluted Samples
This paragraph gives the steps to follow to analyze The Spectroil M/F-W is set-up at the factory
or “burn” a fuel sample or a calibration standard with two routine analysis programs, one for light
using the disposable sample holders. Refer to the fuel and the other for heavy fuel. The appropri-
referenced sections for details. The various parts ate analysis program must be selected to coincide
referred to are shown with labels in Figure 2-1. with the type of fuel sample to be analyzed.
Refer to Section 2.9 if sulfur in fuel is to be ana-
lyzed. NOTE: When a new lot of disc electrodes is started,
either from a new manufacturer or a different lot
Most fuel samples can be analyzed without any from the same manufacturer, the disc electrode offset
preparation by pouring them into a ample holder. procedure of Section 4.4 must be performed.
However, #6 residual fuels must diluted in a 1:1
ratio with base oil prior to analysis, see Section NOTE: Rubber gloves or finger tip covers such
2.3.2. as Anti-static Nitrie COTS should be worn when
handling fuel samples, standards and consumables.
Note On Sample Contamination This will protect the user and minimizes contami-
nation.
The data generated by an analytical instru-
ment is only as good as the samples that are
The Spectroil M/F-W is set-up at the factory
provided. It is imperative that the fuel sam-
ple be taken from the same sampling point with two routine analysis programs, one for light
and in an approved and repeatable manner fuel and the other for heavy fuel. The appropri-
such as ASTM D 4057 Manual Sampling of ate analysis program must be selected to coincide
Petroleum and Petroleum Products. The with the type of fuel sample to be analyzed.
sampling container must be clean and free of
any contamination. In the laboratory, sample 1. The video monitor should display the Analy-
handling and analytical techniques are also sis Program screen, Figure 2-3. If a screen
important. Incorrect or careless procedures saver is in use, the Analysis Program screen
can influence analytical data that may lead to will not be displayed. Press any key on the
inaccurate data.
keyboard to terminate the screen saver and
re-display the Analysis Program screen.
Contamination through careless operation
can also be a source of error. The fuel sam-
ple and the graphite electrodes of the RDE The currently selected program is listed in the up-
spectrometer should never be touched by per left hand corner of the screen below the icons
hand. The electrodes must always be in-
stalled with a laboratory disposable towel to
avoid contamination from the fingers. Per-
spiration from the body will easily add sev-
eral parts per million of sodium to the analy-
sis. The the rod electrodes must be wiped
off before sharpening and the electrode
sharpener must be emptied and cleaned fre-
quently. Resulting errors, when not detected
can lead to erroneous conclusions and cost-
ly consequences about the status of the fuel
or the fuel treatment system. Although the
fuel analyzer is simple to operate, proper
housekeeping procedures must always be Figure 2-3, Sample Analysis Screen
followed.
23 December 2009 / v.3.4.1
12  |  Operator’s Manual

Figure 2-4, Select Program Screen

(Light Fuel in figure 2-3). If this is not the desired

program, select the correct one from the File pull-
down menu by selecting Open. A screen similar
to Figure 2-4 will appear. Click on the desired
programs radio button followed by OK.
Figure 2-6, Cover Placement on Disposable Sample
Holder
2. Install a carbon disc on the disc shaft using a NOTE: When light fuel samples are analyzed,
clean laboratory grade tissue to avoid contact reusable sample holders and sample holder covers
with fingers (Section 1.3). must be used to prevent sample ignition.

3. Place a disposable sample holder on the 5. Raise the sample table using the sample table
sample holder adopter and fill the holder positioning lever (sample fluid will contact
with sample to be analyzed, Figure 2-5. Be bottom of disc) (Section 1.5). See Section
sure to always fill sample holders to the rim 2-8 if Sample ID’s are to be entered.
(Section 1.5).
6. Place the cover on the disposable sample
NOTE: The adopter is not required when reusable holder and disc electrode, Figure 2-6. Note
sample holders are used. that the cover fits only in one direction and
has a cutout for the disc electrode shaft.
4. Place the adopter with the filled sample
holder on the table and slide it back to the 7. To install the rod electrode, press inward on
end of the groove on the table (Section 1.5). the black plastic knob of the spring loaded
rod electrode clamp to open the jaws of the
clamp. Insert a graphite rod electrode until
the tip of the carbon rod is in contact with
the disc electrode, then release the knob to
secure the electrode in the clamp.

8. Set the analytical gap mechanism by raising

and then lowering the analytical gap setting
lever. This will set a gap distance of 0.090
inches between the disc and rod electrodes
Figure 2-5, Disposable Sample Holder on Adopter (Section 1.4).

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  13

Turbine and Diesel Fuel by Rotating Disc Electrode

9. Close the sample stand door and press Atomic Emission Spectrometry can be obtained
the START button or function key 9 (F9) from ASTM International at www.astm.org.
START. The analysis cycle for light fuels is
48 seconds consisting of 24 seconds of pre- The 20% rule can be used to reject an analysis.
burn followed by 24 seconds of the analyti- View the analyses on the video screen and if one
cal cycle. of three, or up to two of five are more than 20%
different from the remainder, they should be re-
10. When the burn is complete, results will ap- jected. To reject an analysis, click on the sample
pear on the video screen. number to select the entire analysis and press the
DELETE key. Pour another sample and analyze
11. After the burn is complete, open the sam- it to replace the rejected one.
ple stand door and remove the rod electrode.
Set it aside for subsequent re-sharpening 16. When you are satisfied with the analyses, press
before it is used again. function key (F6) or click on the Averages icon to
complete the analysis procedure.
12. Lower the sample table, remove and discard
the sample holder and set aside the sample CAUTION: When all the fuel samples have been
cover for cleaning. analyzed, any disc electrodes that have been
dispensed from their holder should be set aside
CAUTION: The disc electrode will be hot to the for warm-up burn use only, or they should be
touch. discarded to avoid the possibility of picking up
contamination.
13. Using a paper towel to protect fingers from
the hot disc, remove and discard disc elec- 2.3.2 Sample Preparation for #6 Residual
trode. Fuels

14. Using a tissue or paper towel, wipe ex- Heavy fuel analysis, such as #6 residual, can be
cess, spilled or splattered sample fluid from accomplished using the RDE/AES analytical
sample table and disc electrode shaft. technique of the Spectroil M/F-W. The RDE/
AES technique has sufficient sensitivity as well as
NOTE: The quartz protective window should be dynamic range to detect low trace elements such
cleaned every burn. as sodium, potassium and lithium as well as con-
centrates of vanadium, lead, calcium, nickel etc.
15. The Spectroil M/F-W is now ready to analyze
another sample by again following the above 14 Due to the complex matrix of #6 residual fuels, all
steps. samples must be properly prepared through sam-
ple dilution prior to analysis in order to achieve
To improve precision and to comply withe ASTM full excitation of the elemental constituents. This
D 6728, the sample should be analyzed at least procedure has been developed to provide step-
three to five times and averaged. The spectroil by-step instructions on sample preparation of
M/F-W will calculate an average for the analyses #6 residual fuels for elemental analysis using the
on the screen when function key 6 (F6) or the Spectroil M/F-W spectrometer.
average icon are pressed.
2.3.2.1 Pre-Dilution Sample Heating
NOTE: A copy of ASTM D 6728 Standard Test Depending on the source of the crude oil that re-
Method for Determination of Contaminants in Gas sults in refined products, the heavy volatiles that

23 December 2009 / v.3.4.1

14  |  Operator’s Manual

constitute #6 residual fuels may or may not be the Spectroil M/F-W is also used as the diluent.
sufficiently viscous to pour at room temperature.
The dilution procedure can be performed by the
For good statistical analysis of the elemental con- gravimetric or volumetric method. Both tech-
tent of any #6 residual fuel, it is highly recom- niques will provide valid results, however, gravi-
mended that the sample of #6 fuel is preheated metric is preferred when absolute accuracy is a
and hand or mechanically shaken before decant- requirement. A laboratory balance is required if
ing for sample preparation and analysis. This pro- the dilution is to be performed by the gravimet-
cedure requires a variable temperature hot plate, ric method. For volumetric dilutions a graduated
and a metal container of sufficient size to hold cylinder or similar device can be used to measure
water plus the volume of the sample bottle con- equal volumes of diluent and sample.
taining the #6 residual fuel. A thermometer may
also be necessary if the hot plate does not have a The dilution procedure to prepare sufficient sam-
calibrated temperature control dial. ple for five analyses is as follows:

To heat the sample prior to dilution: 1. Remove the residual fuel sample bottle from
the temperature bath. Tighten the sample
1. Fill the metal container with water to a bottle lid to be sure the contents do not leak
height that will allow approximately 1/4 to out.
1/3 of the sample bottle to be immersed in
the water. Slightly crack the seal on the lid WARNING: The sample is hot! Use gloves to
of the fuel sample to permit gas pressure to protect hands and goggles to protect eyes. Wear a
escape as the sample heats. laboratory coat to protect against accidental spill-
age on body parts.
2. Place the metal container with water and
the fuel sample on the hot plate and adjust 2. Wipe the sample bottle dry then hand or
the temperature control on the hot plate mechanically agitate the fuel sample for
to a temperature of approximately 150° F 30-60 seconds.
(66°C). If the hot plate does not have a cali-
brated temperature dial, use a thermometer 3. Open the sample bottle to decant some of
to determine and control the temperature. the fuel sample.

3. Allow the sample to reach the set point tem- WARNING: Carefully crack open the sample
perature of 150° F (66°C) and stabilize for 5 container lid, contents may be under pressure.
minutes.
4. Using a new and clean disposable pipette,
4. Once the temperature has stabilized, it is decant a minimum of 50g of fuel sample
ready for sample agitation, decanting and into a new (clean) plastic sample container.
preparation. Follow the sample preparation
(dilution) procedure Section 2.3.2.2. 5. Using a new disposable pipette, add 50g of
75Cst base oil used for standardization of
2.3.2.2 Sample Dilution of # 6 Residual Fuel the Spectroil M/F-W spectrometer.
Once the fuel sample has reached the temperature
set point and has stabilized for at least 5 minutes, NOTE: For volumetric dilutions, measure and
it can be removed from the metal container, hand pour equal amounts of 75Cst base oil and fuel sam-
or mechanically shaken, then decanted for dilu- ple into a clean container. Approximately 15 ml of
tion. The 75Cst base oil used for calibration of base oil and sample is sufficient for five analyses.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  15

Table 2-1, Acceptable Range Indices for Daily

Standardization Check
6. Place the lid tightly on the plastic sample
container and hand or mechanically shake Concentration Maximum Minimum
the sample for a minimum of 30 seconds or Base Oil,
until it is 100% homogenous. 0.5 0.0
Na, K, Li
Base Oil
7. If necessary, place the sample container back (all elements except 1.0 0.0
into the water bath to raise the temperature Na, K and Li.
and restore the fluidity of the fuel/base oil
10 PPM 9.0 11.0
mixture. Agitate the fuel/base oil mixture
until it is homogeneous and ready for analy- 30 PPM 27.0 33.0
sis. 50 PPM 45.0 55.0
100 PPM 90.0 110
Once the sample has been prepared following the
procedures described above, it is ready to be ana- Daily Routine Prior to Use, Section 2.1.
lyzed on the Spectroil M/F-W spectrometer. The
Heavy Fuel Program is used to analyze #6 residual 2. Make 3-4 warm-up burns per Section 2.2.
fuel samples. Select the Heavy Fuel Program from
the File pull-down menu by selecting Open. A 3. Clean the quartz window.
screen similar to Figure 2-4 will appear. Click on
the Heavy Fuel Programs radio button followed 4. Make one burn of the HP Base standard.
by OK. Proceed with Routine Fuel Sample Anal-
ysis as described in Section 2.3. 5. Compare the results of this burn with Table
2-1. If all the elements are within the ac-
ceptable range, proceed to Step 7, 8, and
2.4 Daily Standardization Check 9. If the results are not within the range,
proceed to Step 7.
The standardization check is performed to verify
that the instrument has remained in calibration. 6. Make a two more (total of three) burns of
It is a quick method of verifying that the instru- the HP Base standard and press function key
ment can give accurate results without conduct- (F6) to average the results. If all elements
ing a full standardization. are within the range, proceed to step 7, 8,
and 9. If not, perform complete Standard-
This procedure requires that the operator analyze ization Procedure , Section 2.5, in accor-
three different levels of calibration standards and dance with the Daily Operating Procedure
compare the results to Table 2-1. The first stan- Flow Chart.
dard is a 0 ppm high-purity base oil (HP Base)
standard, the next is a 1 ppm standard for Na, K 7. Make one burn of the 1 ppm Na, K, Li stan-
and Li and finally a 10/30 ppm standard for the dard and repeat steps 5 and 6.
other elements.
8. Make one burn of the 10/30 ppm standard
The following steps should be conducted only af- and repeat steps 5 and 6.
ter the warm-up procedure has been completed
and the window has been cleaned in accordance 9. Daily Standardization Check is now com-
with Section 1.6.3. plete.

1. Prepare sample stand in accordance with

23 December 2009 / v.3.4.1

16  |  Operator’s Manual

2.5 Complete Standardization Ca, Zn and Mg are standardized using the 10/30
ppm standard. The 10/30 ppm standard contains
Complete standardization is a procedure per- 10 ppm of all these elements but 30 ppm of Mg.
formed to place the calibration of the instrument A third calibration point with a 100/300 ppm
as close to the standard values as the instrument standard is used to standardize all other elements.
originally produced during factory calibration. These concentration levels are programmed into
This procedure involves burning oil standards at the computer and are displayed at the appropriate
predetermined points along the calibration curve. time in the following procedure.
After these standards are analyzed, the computer
software will determine mathematical factors to NOTE: Calibration standards are not flammable
correct for any change in the calibration. Com- for normal analysis times and do not require a
plete standardization is performed under the fol- sample holder cover for analysis.
lowing conditions:
From the Analysis Program screen, press function
• When the instrument has been relocated to key 7 (F7), choose the Standardization icon, or se-
another site for operation. This is generally lect the Operations/Standardize pull down menu.
performed after the optical profile procedure The software will automatically clear all previous
has been completed. measurements from the video display. A dialog
• When results from the daily standardization with the name of the first calibration standard the
check fall outside of acceptable limits for instrument will expect to measure will appear. Re-
operation. fer to Figure, 2-7.
• After optical profiling procedure has been
performed. Three options exist when this dialog appears. The
first is to select the OK button which confirms
A complete standardization is performed by that the operator will begin to measure the 0 PPM
burning calibration standards that have been standard. The second option is to select the SKIP
pre-selected during factory calibration of the in- button indicating the operator does not intend or
strument. The concentration levels for complete need to measure the 0 PPM standard and wants to
standardization have been selected based on the increment to the next standard in the standardiza-
application and typical operating range for the el- tion process. The last option is to press CANCEL
ements of interest. and this action will terminate the standardization
routine completely and return the software to the
For the light fuel analysis application, all elements Analysis Program screen.
are standardized with a 0 ppm base oil standard
standard to determine the background level. For
a second calibration point, all other elements are
standardized using the 10/30 ppm standard. The
10/30 ppm standard contains 10 ppm of all ele-
ments but 30 ppm of Mg. These concentration
levels are programmed into the computer and are
displayed at the appropriate time in the following
procedure.

For the heavy fuel analysis application, all ele-

ments are standardized with a 0 ppm base oil
standard standard to determine the background
level. For a second calibration point, Na, K, Li, Figure 2-7, First Standardization Sample Dialog

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  17

In most cases, the OK button will be selected and one time. This will highlight the burn in a black
the dialog will disappear. Centered just below the background. Pressing the DELETE key on the
tool bar will be the name of the standard, 0 PPM keyboard one time will remove this measurement
in a red banner. This banner will remain there off of the screen. In the event that the wrong
until an average is made and the next standard measurement has been highlighted, position the
will appear. Those elements to be standardized pointer over the measurement again and left click
at this concentration level will have their values the mouse a second time. This will remove the
appear and those elements not standardized will highlight, then select the proper measurement to
have no values appear. reject and press the DELETE key.

NOTE: Reference channels are not standardized If a group of sequential measurements are to be
and therefore will not appear highlighted. rejected, for example measurements 3 through 7,
place the pointer over the first measurement (#3)
1. Select the 0 ppm standard and fill five and left click the mouse one time to highlight the
sample holders. Take care to always fill the measurement. Then move the pointer over the
sample holder to the rim. last measurement (#7) and hold the SHIFT key
down and left click the mouse one time. All mea-
2. With an optical lens cleaning solution (not surements from number 3 through number 7 will
containing silicon), isopropyl alcohol, or a be highlighted. Press the DELETE key to remove
window cleaning solution with ammonia, all five measurements.
clean the quartz window attached to the
Fiber Optic Lens Holder in accordance with 5. After making as many measurements as
Section 1.6.3. necessary to obtain a good average, press
function key 6 (F6), click the average icon,
3. Following procedures set forth in Section or select Operations/Average from the pull
2.3, burn all five samples of the 0 ppm down menu. The average of each element
standard. will be calculated and displayed below each
element’s column of measurements. To
4. On completion of Step 4, look at the read- make a printout of the measurements and
ings on the video screen. If one of the five their average, press the print icon. Auto-
burns does not appear to represent the other matically, the next dialog will appear provid-
four, it may be rejected. ing instructions to make measurement of the
10/30 ppm standard, Figure 2-8.
NOTE: The decision to accept or reject burns dur-
ing this procedure is at the discretion of the opera- 6. Select the 10/30 ppm standard and fill five
tor. Quite often an operator will know the cause of
a rejectable burn and therefore reject it almost auto-
matically. Rejectable burns can be caused by incon-
sistencies in consumables such as excess variation in
the specific density (hardness) of the disc electrode,
a loose fitting disc electrode, a poorly sharpened rod
electrode, an under- or over-filled sample holder or
an analytical gapping error.

To reject one of the measurements from the video

display, move the selection pointer over any por-
tion of the measurement and left click the mouse Figure 2-8, Second Standardization Sample

23 December 2009 / v.3.4.1

18  |  Operator’s Manual

sample holders. Take care to always fill the

sample holder to the rim.

7. With an optical lens cleaning solution (not

containing silicon), isopropyl alcohol, or a
window cleaning solution with ammonia,
clean the quartz window attached to the
Fiber Optic Lens Holder in accordance with
Section 1.6.3.

8. Following procedures set forth in Section

Figure 2-9, Third Standardization Sample
2.3, burn all five samples of the 10/30 ppm (Heavy Fuel Program Only))
standard.
window cleaning solution with ammonia,
9. On completion of Step 8, look at the read- clean the quartz window attached to the
ings on the video screen. If one of the five Fiber Optic Lens Holder in accordance with
burns does not appear to represent the other Section 1.6.3.
four, it may be rejected. Refer to the note re-
garding the 80% rule to determine if a burn 13. Following procedures set forth in Section
qualifies to be rejected. 2.3, burn all five samples of the 100/300
ppm standard.
10. After making as many measurements as
necessary to obtain a good average, press 14. On completion of Step 13, look at the
function key 6 (F6), click the average icon, readings on the video screen. If one of the
or select Operations/Average from the pull five burns does not appear to represent the
down menu. The average of each element other four, it may be rejected. Refer to the
will be calculated and displayed below each note regarding the 80% rule to determine if
element’s column of measurements. a burn qualifies to be rejected.

If the Light Fuel Program is selected, the standard- 15. After making as many measurements as
ization program will continue with step 16. If the necessary to obtain a good average, press
The Heavy Fuel Program is selected, to make a function key 6 (F6), click the average icon,
printout of the measurements and their average, or select Operations/Average from the pull
press the print icon. The procedure continues down menu. The average of each element
with the third calibration standard. will be calculated and displayed below each
element’s column of measurements. If there
Thee next dialog will appear providing instruc- are no additional standards to be measured
tions to make measurement with the next stan- as part of the standardization routine, next
dard. The name of the standard 100/300 ppm dialog to appear will indicate standardization
Figure 2-9. is complete and inquire if the average and
burns for the last standard measured should
11. Select the 100/300 ppm standard and fill be printed, Figure 2-10.
five sample holders. Take care to always fill
the sample holder to the rim. 16. Click on the Yes button if a printed copy of
the analyses is desired. After clicking on the
12. With an optical lens cleaning solution (not Yes or the No button, the Standardization
containing silicon), isopropyl alcohol, or a Values Screen, Figure 2-11 is displayed. This
table can also be displayed at any time by

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  19

Figure 2-10, Standardization Complete, Dialog

Figure 2-12, Standardization Factors Table (Example)

displayed on the screen by selecting Program/

Standardization Samples/Standardization Fac-
tors.

This table displays a factor for each element. At

best, the factor would be exactly 1.000. In prac-
tice, differences in electrode grades, standards,
and instrument variables will cause the intensi-
ties achieved to result in factors which are either
slightly above or below 1.000. These factors should
Figure 2-11, Standardization Values Table (Example) remain somewhere between 0.5 and 5.0. If a fac-
tor exceeds these tolerances, it is not always an
selecting Program/Standardization Samples/ indication of an error or pending problem. If such
Standardization Values. a case should occur, consult Spectro Incorporated
Field Service for analysis and explanation.
NOTE: It is strongly recommended that accurate
records of the complete standardization data be 18. A daily standardization check in accor-
kept for future reference. For this reason we highly dance with Section 2.4 should be carried out
recommend that printouts of all daily standardiza- to verify calibration.
tions be printed and kept on file. This data reflects
the current Spectroil M standardization. 19. Standardization is now complete and it is
possible to burn routine used oil samples.
The table in Figure 2-11 compares the expected
intensities (the intensities generated during fac-
tory calibration) to the obtained intensities (the 2.6 Daily Routine Prior to Securing
intensities obtained from the most recent com-
plete standardization). From the relationship of 1. Turn the MODE switch on the control
the expected intensities compared to the obtained panel to STANDBY.
intensities of the low standard and the high stan-
dard, the standardization factor is derived. 2. Turn the printer power switch OFF.
Another table is displayed after you click OK or 3. Remove disc and rod electrodes.
Cancel on the Standardization Values Screen, Fig-
ure 2-12. This second table is called the Stan- 4. Clean disc electrode shaft with a paper
dardization Factors Table. This table can also be
23 December 2009 / v.3.4.1
20  |  Operator’s Manual

towel. trodes in accordance with the appropriate

paragraphs of the General Operating Re-
5. Clean and wipe the entire sample stand area. quirements section of this manual.

6. Clean the quartz protective lens using a NOTE: it is important to only use the standard
clean soft disposable laboratory tissue. specified by the software profiling dialog for the
profiling procedure.
7. Wipe all oil standard bottles clean.
1. To begin the optical profile procedure press
8. Check supply of standards (don’t run out). function key 4 (F4), left click the profile
icon, or select Operations/Profile from the
9. Clean and wipe used oil container. pull down menu options.

10. Clean the working area. 2. The screen shown in Figure 2-13 appears
and calls for the first analysis of the profiling
11. Sharpen all rod electrodes and store them standard..
so they are protected from inadvertent con-
tamination. 3. Fill a sample holder with the profiling stan-
dard and following procedures set forth in
Section 2.3, to burn an oil sample.
2.7 Optical Profiling
4. At the completion of the burn, a screen
The Spectroil M/F-W optical system is shock similar to Figure 2-14 will appear with the
mounted in a light-sealed and environmentally profile log. The profile log shows the current
protected temperature stabilized enclosure. Con- profile for each chip, the previous profile and
sequently, the optics do not need to be profiled the difference between the two. The status
frequently. However, detection limit and repeat- for each chip should be OK, if not repeat
ability suffer when the optics are off profile. Un- the profile procedure one or two more times
fortunately, there is no one rule which ensures that until the status is OK for all chips. If this
the optics are on profile. The following guidelines condition cannot be achieved after three at-
are presented to indicate when profiling should tempts, contact Spectro for assistance.
be done:
• At least once every month. 5. Click on OK to return to the main analy-
• After the instrument has been transported to sis screen. The profiling procedure is now
a new location. complete.
• Whenever the instrument has been subjected
to temperature variations greater than 15° F
(10° C).

If one of these apply, it is also reasonable to per-

form a standardization as detailed in Section 2.5.

Follow the next steps as detailed in this procedure

to determine the optimum optical peak profile
position for operation.

1. Prepare the sample stand with new elec-

Figure 2-13, Optical Profile Screen

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  21

sample identification and name each of these field

segments.

Each field segment can also be auto-incremented,

which means that after the first sample number
is entered, and if all numbers that follow are in
numeric order, they can be automatically filled in
ascending order thus saving time.

The sequence of how the fields will appear can be

determined or altered and the size of each field
can be customized up to a maximum of 40 char-
Figure 2-14, Optical Profile Log acters total. The last column of the sample I.D.
dialog is for V4.2 protocol. This protocol is ca-
2.8 Sample Identification (I.D.)
pable of storing up to two segments of the sample
ID in the file. More than three segments are not
A sample identification (I.D.) can be added to
permitted. That portion of the sample identifi-
each analysis for identification purposes. The
cation that has V4.2 assigned as segment 1 or
ample I.D. can be configured by the user to in-
segment 2 will be transmitted or stored under the
clude a variety of information about the analyzed
V4.2 protocol.
sample. This section describes the setup process
to format the sample I.D. and how to enter it in
2.8.2 Using Sample ID.’s
routine operation.
When the Spectroil M/F-W is ready to analyze a
sample, the Sample I.D. can be entered by press-
2.8.1 Setup of the Sample I.D.
ing function key 3 (F3), or by clicking on the
To configure the format for the sample I.D., select
Sample I.D. icon. This menu option will pro-
“Sample I.D.” from the System pull-down menu.
duce a dialog to permit the entry of one single
This menu option produces a dialog, Figure 2-15,
ID, Figure 2-16, or provide the capability to pre
that can be configured by the user to meet any
enter multiple sample ID’s, Figure 2-17, using the
combination of alpha-numeric characters for
MULTIPLE button. Both dialogs are configured
global sample identification.
at the system level by the System/Sample ID op-
tion.
A sample can be identified by up to six field seg-
ments. This dialog permits the operator to choose
The Multiple Sample ID Entry dialog allows up
how many field segments will be used for the

Figure 2-15, System/Sample ID Setup Menu Figure 2-16, Single Sample ID Entry Menu

23 December 2009 / v.3.4.1

22  |  Operator’s Manual

Figure 2-17, Multiple Sample ID Entry Menu Figure 2-19, Sample ID File Selection Screen
to 50 sample identifications to be pre loaded to 2.9 Sulfur Analysis
facilitate rapid sample throughput. All sample ID
fields are configured at the system level through An optional sulfur analysis capability is available
the System/Sample ID menu option. Along the for the spectroil M/F-W. The optional capability
bottom of the Multiple ID dialog are buttons to consists of a separate sulfur optic attached to the
expedite the entry of sample numbers. The Copy right hand side of the sample stand and some mi-
button will copy the contents of one field and per- nor modifications to the sample stand. The sulfur
mit it to be copied into another field of equal or spectral line is in a region of the spectrum where
greater field size using the Paste button. Copy All any signal resulting from the excitation process
will copy one sample and insert it into all remain- is absorbed by air. For this reason, when sulfur
ing empty fields in that column. If that column analysis is required, the sample stand area and the
is set for auto increment, the sample number will optic must be purged with an inert gas so that the
increase one value per row. Insert, Delete, and CCD detector is able to see the sulfur signal gen-
Clear are self-explanatory. erated at the analytical gap. To solve this problem,
the Spectroil M/F-W uses nitrogen as a gas and a
Click load to proceed. The first time that this op- separate optic just for the sulfur capability.
tion is enabled, an input file layout screen, Figure
2-18 appears and must be filled in with the user 2.9.1 Set-up for Sulfur Analysis
layout preferences. Click OK when complete and Follow this procedure to prepare the sulfur optic
the a screen enabling the user to select the sample for routine analysis.
ID files appears, Figure 2-19.
1. Attach a low pressure regulator onto a
Nitrogen bottle or other nitrogen source.
The output of the regulator should have a
1/4 inch barbed quick disconnect, or ferrule
hose fitting

2. Attach the 1/4 inch ID (inner diameter)

hose that comes out of the back of the sulfur
optic to the 1/4 inch barbed quick discon-
nect, or ferrule hose fitting on the regulator.
Verify that all hose fittings are secure and
no pressure leaks are present. Teflon tape
Figure 2-18, Sample ID File Layout Preference Screen should be used on all threaded hose fittings.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  23

CAUTION: Pressure leaks will cause the intro-

duction of fresh air to the purge path and will
result in low readings for sulfur.

Sulfur is analyzed separately from the other ele-

ments, therefore the sample stand must be set-up
so that the excitation process is viewed by the sul-
fur optic and not the routine optic. The excita-
tion process can be selectively viewed to the left
by way of the sulfur light pipe, or to the right for
the routine analysis by way of the lens assembly.

3. To activate the view to the sulfur optic, Figure 2-21, “L” Bracket Installed Covering Lens
the “L” bracket must be removed from the Assembly
sulfur optic light pipe. Unscrew the round knurled nut. Verify that the other “L” bracket over
knurled nut that holds the “L” bracket in the lens assembly is in the “down” position.
place and remove it from in front of the
sulfur light pipe, Figure 2-20 5. Open the nitrogen bottle to allow the nitro-
gen to pass through the regulator, adjust the
4. Relocate the “L” bracket over the lens as- regulator to approximately 25 PSI.
sembly of the routine optic located to the
left of the analytical gap, Figure 2-21. Use 6. Turn the main Nitrogen valve on the sulfur
the round knurled nut to fasten it in the optic control panel to “ON”, Figure 2-22.
new location. This will help to keep the lens
assembly clean during the sulfur analysis. 7. If the Spectroil M/F-WLD is OFF, turn it
ON by raising the circuit breaker (CB1)
NOTE: Some instruments may be delivered with on the right side of the instrument. The
two “L” brackets installed. When that is the case, spectrometer will power up and the OilM
loosen the round knurled nut, flip up the “L” brack- Windows software program will load.
et for the sulfur light pipe and tighten the round

Figure 2-20, “L” Bracket Installed Covering Sulfur Optic

Light Pipe Figure 2-22, Sulfur Optic Control Panel

23 December 2009 / v.3.4.1

24  |  Operator’s Manual

8. Depress the “OPTIC PURGE” button, Fig- Note: During the profiling procedure, both optics
ure 2-22, on the sulfur optic control panel must see the analytical gap. Make sure the “L”
for 5 seconds, and release for 5 seconds. brackets are removed from the sulfur light pipe and
Repeat this process 5 times to flush the opti- the lens assembly. If two “L” brackets are installed,
cal system. they should be in the up position.

9. To get load the Sulfur program select File 2.9.3 Standardization of the Sulfur Optic
from the pull down menu options, then The software must be in the sulfur program to
Open. A list of available programs will be perform this function. If not, see step 9 in Sec-
displayed. Select the radio button for the tion 2.9.1.
Main Sulfur program and press OK. The
sulfur optic is now ready for operation. 1. From the main analysis screen, press func-
tion key 7 (F7), choose the Standardization
WARNING: Irritating and toxic hydrogen sul- icon or select the Operations/Standardize
fide gas may be found in confined vapor spaces pull down menu. The software will auto-
when samples with large percentages of sulfur are matically clear all previous measurements
analyzed. Greater than 15 - 20 ppm continu- from the video display. A dialog box with
ous exposure (in air, not to be confused with the the name of the first calibration standard the
liquid calibration standard) can cause mucous instrument will expect to measure will ap-
membrane and respiratory tract irritation. pear. A blank oil is used or this step and the
50 - 500 ppm can cause headache, nausea, and dialog box may call for “Base Oil”, “Blank
dizziness, loss of reasoning and balance, difficulty Oil”, or 0 PPM Oil.
in breathing, fluid in the lungs, and possible loss
of consciousness. Greater than 500 ppm can cause 2. Following the procedure set forth in Sec-
rapid or immediate unconsciousness due to respi- tion 2.3, burn three samples of Base/Blank
ratory paralysis and death by suffocation unless oil and press function key 6 (F6), click the
the victim is removed from exposure and success- Average icon or select Operations/Average
fully resuscitated. from the pull down menu to average them.
To make a printout of the measurements
The “rotten egg” odor of hydrogen sulfide is not a and their average, press the print icon. Au-
reliable indicator for warning of exposure, since tomatically, the next dialog box will appear
olfactory fatigue (loss of smell) readily occurs, es- providing instructions to make measure-
pecially at concentrations above 50 ppm. At high ments of the next standard. The concentra-
concentrations, the victim may not even recog- tion of this standard is 1,000 PPM The
nize the odor before becoming unconscious. name in the dialog box will vary depending
on the calibration of the Spectroil M/F-W
2.9.2 Profiling the sulfur Optic which can be or light fuel, heavy fuel, crude
The sulfur optic is profiled at the same time as the oil, residual oil or # 2 diesel fuel.
standard optic. Profiling should be performed if
the instrument has been relocated and or shut off 3. Following the procedure set forth in Section
for an extended period of time. 2.3, burn the three samples of the 1,000
PPM sulfur standard and press function key
The Nitrogen purge should be turned OFF at the 6 (F6), click the Average icon or select Op-
sulfur optic control panel during profiling. To erations/Average from the pull down menu
profile the optic, follow the instructions in Sec- to average them.
tion 2. 7 in this manual.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  25

4. The next dialog box that appears will indi- pipe bracket and flip up the lens assembly
cate standardization is complete and inquire bracket.
if the average and burns for the last standard
measured should be printed, select YES. 3. Place the Mode/Operate switch on the
Spectroil M/F-W control panel to STAND-
5. After confirmation that the burn data and BY.
average are to be printed, the last dialog
box to appear will inquire if the Factors and 4. Thoroughly clean the sample stand area, es-
Offsets should be printed, again select YES. pecially the quartz window and gap sensors.
The Standardization procedure is now com- They will be extremely dirty since the nitro-
plete. Review the factor for sulfur; it should gen was blowing the sample flame towards
be close to one, +/- 20 %. the left side of the sample stand during the
sulfur analysis.
2.9.3 Verification
It is good practice to verify calibration after the
Spectroil M/F-W has been standardized. 2.10 Water Analysis

1. In PPM mode, run five samples of each cali- This section describes how to set up the Spectroil
bration standard in the set. Print all burns, M/F-W for the optional elemental analysis of tur-
averages and statistics. Remember the read- bine cleaning water and NOx suppression water.
ings are displayed in percentages.
The optional water method is used for the analysis
2. Depending on the type of standard analyzed, of corrosive elements in water in support of gas
the averages should be better than +/- 15%. turbine operations. The method provides rapid
If not, repeat the standardization procedure, analysis of sodium, lithium, potassium and other
Section 2.9.3 and if it does, proceed with elements in water that is introduced into the en-
step 3. gine combustor for the purpose of suppressing the
oxides of nitrogen (NOx) in the exhaust gases and
3. Routine samples are analyzed for sulfur water used for on-line compressor cleaning and
content per the procedure in Section 2.3, crank-soak compressor cleaning. All the elements
Routine Sample Analysis. are analyzed in less than one minute and without
auxiliary gases or the need for sample prepara-
2.9.4 Clean Up and Final Checks tion.
This section provides the steps that must be per-
formed when the sulfur analysis procedure is com- The RDE-AES technique of the Spectroil M/F-W
plete nd the Spectroil M/F-W will be used for the has been accepted by turbine and fuel treatment
analysis of routine furl samples. system manufactures as the ideal on-site analy-
sis instrument for metallic contaminants in fuel.
1. Turn the Main Nitrogen valve “OFF”. However, turbine manufacturers actually limit
the total concentration of alkali metals ingested
2. Remove the interchangeable “L” bracket by the turbine from all sources. This includes not
from the lens assembly and place over the just fuel, but also contamination in compressor
end of the sulfur light pipe in the sample inlet air, steam/water injection for NOx control
stand. This will prevent any oil from travel- and cleaning water. A need thus exists for the on-
ing down the pipe and contaminating the site analysis of alkali metals in water. .
sulfur optic lens assembly. If two “L” brack-
ets are installed, flip down the sulfur light

23 December 2009 / v.3.4.1

26  |  Operator’s Manual

2.10.1 Water Program Standardization

In order to prepare the Spectroil M/F-W for the
analysis of water samples, the software must be in
the “WATER” program.

1. To load the WATER program, select File

from the pull down menu options, then
Open. A list of available programs will
be displayed, Figure 2-23. Select the radio
button for the WATER (MAIN WATER Figure 2-25, First Water Program Standardization Point
PROGRAM) and press OK. The program
is now loaded and ready for the standardiza- 3. Following the procedure set forth in Section
tion procedure. 2.3, burn three samples of D.I. Water and
press function key 6 (F6), click the Average
2. From the main analysis screen, Figure 2-24, icon or select Operations/Average from the
press function key 7 (F7), choose the Stan- pull down menu to average them. To make
dardization icon or select the Operations/ a printout of the measurements and their
Standardize pull down menu. The software average, press the print icon. Automatically,
will automatically clear all previous measure- the next dialog box will appear providing
ments from the video display. A dialog box instructions to make measurements of the
with the name of the first calibration stan- Water standard, Figure 2-26.
dard the instrument will expect to measure
will appear. A blank water sample is used The Water standard is a multi level standard and
or this step and the dialog box will call for the included elements and their concentration are
“D.I. Water, Figure 2-25. stated on its label.

4. Following the procedure set forth in Section

2.3, burn the three samples of the Water
standard and press function key 6 (F6), click
the Average icon or select Operations/Aver-
age from the pull down menu to average
them.

4. The next dialog box that appears will indi-

cate standardization is complete and inquire
if the average and burns for the last standard

Figure 2-23, Select Program Screen

Figure 2-26, Second Water Program Standardization

Figure 2-24, Main Water Analysis Screen Point

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  27

Figure 2-27, Standardization Couplet, Dialog

measured should be printed, select YES,

Figure 2-27.

5. After confirmation that the burn data and

average are to be printed, the last dialog
box to appear will inquire if the Factors
and Offsets should be printed, again select
YES. The Standardization procedure is now
complete. Review the factors, they should
be close to 1, +/- 20 %.

2.10.2 Verification
It is good practice to verify calibration after the
Spectroil M/F-W has been standardized.

1. In PPM mode, run five samples of the Water

standard. Print all burns, averages and sta-
tistics.

2. Depending on the type of standard analyzed,

the averages should be better than +/- 15%
for the concentrations listed on the Water
standard bottle. If not, repeat the standard-
ization procedure, Section 2.10.1.

2.10.3 Routine Water Sample Analysis

Water samples are analyzed on the Spectroil M/F-
W as described in Section 2.3, Routine Sample
Analysis.

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28  |  Operator’s Manual

3.0 OPERATOR MAINTENANCE 3.2 Scheduled Periodic Maintenance

To maintain the Spectroil M/F-W performance, This section of the manual details the mainte-
periodic maintenance must be performed by the nance action that is required to be performed
operator. This maintenance falls into two catego- on the Spectroil M/F-W at regularly scheduled
ries: intervals. Periodic maintenance will keep the
• Daily Maintenance instrument in good working condition and help
• Scheduled Maintenance to identify sources of future trouble before they
cause serious downtime. The following tables
separate periodic maintenance inspections by
3.1 Daily Operator Maintenance subassembly and item. Each item has instruc-
This section details the maintenance actions re- tions on what maintenance action is required,
quired of the operator on a daily basis. These the interval in which the maintenance should be
maintenance actions pertain mainly to the opera- performed and by which maintenance level.
tor accessible assemblies such as the sample stand,
the readout and control panel, and the automatic The scheduled maintenance tables are as fol-
printer. Any maintenance that is required to be lows:
performed in the excitation source, optics, or • Table 3-2, External Housing Inspections
computer electronics is strictly limited to techni- • Table 3-3, Internal Housing Maintenance
cally skilled personnel. Inspections
• Table 3-4, Excitation Source and Power
Table 3-1 lists each maintenance action that is au- Distribution Maintenance Inspections
thorized and required of the operator. • Table 3-5, Microprocessor Maintenance
Inspections

TABLE 3-1
DAILY OPERATOR MAINTENANCE

CAUTION: Do not use alcohol or Chlorinated Solvents to clean plastic or painted surfaces.

Component Required Maintenance Frequency Maintenance Level

Clean to remove oil and carbon
Plate, Mounting, Sample buildup especially between disc
Every 5 burns Operator
Stand Component electrode shaft and rod electrode
holder. refer to Section 1.6.
Clean to remove oil and carbon
Window, Quartz, Protec- splashes with isopropyl alcohol or
Every 5 burns Operator
tive an ammonia based window cleaner.
Refer to Section 1.6.3.
Using a Q-tip, clean to remove oil
and carbon splashes with isopropyl
Sensors, Sample Stand Daily Operator
alcohol or an ammonia based win-
dow cleaner. Refer to Figure 1-4.
Clean complete sample chamber
Sample Stand Area to remove oil splashes and carbon Twice Daily Operator
buildup. Refer to Section 1.6.2.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  29

Clean complete door to remove oil

Door, Sample Stand splashes and carbon buildup. Refer Twice Daily Operator
to Section 1.6.
Rotate cutting blade to new edge.
(Can be performed until all three edg-
Electrode Sharpener As Required Operator
es have been used.) Refer to Section
3.3.
Inspect for oil splashes and carbon
Panel, Readout and
residue. If present, remove with mild Daily Operator
Control
cleaning detergent.
Inspect for oil splashes and dust
buildup. If present, remove with mild
detergent.
Frame and Exterior CAUTION: DO NOT USE Daily Operator
Panels
ALCOHOL OR CHLORINATED
SOLVENTS TO CLEAN PLAS-
TIC OR PAINTED SURFACES.
Inspect for worn ribbon, loose cable
connectors, and dirt and dust buildup.
Replace worn ribbon, tighten loose
Printer Daily Operator
connections and clean accordingly.
Refer to printer operation and main-
tenance manual.

TABLE 3-2
EXTERNAL HOUSING MAINTENANCE INSPECTIONS

Component Required Maintenance Frequency Maintenance Level

Weekly or as
Inspect for dust and dirt buildup.
Filter on Heat required depend-
Clean in detergent and water bath Operator
Exchanger ing on operating
by swishing vigorously.
environment.
Inspect for dust and dirt buildup.
Filter, Sample Stand
Clean or replace if holes in the filter Weekly Operator
Exhaust
are blocked.
Inspect for oil, dust, dents, scratches
Frame and Exterior
and rust. Clean with mild detergent Monthly Operator
Panels
and if necessary, sand and repaint.
Inspect for loose or missing hard-
Hardware ware. Tighten loose hardware and Monthly Operator
replace rusted hardware.
Inspect for loose connections. In-
External Cables Monthly Operator
spect for damage.
Clean residue (varnish) from splined
Shaft, Disc Electrode Monthly Operator
end with an ink eraser.

23 December 2009 / v.3.4.1

30  |  Operator’s Manual

TABLE 3-3
INTERNAL HOUSING MAINTENANCE INSPECTIONS

Component Required Maintenance Frequency Maintenance Level

Inspect for smooth rotation. Check
for dust and dirt buildup on blades.
Fans Replace if binding is evident. Clean Six Months Operator
blades if necessary.
Frequency - Six months
Inspect for broken or bent wiring
Wiring connections. Inspect for frayed or Six Months Operator
burned insulation.
Inspect for open or over rated fuse Six Months or as
Fuses Operator
usage. Replace as required. Required
Inspect for good electrical connec- Six Months or as
Transformers Operator
tion and signs of overheating. Required
Inspect for dust and dirt buildup.With
Video Monitor Six Months Operator
a soft cloth, wipe clean if necessary.
Inspect all connectors for proper
seating in sockets.
CAUTION: Do not remove or
Signal Connectors connect any signal cables with the Six Months Operator
power on.

TABLE 3-4
EXCITATION SOURCE AND POWER DISTRIBUTION MAINTENANCE INSPECTION

Component Required Maintenance Frequency Maintenance Level

Inspect the board for proper connec- Six Months or as Operator/Technician
tor seating. Inspect for burn marks or Required
Component
discolored components. Inspect lower
Mounting Boards
cabinet for dust and dirt buildup. Vacuum
if necessary.
Check each capacitor for signs of bulg- Six Months or as Operator/Technician
ing, discolored containers or signs of Required
Capacitors
leaking. Replace if signs of overheating
are evident.
Check each resistor for signs of bulging Six Months or as Operator/Technician
Resistors or discoloration. Replace if overheating Required
is evident.
Inspect for good electrical connection. Six Months or as Operator/Technician
Contactors Observe relay operation. Replace if Required
intermittent or sluggish.
Inspect for signs of arc-over and over- Six Months Operator/Technician
Transformers
heating. Replace if evident.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  31

Inspect the rod electrode holder and Six Months or Operator/Technician

gap setting device for smooth sliding Every 2,000
and release. If tight or binding, adjust or Burns
Analytical Gap remove and replace gap setting device,
refer to the Maintenance Manual Section
2.4.1.1. Check the analytical gap dis-
tance. It should be 0.090 inches.
Polish tips to remove corrosion. Six Months or Operator/Technician
Auxiliary Gap Every 2,000
Burns
Check electrode shape. If electrode Six Months or Operator/Technician
points are flat, remove electrodes and Every 2,000
replace them. At sea level, reset the Burns
auxiliary gap distance to approximately
Auxiliary Gap
0.135 inches. Verify distance by check-
ing excitation source frequency with
Source Frequency Test Meter (refer to
the Maintenance Manual Section 2.2.)
Motor, Disc Elec- Check motor rotation. If loose or binding, Six Months Operator/Technician
trode align and tighten.
Check high voltage cables in the ex- Six Months Operator/Technician
citation source for signs of arc-over or
Cables damage. Check electrical connections.
Replace cables if arc-over is evident.
Tighten connections if loose.
Check to be sure that the disc electrode Six Months Operator/Technician
shaft is tight and properly aligned. See
Shaft, Disc Elec-
the Maintenance Manual Section 2.4.1.2
trode
for replacement procedure and tracking
check.
Check the alignment. If the rod point is Six Months Operator/Technician
Disc Electrode
more than 25% away from disc center,
to Rod Electrode
adjust. See the Maintenance Manual
Alignment
Section 2.4.1.3
Check for smooth rotation and cleanli- Six Months or Operator/Technician
Auxiliary Gap Fan ness. Clean if necessary. Every 2,000
Burns

23 December 2009 / v.3.4.1

32  |  Operator’s Manual

TABLE 3-5
MICROPROCESSOR MAINTENANCE INSPECTIONS

Component Required Maintenance Frequency Maintenance Level

Inspect each card for signs of discol-
oration due to component overheat-
Printed Circuit ing. If present, replace the appropri- Operator/Techni-
Six Months
Assemblies ate card. Check each card for proper cian
connector seating. Re-seat if neces-
sary.
Inspect each fiber optic in the M58000
and M59200 cards for a tight mount-
ing. If loose, remove the fiber and re- Operator/Techni-
Optical Fibers Six Months
seat. If broken, replace. cian
Frequency - Six months

Check both connectors of each inter-

connecting cable. If loose, Re-seat
the connector in the appropriate plug. Operator/Techni-
Cables, Interconnecting Six Months
If broken or damaged, replace. cian
CAUTION: Do not remove or connect
any signal cables with the power on.

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  33

3.3 Procedure to Replace Electrode Sharpener 4.0 PERFORMING CALIBRATION

Cutter Blade, M90102 CURVE VERIFICATION

The cutter blade has three sharpened edges and The purpose of performing a calibration curve
can thus be used three times before it is replaced. verification is to determine if the instrument re-
peats the curve generated at the factory or by an
To replace or rotate the cutter blade to a new cut- authorized service representative.
ting edge, unplug the sharpener power connector
J2 at the power connection plate. Next, remove To perform a calibration curve verification, the in-
the graphite collector barrel assembly to empty strument must first be standardized. Refer to Sec-
out any accumulated graphite and to expose the tion 2.5 in this manual for a detailed procedure
cutter blade, Figure 3-1. on daily standardization. When the instrument
has been standardized using the calibration stan-
To remove the barrel assembly, locate the sharp- dards for the new program, the calibration curve
ener over a waste basket with the collector barrel verification can be performed.
pointing downward. Grasp the barrel with the
opposite hand and rotate it while pulling it away The calibration curve verification consists of per-
from the motor mount and face plate. Once the forming an analysis of each synthesized standard
O-ring disengages the face plate, it will be easy as if it were an unknown sample. It is recom-
to separate and empty. Use a flat blade screw mended that the operator conduct te n analyses
driver to remove the #4-40 screw which mounts of each standard and perform statistics on the
the cutter blade, see Figure 2-14. When replac- measurements to obtain the average and standard
ing or rotating the cutter blade, be sure to place deviation for each element. Instrument perfor-
the rear edge of the cutter blade tight against the mance for alkali metal analysis should be within
cutter head. This is the reference point to achieve the limits listed in Table 4-1.
the correct angle on the graphite rod electrode.
Replace the barrel assembly and reconnect the
sharpener to its power connector. 4.1 Repeatability Testing

Perhaps one of the most important technical char-

acteristics of a spectrometer is its ability to perform
the same measurement over and over again with
the same result. This characteristic is referred to as
repeatability, reproducibility, sigma, standard de-
viation or precision. Repeatability is determined
by the standard deviation of a series of measure-
ments made on the same sample. Mathematically,
standard deviation is calculated as:

Std. Dev.= [N(∑Xi2) - (∑Xi)2] / [N(N-1)]

where:
N = the number of analyses (normally 10)
Figure 3-1, Electrode Sharpener Blade

∑Xi2 = is the sum of the 10 squared individual

measurements

23 December 2009 / v.3.4.1

34  |  Operator’s Manual

(∑Xi)2 = is the square of the sum of the 10

individual measurements. The average of ten burns should be used to de-
termine the reading of a particular standard. Ac-
For the purpose of conveniently comparing the curacy failures at low concentrations may be due
standard deviation to the mean for a series of mea- to contamination and spot impurities in the disc
surements, relative standard deviation, or R.S.D., electrodes. The effect of the contamination and
is used. R.S.D. expresses the standard deviation as impurities can be compensated for by perform-
a percent of the mean and is calculated as: ing the electrode offset procedure in Section 4.4.
Spectro Incorporated Field Service should be con-
R.S.D. = 100[Std. Dev./Xavg] sulted if the Spectroil M/F-W is unable to meet
the accuracy criteria presented in Tables 4-1.
The Spectroil M/F-W automatically calculates
mean, standard deviation and R.S.D. for a series
of measurements by pressing function key 5 (F5), 4.3 Factors Affecting Repeatability and
see Section 5.4.8.9 for a description of this func- Accuracy
tion.
Many factors affect repeatability and accuracy on
NOTE: At 0 ppm, R.S.D. is not considered a actual fuel sample. Among them are:
valid statistic. A minimum of three warm-up burns
must be made prior to the performance of statistical 1. The sample must be homogenous. The ac-
analysis. curacy test done at Spectro is always done
with standards. Routine samples are never
used for repeatability and accuracy testing
4.2 Accuracy because it cannot be assured they do not
contain agglomerates, second phases and
Accuracy is the ability of a spectrometer to give large particulates, all of which will affect
the correct concentration value of a standard. repeatability and accuracy.
Accuracy requirements for fuel analysis are tighter
than those for wear metals. Even extremely low 2. The Spectroil M/F-W must be on profile. If
concentrations of contaminants such as sodium, analytical lines are off profile, the repeatabil-
potassium or lithium in the fuel can have detri- ity will be adversely affected. If the repeat-
mental affects on a gas turbine. Typical perfor- ability specifications cannot be met, one of
mance requirements for the Spectroil M/F-W for the first diagnostic tests is to check profile
fuel analysis are shown in Table 4-1. (Section 2.7).

Table 4-1,Performance Specifications for Key Fuel Elements

Contaminant Range in PPM, Accuracy Table

K 0.0 to 1.0 ppm, +/- 0.1 ppm 1.0 to 20 ppm, +/- 10% >20 ppm, +/- 15%
Na 0.0 to 1.0 ppm, +/- 0.1 ppm 1.0 to 20 ppm, +/- 10% >20 ppm, +/- 15%
Ca 0.0 to 2.0 ppm, +/- 0.2 ppm >2.0 ppm, +/- 10%
Mg 0.0 to 2.0 ppm, +/- 0.2 ppm >2.0 ppm, +/- 10%
V 0.0 to 8.0 ppm, +/- 0.8 ppm >8.0 ppm, +/- 10%
Pb 0.0 to 8.0 ppm, +/- 0.8 ppm >8.0 ppm, +/- 10%

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  35

that Spectro Incorporated Field Service be con-

3. The quality and handling of the disc and sulted. It is strongly recommended that adjust-
rod electrodes will affect repeatability and ments to the sample stand as described in item 8
accuracy. The density, and hence the poros- above be made only by Spectro personnel or at the
ity, residual contamination and dimensional direction of Spectro personnel.
accuracy of the disc and rod electrodes will
affect repeatability. Care must be taken to
properly sharpen the rod electrode (Sec- 4.4 Disc Electrode Offset Procedure
tion 1.2). Proper care must also be exercised The Spectroil M/F-W is designed to incorporate a
when installing the electrodes (Sections 1.3 background measurement and correction system.
and 1.4). T he purpose of this system is to offset or null the
output of all CCD chips when measuring a 0 ppm
4. The sample must be homogenized by shak- standard. This is also known as measuring back-
ing before filling the sample holders. ground light because 0 ppm has no concentration
of elements present in the sample. Therefore, the
5. The sample holders must be filled to the light produced when analyzing a 0 ppm standard
same level (Section 1.5). must only be background emission. This is, how-
ever, only true in theory.
6. Line voltage to the Spectroil M/F-W must
be within specification. In practice, elemental contamination is present
in everything used for the analysis process. The
7. Electronic stability of the Spectroil M/F-W sample holders may pick up contamination from
will affect repeatability. the environment, the 0 ppm standard may have
sub-ppm trace levels of certain elements, and the
8. Sample stand geometry will affect repeat- graphite disc electrodes are known to have trace
ability. The rod electrode to disc electrode contamination of certain elements. Manufac-
gap distance, the quartz lens assembly to turers of graphite electrodes commonly list and
arc distance, the position of the fiber optic quantify the known trace or spot impurities on
within the lens assembly mounting block, each box of disc electrodes. The purpose of this
and the angle of the quartz lens assembly procedure is to offset these trace contaminates in
with respect to the arc will affect not only the consumables and is absolutely necessary to be
the intensity of the light entering the en- performed.
trance slit of the polychromator (optical as-
sembly), but will also affect the repeatability This procedure should be performed every time a
. These adjustments to the Spectroil M/F-W new batch and/or lot number of disc electrodes are
are optimized at the factory. to be used. For maximum efficiency in a labora-
tory operation, all graphite disc electrodes should
9. A variety of mechanical or electronic faults be grouped and stored by batch and lot number.
could degrade repeatability and accuracy. Only one batch or lot should be used at a time
Among these are faulty CCD chips, damage until it is totally consumed. Once a new lot is
to the entrance slit, or damage to the fiber opened and the instrument is standardized to the
optic cable. new lot, the low end of the calibration curve (5
ppm and/or 10 ppm) should always be checked.
The operator has control over the first five factors. If accuracy at these levels fails to meet the speci-
If care is taken to properly operate the Spectroil fied criteria, it may be due to variance in trace
M/F-W and accuracy is still worse than specifica- contaminants levels and the following procedure
tion and it is on profile, then it is recommended should be performed to correct for the presence of

23 December 2009 / v.3.4.1

36  |  Operator’s Manual

this contamination.

1. To perform the disc electrode offsets opera-

tion, the operator can select function key
10 (F10), left click the disc electrode offsets
icon or choose Operations/Offsets/Perform
Disc Offsets from the pull down menu op-
tions.

NOTE: The software has now been placed in a

mode that is not to be used for normal operation.
“Disc Electrode Offset” appears highlighted in red
across the top of the analysis program screen to draw
attention to the fact that this is not a normal condi-
tion for operation. Once this procedure is complet-
ed, the readout mode will have to be restored to the
Figure 4-1,Sample Background Correction Factors
instrument’s normal operating condition.
in the forward or peak measurement is iden-
2. Prepare five sample holders of the 0 ppm oil tical to the intensity produced in the reverse
standard. The screen will automatically clear or background measurement.
any previous measurements when this mode
is selected. Using the new batch or lot of 5. The purpose of this procedure is to set the
disc electrodes, burn these five samples in ac- new ratio calculated and shown on the F/R
cordance with the routine operating proce- RATIO column into the BKG FACTOR
dures outlined in Section 2.3. column for most elements.

3. After all five samples have been burned, NOTE: It is extremely important to pay attention
press function key 6 (F6), the average icon, to which elements this ratio is applied. Not all ele-
or Operations/Average to calculate the aver- ments have a background factor as indicated by the
age of the five measurements. Once the value 0.00000. For the elements specified below*,
average is calculated, a dialog with the title do not set the F/R RATIO value in the BKG FAC-
Background Correction Factors will appear TOR column. Failure to do so will adversely affect
on the screen. This table will vary from the analytical results of the instrument!
instrument depending on the analytical con- *Spectroil M/F - MgHi 518.36, C 387.10 and H 486.133.
figuration of the spectrometer; however, the
format is the same as shown in Figure 4-1. 6. The cursor will automatically be located
in the first row of the background factor
4. This dialog will display (from the left) column. To set the new F/R RATIO for all
ELEMENT in the second column, WAVE- elements, left click the Set All button. Au-
LENGTH in the third, FORWARD inten- tomatically, the new factors calculated and
sity in the fourth, REVERSE intensity in displayed in the F/R RATIO column will
the fifth, F/R RATIO in the sixth and BKG appear in the background factor column.
FACTOR in the last column. The cursor
will appear in the upper right corner of the 7. Once all of the elements that have a back-
screen under the column BKG FACTOR. ground factor have been updated to the new
The absolute value for this mode is 1.00000 F/R RATIO, a copy of this screen may be
which indicates that the intensity produced made for your records by left clicking the

23 December 2009 / v.3.4.1

Spectroil M/F-W Fuel Analysis Spectrometer (Mod. 6 CCD & 7 CE)   |  37

Print button. Keep this printout for future

reference. Left click the OK button to exit
this dialog.

8. To exit the disc electrode offset procedure,

press function key 10 (F10), left click the
icon, or select Operations/Offsets/Perform
Disc Offsets from the pull down menu op- Figure 5-1, Operations/User Functions Menu
tions. This will place the software back to
the Analysis Program screen which is the Figure 5-2 will open. Proceed with step 4.
normal mode for operation and the mode
the instrument was in before initiating this 4. In the “Set up user functions paths” window
procedure. click on the square button to the right of
Removable drive:.
9. This concludes the disc electrode offset
procedure. Standardize the instrument for 5. The “Removable Drive:” window will open,
normal operation in accordance with Section Figure 5-3. Select the drive that says “Re-
2.5 of this manual. Perform a daily standard- movable Disc (D:)”. With the disc drive
ization check in accordance with Section
2.4 to confirm that all elements at the lower
concentrations meet the accuracy criteria.
If any element fails to meet this criteria,
contact Spectro Incorporated Field Service
for assistance.

5.0 BACKUP OF COMPLETE OilM

SOFTWARE

These steps will take the user through the process

of backing up OilM for Windows on Microsoft® Figure 5-2, Selection of User Function Menu
Windows XP.

1. While running OilMWindows open the File

menu and select Exit. OilmWindows will
shutdown.

2. Reopen OilMWindows by selecting from

the Start menu or the shortcut on the desk-
top. After the communications are up select
Operations/User Functions menu, Figure
5-1.

3. If user functions have been accessed, the

window shown in Figure 5-4 open. Proceed
with step 7. If no user functions have been
previously accessed, the window as shown in
Figure 5-3, Set-up User Functions Paths Screen

23 December 2009 / v.3.4.1

38  |  Operator’s Manual

Figure 5-4, Removable Drive Selection Screen

highlighted click on the OK button.

6. The “Set up user functions paths” window,

Figure 5-2, reopens. Click on the OK but-
ton to continue.

7. The “User Functions” window, Figure 5-4

opens. Select the “Backup to Removable
Media” option. Click the OK button to
continue.

8. OilMWindows will start a transfer of all

OilM Windows and program files to the
removable media.

9. When all the files are copied the “Backup

completed successfully” message box will

open. Click on the OK button

to complete the back up procedure.

23 December 2009 / v.3.4.1