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Tar and Bituminous Materials - Methods For Test - Determination of Solubility in Trichloroethylene

This document is an Indian Standard (IS 1216:2023) that prescribes the method for determining the solubility of tar, bituminous materials, and asphalts in trichloroethylene. It outlines the process which involves weighing a sample, adding trichloroethylene solvent, allowing it to stand for an hour, then filtering through a pre-weighed Gooch crucible to separate insoluble material. The insoluble material and crucible are then weighed to determine the solubility percentage. The standard provides apparatus requirements and procedures for preparing the crucible and performing the test.
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0% found this document useful (0 votes)
424 views10 pages

Tar and Bituminous Materials - Methods For Test - Determination of Solubility in Trichloroethylene

This document is an Indian Standard (IS 1216:2023) that prescribes the method for determining the solubility of tar, bituminous materials, and asphalts in trichloroethylene. It outlines the process which involves weighing a sample, adding trichloroethylene solvent, allowing it to stand for an hour, then filtering through a pre-weighed Gooch crucible to separate insoluble material. The insoluble material and crucible are then weighed to determine the solubility percentage. The standard provides apparatus requirements and procedures for preparing the crucible and performing the test.
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भारतीय मानक IS 1216 : 2023

Indian Standard

टार और िबटुिमनस सामग्री — परी�ण


पद्धितयाँ — ट्राइक्लोरोइिथलीन में
घुलनशीलता का िनधार्रण
( दसू रा पनु री�ण )

Tar and Bituminous Materials —


Methods for Test — Determination of
Solubility in Trichloroethylene
( Second Revision )

ICS 75.140

 BIS 2023

भारतीय मानक ब्यरू ो


BUREAU OF INDIAN STANDARDS
मानक भवन, 9 बहादरु शाह ज़फर मागर्, नई िदल्ली - 110002
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI - 110002
www.bis.gov.in www.standardsbis.in

August 2023 Price Group 5


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Bitumen, Tar and Related Products Sectional Committee, PCD 06

FOREWORD

This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Bitumen, Tar and Related Products Sectional Committee had been approved by the Petroleum, Coal and
Related Products Division Council.

This standard was first published in 1958 as ‘Methods for testing tar and bituminous materials — Determination
of solubility in carbon disulphide or trichloroethylene’ and subsequently revised in 1978. A series of published
Indian Standards cover tar, bitumen and bituminous materials and a booklet was published containing a series of
22 standards as listed below:

IS No. Title
IS 1201 : 1978 Sampling
IS 1202 : 1978 Determination of specific gravity
IS 1203 : 1978 Determination of penetration
IS 1204 : 1978 Determination of residue of specified penetration
IS 1205 : 1978 Determination of softening point
IS 1206 : 1978 Determination of viscosity:
(Part 1) Industrial viscosity
(Part 2) Absolute viscosity
(Part 3) Part 3 Kinematic viscosity
IS 1207 : 1978 Determination of equiviscous temperature (EVT)
IS 1208 : 1978 Determination of ductility
IS 1209 : 1978 Determination of flash point and fire point
IS 1210 : 1978 Float test
IS 1211 : 1978 Determination of water content (dean and stark method)
IS 1212 : 1978 Determination of loss on heating
IS 1213 : 1978 Distillation test
IS 1214 : 1978 Determination of matter insoluble in benzene (WITHDRAWN due to toxic nature of
benzene)
IS 1215 : 1978 Determination of matter insoluble in toluene
IS 1216 : 1978 Determination of solubility in carbon disulphide or trichloroethylene
IS 1217 : 1978 Determination of mineral matter (ash)
IS 1218 : 1978 Determination of phenols
IS 1219 : 1978 Determination of naphthalene
IS 1220 : 1978 Determination of volatile matter content

However, the Committee responsible for the formulation of standards in the field of bitumen, tar and related
products decided to publish these Indian Standards separately for each test so as to make it user friendly.

(Continued on third cover)


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IS 1216 : 2023

Indian Standard
TAR AND BITUMINOUS MATERIALS — METHODS FOR
TEST — DETERMINATION OF SOLUBILITY IN
TRICHLOROETHYLENE
( Second Revision )

1 SCOPE 4.2 Solvent

This standard prescribes the method of test for 4.2.1 Trichloroethylene — (see IS 245)
determination of solubility in trichloroethylene for 4.3 Preparation of Material
asphaltic bitumen and native asphalts.
If the sample contains water, heat it to a temperature
2 REFERENCES not exceeding 130 °C until the water has been
removed, stirring constantly, when possible, during
The standards given below contain provisions which, heating. Perform this operation as expeditiously as
through reference in this text, constitute provisions of possible.
this standard. At the time of publication, the editions
indicated were valid. All the standards are subject to 4.4 Preparation of Gooch Crucible
revision, and parties to agreements based on this
4.4.1 Insert the filter tube in the stopper of the
standard are encouraged to investigate the possibility
filtering flask, set the Gooch crucible in the filter
of applying the most recent edition of these tube, and connect the flask to the suction pump. Fill
standards: the crucible with some of the suspension of asbestos
or glass microfiber in the water, allow it to settle
IS No. Title partly in the crucible and apply a light suction to draw
IS 245 : 2020 Specification for trichloroethylene, off the water, leaving a firm mat of asbestos or glass
technical (fourth revision) microfiber in the crucible. Add more suspended
asbestos or glass microfiber and repeat the process
IS 334 : 2023 Glossary of terms relating to until a mat weighing (0.5 ± 0.1) g is built up after
bitumen and tar (fourth revision) drying. Wash the asbestos or glass microfiber mat
IS 1211 : 2022 Methods for testing tar and thoroughly with water and dry in the oven at a
bituminous materials — temperature of 150 ºC. Cool the crucible in the
desiccator, weigh and replace it in the dry filter tube
Determination of water content —
supported in the clean and dry filtering flask.
Dean and stark method (second
revision)
4.4.2 In the determination, the asbestos or glass
microfiber apparently absorbs irreversibly an amount
3 TERMINOLOGY
of soluble bitumen (usually 1 mg/g to 5 mg/g of
asbestos or glass microfiber) which is not removed
For the purpose of this standard, definitions given in
by a subsequent washing with solvent. The weight of
IS 334 shall apply.
asbestos used, therefore, shall be kept within the
specified limits to ensure reproducible results.
4 METHOD A (FOR ASPHALTIC BITUMEN)
4.5 Procedure
4.1 Apparatus
Weigh about 2 g of the dry sample correct to the
4.1.1 Balance — capable to weigh with the least nearest 0.001 g into a 200 ml conical flask and add
count of 0.001 g. 100 ml of trichloroethylene. Stir the contents of the
flask, and then allow it to stand, loosely corked, for a
4.1.2 Oven period of one hour. Filter the contents of the flask
through the Gooch crucible prepared as described
4.1.3 Gooch Crucible under 4.4 which has been weighed to the nearest
0.001 g. Moisten the filter pad with trichloroethylene
4.1.4 Conical Glass Flask — 200 ml capacity before commencing filtration and filter at a rate of not

1
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IS 1216 : 2023

more than two drops per second at first. The filtrate than the following:
shall be quite clear. Transfer the insoluble matter
remaining in the flask to the crucible by washing out Sl Matter Repeatability Reproducibility
the flask with a stream of trichloroethylene from a No. Soluble in
wash bottle. Wash the sample retained in the crucible Trichloroethylene
with successive small amounts of trichloroethylene (1) (2) (3) (4)
until a filtrate is obtained which is not discoloured.
Allow the crucible to dry in air for 30 min, after i) Below 98 percent 0.5 1.0
which place it in an oven at 100 ºC to 110 ºC for one ii) 98 to 100 percent 0.1 0.2
hour. Allow the crucible to cool in a desiccator and
then weigh.

4.6 Calculation 5 METHOD B (FOR NATIVE ASPHALTS)

Calculate the matter soluble in trichloroethylene as 5.1 Apparatus


follows:
5.1.1 Glass Tap Funnel — approximately 100 mm
Matter soluble in trichloroethylene, percent diameter, the stem fitted with a tap and the top ground
flat.
𝑊𝑊1 − 𝑊𝑊2
= × 100
𝑊𝑊1 5.1.2 Glass Plate — to cover the funnel, about
where 120 mm in diameter, with a hole of about 16 mm
W1 = mass, in g, of dry sample taken for the test; diameter in the centre.
and
5.1.3 Glass Funnel — smaller than that described
W2 = mass, in g, of insoluble material retained under 5.1.1 with its stem passing through a cork
in the Gooch crucible. placed in the hole in the glass plate, the lower end of
the stem reaching approximately half-way down the
4.7 Report tap funnel.
Report the result obtained in 4.6 to nearest
5.1.4 Filter Papers — two, Whatman filter paper No.
0.05 percent as the matter soluble in trichloroethylene
5 or equivalent filter papers, 185 mm in diameter,
of the dry material.
dried in a suitable oven, cooled in a desiccator,
counterpoised and folded together as shown in Fig. 1.
4.8 Precision

Test results shall not differ from the mean by more

FIG. FOLDED FILTER PAPER

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IS 1216 : 2023

5.2 Solvent and Sample where

5.2.1 Trichloroethylene (see IS 245) W1 = mass, in g, of the dry sample taken for the
test;
5.2.2 Cement W2 = mass, in g, of recovered insoluble matter;
and
Suitable for sealing the glass plate to the funnel. It W3 = water content of sample, in g, if determined.
may be prepared with 10 g of gelatin, 80 ml of water
and 20 g of glycerine. 5.6 Report
5.3 Preparation of Sample
Report the result obtained in 5.5 to the nearest
0.05 percent as the matter soluble in
5.3.1 If the sample contains water, heat a 100 g
trichloroethylene.
portion at a temperature not exceeding 130 ºC, the
material being constantly stirred when possible, 5.7 Precision
until the rate of loss in weight of the sample does not
exceed 0.1 g during a 15 min period of heating. Test results shall not differ from the mean by more
than the following:
5.3.2 If the loss in weight on drying exceeds
0.1 percent, determine the water content of another Repeatability 0.5
sample of the material in accordance with IS 1211. Reproducibility 0.5

5.4 Procedure These precision figures do not include any


allowance for differences due to variations in
Dry the two filter papers (see 5.1.4) in an oven at samples.
100 °C to 110 °C, cool in a desiccator, counterpoise,
fold together as illustrated in Fig. 1 and place in the 6 PRECAUTIONS
tap funnel. Weigh about 2 g of the dry sample, as
prepared in 5.3, correct to the nearest 0.001 g in the 6.1 Barriers
filter papers and secure the cover to the funnel by
means of the cement. Now add trichloroethylene Handling of trichloroethylene shall be done in fume
through the small funnel until the filter paper is cupboard with ventilation.
about half filled and then allow it to stand for 30 min.
Draw the solution off through the tap. Place a watch 6.2 Personal Protective Equipment (PPE)
glass on the small funnel to minimize evaporation.
Close the tap and introduce a further quantity of Chemical gloves, eye goggles, face shield, spill
trichloroethylene through the small funnel and again proof clothing, chemically resistant safety shoes
draw the solution off after 30 min. Repeat this shall be provided.
procedure until the solvent drawn off is no longer
discoloured. When the filtration is completed, 6.3 Safety shower nearby and eye wash in
remove the cover and allow the filter papers to dry immediate vicinity shall be provided.
in air for 30 min before placing them in a ventilated
air oven at 100 ºC to 110 ºC for 1 h. Next place the NOTE — It is strongly recommended that the safety in-
filter papers in a desiccator and when cool, weigh charge reviews the safety data sheet (SDS) of these
the inner filter paper and contents, using the outer materials and setup the operating procedure, PPE and
barriers accordingly.
filter paper as a counterpoise.

5.5 Calculation
Calculate the solubility of the dry sample as follows:
Matter soluble in trichloroethylene =
𝑊𝑊1 − 𝑊𝑊2 100
( × 100) ×
𝑊𝑊1 100 + 𝑊𝑊3

percent by weight

3
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IS 1216 : 2023

ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Bitumen, Tar and Related Products Sectional Committee, PCD 06

Organization Representative(s)
CSIR - Central Road Research Institute, New Delhi PROF MANORANJAN PARIDA (Chairperson)

Airports Authority of India, New Delhi SHRI VINOD KUMAR SHARMA


SHRI SUPRIO GOSH (Alternate)

Bharat Oman Refineries Limited, Bina SHRI AJAY PRAKASH SHARMA


SHRI BALA KRISHAN SRIDHAR (Alternate)

Bharat Petroleum Corporation Limited, Mumbai SHRI MAHESH SHEVADE


DR TUSHAR S. THORAT (Alternate I )
MS SONAL MAHESHWARI (Alternate II)
SHRI VINAY V. SUVE (Alternate III)
MS JAYA RAWAT (Alternate IV)

Birla Institute of Technology and Science, Pilani PROF SRIDHAR RAJU


PROF V. VINAYAKA RAM (Alternate)

Central Public Works Department, New Delhi SHRI DINESH K. UJJAINIA

Chennai Petroleum Corporation Limited, Chennai DR V. SELVAVATHI


SHRI H. RAMAKRISHNAN (Alternate)

CSIR - Central Building Research Institute, MS RAJANI LAKHANI


Roorkee

CSIR - Central Road Research Institute, New Delhi DR AMBIKA BEHL


DR SIKSHA SWAROOP KAR (Alternate)

CSIR - Indian Institute of Petroleum, Dehradun SHRI MANOJ SRIVASTAVA


DR KAMAL KUMAR (Alternate)

CSIR - North East Institute of Science and DR SHASHI D. BARUAH


Technology, Jorhat DR B. P. BARUAH (Alternate)

Dilip Buildcon Limited, Bhopal SHRI B. B. KAMESWARA RAO


SHRI ANUSH K. C. (Alternate)

Directorate General Border Roads, New Delhi LT COL NITIN CHANDRA JOSHI

Directorate General of Quality Assurance, DR OM PRAKASH SINGH


Ministry of Defence, Kanpur

Directorate General of Quality Assurance, SHRI A. K. KANAUJIA


Ministry of Defence, New Delhi SHRI SACHIN VINAYAK ZOPE (Alternate)

Engineer in Chief Branch, New Delhi SHRI R. JAYAPRASAD


SHRI O. P. SRIVATAVA (Alternate)

GP Global Asphalt Private Limited, New Delhi SHRI RAJESH KUMAR JAIN

G R Infra-Projects Limited, Gurugram SHRI U. C. GUPTA

4
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IS 1216 : 2023

Organization Representative(s)
Highways Research Station, Chennai ER S. USHA DEVI
SHRI C. S. SHENBAGAVALLI B. E. (Alternate)
Hindalco Industries Limited, Mumbai SHRI HARSHAD KUMAR PANDIT

Hindustan Colas Private Limited, Mumbai SHRI T. K. SUBHAASH


SHRI K. G. RANGANATHA (Alternate)
Hindustan Petroleum Corporation Limited (HP SHRI B. RAVI
Green R & D Center), Bengaluru SHRI K. RAGHAVA KRISHNA (Alternate)

Hindustan Petroleum Corporation Limited, SHRI SANTOSH DHAKU BHOGALE


Mumbai

Indian Institute of Technology Bombay, Mumbai DR DHARAMVEER SINGH

Indian Institute of Technology Delhi, New Delhi SHRI ARAVIND SWAMY


PROF RAJIB B. MALIICK (Alternate)

Indian Institute of Technology Madras, Chennai DR ATUL NARAYANAN

Indian Institute of Technology Roorkee, Roorkee SHRI SHAM SUNDAR RAVINDRANATH

Indian Oil Corporation Limited, New Delhi DR N. S. RAMAN

Indian Oil Corporation Limited - Refineries and SHRI ANINDITA MOITRA


Pipelines Division, New Delhi SHRI SOUMEN MONDAL (Alternate I)
SHRI P. MADHUSUDHANA REDDY (Alternate II)

Indian Oil Corporation (R and D Centre), SHRI DHANESH KUMAR (Alternate)


Faridabad DR I. DEVOTTA (Alternate)

Indian Oil Total Private Limited, Mumbai DR. PANKAJ KUMAR JAIN
SHRI GAURAV GOGNE (Alternate)

Indian Road Congress, New Delhi SHRI S. K. NIRMAL


SHRI R. V. PATIL (Alternate)

IRB Infrastructure Developers Limited, Mumbai SHRI SUDHIR HOSHING


SHRI JITENDER CHAUHAN (Alternate)

Larsen and Toubro Infotech Limited, Mumbai SHRI S. NAGA SRINIVASA SARMA
SHRI DEEPAK GAIKWAD (Alternate)

Mangalore Refinery and Petro Chemical Limited, MS ANITHA SHETTY


Mangaluru SHRIMATI YOGEESHA (Alternate)

Ministry of Road Transport and Highways, SHRI SANJEEV KUMAR


New Delhi SHRI VARUN AGGARWAL (Alternate)

National Highways Authority of India, New Delhi SHRI S. K. MISHRA


SHRI A. K. SABHARWALL (Alternate)

National Institute of Technology, Warangal SHRI VENKAIAH CHOWDARY


DR S. SHANKAR (Alternate)

National Rural Roads Development Agency, SHRI B. C. PRADHAN


New Delhi

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IS 1216 : 2023

Organization Representative(s)
National Test House, Kolkata SHRI VINAY KUMAR
SHRIMATI ANSHUMALA SHUKLA (Alternate)

Nayara Energy Limited, Mumbai SHRI MRIGANKA TARAFDAR


SHRI DHIRAJ GONDALIA (Alternate)

Om Infracon Private Limited, Guwahati SHRI A. N. DAS


SHRI MANISH BAJAJ (Alternate I)
SHRI DIGAMBAR DEKA (Alternate II)

Ooms Polymer Modified Bitumen Private Limited, SHRI B. R. TYAGI


Gurugram SHRI PALASH KATHAL (Alternate)

Shell Bitumen India Private Limited, Gurugram SHRI NILANJAN SARKER

Zydex Industries Limited, Vadodara SHRI AJAY RANKA


SHRI HIMANSHU AGARWAL (Alternate I)
SHRI VISHAL SALUJA (Alternate II)

In Personal Capacity (Karanpura House, 50 Raj SHRI P. S. KANDHAL


Bhawan Road, Civil Lines, Jaipur - 302006)

BIS Directorate General SHRIMATI MEENAL PASSI, SCIENTIST ‘F’/


SENIOR DIRECTOR AND HEAD (PETROLEUM,
COAL, AND RELATED PRODUCTS)[REPRESENTING
DIRECTOR GENERAL (Ex-officio)]

Member Secretary
SHRI HARI MOHAN MEENA
SCIENTIST C/DEPUTY DIRECTOR
(PETROLEUM , COAL, AND RELATED PRODUCTS), BIS

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(Continued from second cover)

This second revision has been brought to formulate individual standard on determination of solubility in
trichloroethylene. In this revision following major changes have been made:
a) Use of carbon disulphide has been removed from the test method due to its carcinogenicity; and
b) Precautions for use of trichloroethylene have been incorporated.

The composition of the Committee responsible for formulation of this standard is given in Annex A.

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2 : 2022 ‘Rules for rounding off
numerical values (second revision)’.

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development of the activities of standardization, marking and quality certification of goods and attending to
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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the website-
www.bis.gov.in or www.standardsbis.in.
This Indian Standard has been developed from Doc No.:PCD 06 (19995).

Amendments Issued Since Publication


Amend No. Date of Issue Text Affected

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