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IS 6135 (1981): Soda Ash, Fused, Technical [CHD 1:Inorganic Chemicals]

IS : 6135 - 1981

Indian Standard SPECIFICATION FOR

SODA ASH, FUSED, TECHNICAL

( First Revision )

First Reprint MARCH 1993

UDC 661.321.1

© Copyright 1982

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

January 1982 Gr 3

AMENDMENT NO. 1 JULY 1988 TO

IS : 6135 - 1981 SPECIFICATION FOR SODA ASH, FUSED, TECHNICAL

( First Revision )

( Page 4, clause 2.2 ) — Substitute the following for the existing clause : '2.2 Volatile Matter Content — The material, when tested according to the method prescribed in Appendix A, shall show volatile matter content not exceeding 2 percent at the time of manufacture and packing.'

( CDC 56 )

Printed at Simco Printing Press , Delhi, India

Acids, Alkalis and Halides Sectional Committee, CDC 56

Chairman P R O F K. S. R A O

Members DR J. R. SANGHAVI ( Alternate

Prof K. S. Rao ) S H R I S. K. BASU

Representing Central Salt & Marine Chemicals Research Institute,

Bhavnagar

to

Directorate General of Supplies and Disposals, New Delhi

S H R I D. S. CHOWDHURY ( Alternate ) S H R I M. L. BHAMBANI S H R I R. C. BHATACHARYA

National Test House, Calcutta Directorate General of Technical Development,

New Delhi S H R I H. KHAPARDE ( Alternate )

S H R I P. S. HARIHARAKRISHNAN S H R I B. N. L A H I R I S H R I A. S. NATARAJAN

The Travancore Rayons Ltd, Rayonpuram Salt Commissioner, Govt of India, Jaipur Standard Alkali, Chemicals Division, Bombay

S H R I T. P. VENAKATRAMAN ( Alternate ) S H R I M. PADMANABAN

S H R I ASHOK P A R E K H

The Mettur Chemical & Industrial Corporation Ltd, Mettur Dam

Gwalior Rayon Silk Mfg ( Wvg ) Co Ltd, Nagda S H R I M. K. MAHESHWARI ( Alternate )

S H R I N. S. PARTHASARTHY E. I. D.-Parry ( India ) Ltd, Madras S H R I A. G. K R I P A L SINGH ( Alternate )

S H R I A. K. R A O D. C. M. Chemical Works, New Delhi S H R I D. V. N. SASTRY ( Alternate )

S H R I V. N. R A O Tata Chemicals Ltd, Bombay S H R I R. K. G A N D H I ( Alternate )

S H R I P . R A O Bengal Chemicals & Pharmaceuticals Ltd, Calcutta S H R I R. K. CHATTERJEE ( Alternate )

S H R I N. K. SACHAR S H R I J . B. SHARMA ( Alternate )

S H R I G. R. SANTHANAKRISHNAN S H R I K. V. M A N I ( Alternate )

Gujarat Alkalies and Chemicals Ltd, Vadodara

Travancore Chemical & Mfg Co Ltd, Mettur Dam

( Continued on page 2 )

© Copyright 1982 BUREAU OF INDIAN STANDARDS

This publication is protected under the Indian Copyright Act ( XIV of 1957 ) and reproduction in whole or in part by any means except with written permission of the publisher thall be deemed to be an infringement of copyright under the said Act.

Indian Standard SPECIFICATION FOR

SODA ASH, FUSED, TECHNICAL

(First Revision)

IS : 6135 - 1981

IS : 6135 - 1981

( Continued from page 1 )

Members SHRI V. S. SAXENA

S H R I R. C. SINHA ( Alternate ) D R N. SEN

SHRI S. K. SUBBAROYAN DR A. N. BHAT ( Alternate )

SHRI J. N. TAWAKLEY

Representing Ballarpur Industries Ltd, New Delhi

Indian Soap and Toiletries Makers' Association, Bombay

Hindustan Lever Ltd, Bombay

Indian Dyestuff Industries Ltd, Bombay SHRI N. R. FADNIS ( Alternate )

SHRI S. S. T H A K U R Indian Paper Mills Association, Calcutta SHRI N. K. GUPTA ( Alternate )

DR M. S. VAIDYA SHRI H. K. VENKATARAMAIAH DR K. M. VERMA

SHRI B. R. WALAVALKAR

Dharamsi Morarji Chemical Co Ltd, Bombay Hindustan Organic Chemicals Ltd, Rasayani Fertilizer ( Planning and Development ) India Ltd,

Sindri Saurashtra Chemicals, Porbandar

S H R I L. K. MALAVIYA ( Alternate ) D R H A R I BHAGWAN,

Director ( Chem ) Director General, ISI ( Ex-officio Member )

Secretary

SHRI S. K. MATHUR Deputy Director ( Chem ), ISI

Alkalis and Allied Products Subcommittee, CDC 56 : 2 Convener

SHRI B. R. WALAVALKAR

Members

Saurashtra Chemicals, Porbandar

SHRI L. K. MALAVIYA ( Alternate to Shri B. R. Walavalkar )

SHRI M. L. BHAMBANI SHRI M. V. DESAI

DR J. M. T U R E L ( Alternate ) SHRI P. S. HARIHARAKRISHNAN SHRI J A I . GOPAL JAIN SHRI R. N. MODY

National Test House, Calcutta The Atul Products Ltd, Atul

Travancorc Rayons Ltd, Rayonpuram Dhrangadhra Chemical Works Ltd, Dhrangadhra Indian Soap & Toiletries Makers' Association,

Bombay SHRI R. S. VAIDYANATHAN ( Alternate )

SHRI A. S. NATARAJAN Standard Alkali, Bombay SHRI T. P. VENKATARAMAN ( Alternate )

SHRI M. R. RAMACHANDRAN Tata Chemicals Ltd, Mithapur SHRI S. GANAPATHY ( Alternate )

SHRI RAMESH CHAND All India Glass Mfrs' Association, New Delhi SHRI C. K. L. SOMANY ( Alternate )

SHRI D. SESHASAYEE Mettur Chemical & Industrial Corporation Ltd, Mettur Dam

SHRI R. V. RAMANI ( Alternate ) S H R I M. P. SHENOY SHRI R. C. SINHA

SHRI T. L. BOLIA ( Alternate ) SHRI J . N. TAWAKLEY

S H R I N. R. FADNIS ( Al ternate ) SHRI S. S. THAKUR

Tata Oil Mills Co Ltd, Bombay Ballarpur Industries Ltd, Yamunanagar

Indian Dyestuff Industries Ltd, Bombay

Indian Paper Mills Association, Calcutta SHRI P. L. BURMAN ( Alternate )

2

IS : 6135 - 1981

Indian Standard SPECIFICATION FOR

SODA ASH, FUSED, TECHNICAL

(First Revision)

0 . F O R E W O R D 0.1 This Indian Standard ( First Revision ) was adopted by the Indian Standards Institution on 1 October 1981, after the draft finalized by the Acids, Alkalis and Halides Sectional Committee had been approved by the Chemical Division Council.

0.2 This Indian Standard was originally issued in 1971. The Sectional Committee responsible for its preparation decided to revise it in the light of the progress made by the industry. In the revised standard, the minimum limit for alkalinity has been raised from 96 to 97 percent and the maximum limit for sulphate has been lowered to 1.5 percent. The material is hygroscopic and it absorbs moisture and carbon dioxide from the atmosphere. An adjustment in the mass of the material has, therefore, been permitted in the present revision if the volatile matter exceeds 2 percent.

0.3 Soda ash, fused, is mainly used in foundries for ferious castings for the removal of sulphur from pig iron. It melts high up in the cupola stack where it fluxes with limestone and helps to speed up the combustion reactions and restricts the oxidising melting zone at the tuyeres. It thereby gives sound castings with superior grain structure and, being a good degasifier, minimizes the blow hole defects. It also imparts fluidity to the slag, thus ensuring smoother and continuous cupola operation.

0.4 Soda ash, fused, is sold under various trade names. It is the fused and densified form of soda ash, technical, and comes in the form of pigs weighing 1.0 ± 0.2 kg each. In this form, it is less liable to weathering and deterioration. It is mainly soda ash and does not crumble and dust. It has a fusion point of about 850°C. It does not require any special storage facilities.

0.5 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in

3

IS : 6135 - 1981

accordance with IS : 2-1960*. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

1. SCOPE 1.1 This standard prescribes the requirements and the methods of sampling and test for soda ash, fused, technical.

2. REQUIREMENTS 2.1 Description — The material shall be in the form of light grey pigs weighing about 1.0 ± 0.2 kg.

2.2 Volatile Matter Content — The material, when tested according to the method prescribed in Appendix A, shall show volatile matter content not exceeding 2 percent.

2.2.1 If the material shows a volatile matter exceeding 2 percent, the delivery mass shall be adjusted as prescribed below:

Mass of material to be credited =

where M = mass in g of the material actually delivered, and

A = percentage of volatile matter in the material as delivered.

2.3 The material, when tested according to the methods prescribed in Appendix B, shall comply with the requirements given in Table 1. Reference to the relevant clauses of Appendix B is given in col 4 of the table.

3. PACKING AND MARKING 3.1 Packing — Fifty to fifty five pigs shall be packed in double gunny bags with grass packing weighing approximately 50 kg net or as agreed to between the purchaser and the supplier. 3.2 Marking — Each package shall be marked with the manufacturer's name or trade-mark, if any, mass of the material in the container and batch number.

*Rules for rounding off numerical values ( revised ).

4

IS : 6135 - 1981

S L No.

(1) i)

ii)

iii)

iv)

v)

TABLE 1 REQUIREMENTS FOR SODA ASH, FUSED, TECHNICAL

( Clause 2.3 )

CHARACTERISTIC

(2) Total alkalinity ( as Na2CO2 ), percent

by mass, Min Matter insoluble in water, percent by

mass, Max Sulphate ( as Na2SO4 ), percent by

mass, Max Chlorides ( as NaCl ), percent by mass,

Max Iron ( as Fe 2 O 3 ), percent by mass, Max

REQUIREMENT ( ON D R Y BASIS )

(3) 97.0

0.3

1.5

1.0

0.10

M E T H O D OF T E S T ( R E F

TO C L N O . IN APPENDIX B )

(4) B-3

B-4

B-5

B-6

B-7

3.2.1 The bags may also be marked with the ISI Certification Mark. NOTE — The use of the ISI Certification Mark is governed by the provisions of the

Indian Standards Institution (Certification Marks) Act and the Rules and Regu­lations made thereunder. The ISI Mark on products covered by an Indian Standard conveys the assurance that they have been produced to comply with the require­ments of that standard under a well-defined system of inspection, testing and quality control which is devised and supervised by ISI and operated by the producer. ISI marked products are also continuously checked by ISI for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the ISI Certification Mark may be granted to manufacturers or processors may be obtained from the Indian Standards Institution.

4. SAMPLING 4.1 Representative samples of the material shall be drawn and adjudged at prescribed in Appendix C.

A P P E N D I X A ( Clause 2.2 )

DETERMINATION OF VOLATILE MATTER CONTENT A-1. PROCEDURE A-1.1 Place about 2 g of the material ( see B-2.1 ) in a weighing bottle provided with a stopper and weigh accurately. Remove the stopper and heat for 1 h at a temperature of 250 to 300 C. Cool in a desiccator. Place the stopper and weigh. Repeat until the mass remains constant.

5

IS : 6135 - 1981

A-2. CALCULATION Volatile matter content,

percent by mass =

where

M1 = mass in g of the material before heating, and M2 = mass in g of the material after heating.

A P P E N D I X B ( Clause 2.3 and Table 1 )

METHOD OF TEST FOR SODA ASH, FUSED, TECHNICAL

B-1. QUALITY OF REAGENTS

B-1.1 Unless specified otherwise, pure chemicals and distilled water ( see IS : 1070-1977* ) shall be used in tests.

NOTE — 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the results of analysis.

B-2. PREPARATION OF THE SAMPLE

B-2.1 Powder about 20 g of the material and pass it through 250-micron IS sieve and use this material for the determination of voltatile matter content. Use this prepared sample for further analysis.

B-3. DETERMINATION OF TOTAL ALKALINITY

B-3.1 Reagents B-3.1.1 Standard Hydrochloric Acid — 1 N. B-3.1.2 Methyl Orange Indicator Solution — Dissolve 0.01 g of methyl

orange in 100 ml of water. B-3.2 Procedure — Weigh accurately about 1 g of the prepared sample. Transfer it completely to a 500-ml conical flask and dissolve it in 100 ml of water. Add 4 drops of methyl orange indicator solution and titrate with standard hydrochloric acid.

*Specification for water for general laboratory use ( second revision ).

6

IS : 6135 - 1981

B-3.3 Calculation Total alkalinity ( as Na2 CO 3 ),

percent by mass =

where A = volume in ml of standard hydrochloric acid used in

titration, N = normality of standard hydrochloric acid, and M = mass in g of the material taken for the test.

B-4. DETERMINATION OF MATTER INSOLUBLE IN WATER B-4.1 Procedure — Weigh accurately about 10 g of the prepared sample ( see B-2 ). Transfer it to a 400-ml beaker, add about 100 ml of freshly boiled distilled water and boil the soultion for about 10 minutes. Filter through a weighed sintered glass crucible ( G No. 4 ) or Gooch crucible. Wash thoroughly with hot water and dry to constant mass at 110 ± 5°C. B-4.2 Calculation

Matter insoluble water, percent by mass =

where M1 = mass in g of the residue, and M2 = mass in g of the material taken for the test.

B-5. DETERMINATION OF SULPHATES B-5.1 Reagents

B-5.1.1 Concentrated Hydrochloric Acid — See IS : 265-1976*. B-5.1.2 Barium Chloride Solution — 10 percent ( m/v ).

B-5.2 Procedure — Dissolve about 5 g of the prepared sample ( see B-2 ), accurately weighed, in 100 ml of water and add concentrated hydrochloric acid to make the solution slightly acidic. Boil well to decompose the carbonates. Cool, filter through a folded filter paper and wash the filter paper thoroughly, collecting the filtrate and washing in a 500-ml beaker. Dilute combined filtrate and washings to about 250 ml, boil and add 10 ml of hot barium chloride solution to the boiling solution.

*Specification for hydrochloric acid ( second revision ).

7

IS : 6135 - 1981

Boil again for 2 min, let it stand for 4 h and filter through a tared Gooch crucible or sintered glass crucible G 4. Wash the precipitate free from chlorides and dry to constant mass at 110 ± 5°C B-5.3 Calculation

Sulphates ( as Na 2 SO4 ), percent by mass =

where

C = mass in g of the precipitate, and M = mass in g of material taken for the test.

B-6. DETERMINATION OF CHLORIDES B-6.1 Reagents

B-6.1.1 Concentrated Nitric Acid — see IS : 264-1976*.

B-6.1.2 Standard Silver Nitrate Solution — 0.1 N.

B-6.1.3 Nitrobenzene

B-6.1.4 Standard Ammonium Thiocyanate Solution — 0.1 N.

B-6.1.5 Ferric Ammonium Sulphate Indicator Solution — Saturated.

B-6.2 Transfer about 2 g of the prepared sample, ( see B-2 ), accurately weighed, to a conical flask, neutralise with concentrated nitric acid and then add 5 ml of the acid in excess. Add 20 ml of standard silver nitrate solution. Add 3 ml of nitrobenzene and shake vigorously. Titrate with standard ammonium thiocyanate solution using ferric ammonium sulphate indicator. Carry out a blank using 20 ml of standard silver nitrate solution.

B-6.3 Calculation

Chlorides ( as NaCl ), percent by mass =

where V1 = volume in ml of standard ammonium thiocyanate

solution required for 20 ml standard silver nitrate solution,

V2 = volume of standard ammonium thiocyanate solution used in B-6.2,

*Specification for nitric acid ( second revision ).

8

IS : 6135 - 1981

N = normality of standard ammonium thiocyanate, and M = mass in g of the material taken for the test.

B-7. TEST FOR IRON B-7.1 Apparatus

B-7.1.1 Messier Cylinders — 100-ml capacity. B-7.2 Reagents

B-7.2.1 Dilute Hydrochloric Acid — approximately 15 percent ( v/v ).' B-7.2.2 Ammonium Persulphate B-7.2.3 Potassium Thiocyanate Solution — 5 percent. B-7.2.4 Dilute Sulphuric Acid — 10 percent ( v/v ). B-7.2.5 Standard Iron Solution — Dissolve 0.490 g of ferrous ammonium

sulphate [ FeSO4 ( NH4 )2SO4.6H2O )] in 10 ml of dilute sulphuric acid and dilute with water to 1 000 ml. One millilitre of the diluted solution is equivalent to 0.1 mg of iron ( as Fe2CO3 ).

B-7.3 Procedure — Weigh accurately 1.00 g of the prepared sample ( see B-2 ) and dissolve it in 20 ml of water. Add about 5 ml of hydro­chloric acid to make it acidic and 30 mg of ammonium persulphate and boil to oxidize the iron. Cool and make up the volume to 100 ml with water in a volumetric flask. Take 10 ml aliquot of the solution in the Nessler cylinder. Add 5 ml of potassium thiocyanate solution, dilute to make with water, and stir well. Into a second Nessler cylinder, add 5 ml of dilute hydrochloric acid and about 30 mg of ammonium per­sulphate, 5 ml of potassium thiocyanate solution and 1 ml of standard, iron solution. Dilute to the mark with water. Compare the colour of the solution in the two cylinders.

B-7.3.1 The limit prescribed in Table 1 shall be taken as not having been exceeded if the intensity of the colour produced with the material is not higher than that produced by the standard solution.

A P P E N D I X C ( Clause 4.1 )

SAMPLING OF SODA ASH, FUSED, TECHNICAL

C-1. GENERAL REQUIREMENTS OF SAMPLING C-1.0 In drawing samples, the following precautions and directions shall be observed.

9

IS : 6135 - 1981

C-1.1 Samples shall not be taken in an exposed place. C-1.2 The sampling instrument and sample containers shall be clean and dry.

C-1.3 After filling, sample containers shall be sealed air-tight and marked with full details of sampling.

C-2. SCALE OF SAMPLING C-2.1 Lot — In any consignment, material of the same grade and belonging to one batch of manufacture shall constitute a lot. C-2.2 For ascertaining the conformity of the lot to the requirements of the specification, tests shall be carried out for each lot separately. The number of pigs ( n ) to be selected for the purpose depends on the size of the lot ( N ) and shall be in accordance with Table 2.

TABLE 2 SCALE OF SAMPLING

LOT SIZE

(N)

(1) Up to 50 51 to 100

101 to 300 301 to 500 501 and above

SAMPLE SIZE

(n) (2)

3 4 5 7

10

C-2.3 The pigs of soda ash shall be selected equally from the gunny bags. If there are more than 10 gunny bags in the lot, selection of 10 bags shall be made at random. For random selection procedures IS : 4905-1968* may be referred to.

C-3. PREPARATION OF TEST SAMPLES C-3.1 From each of the pigs selected under C-2, 50 g of soda ash shall be collected. These portions, termed as individual samples, shall be used for making prepared samples as prescribed under B-2.1. There shall be as many prepared samples as the number of pigs selected in the sample. The remaining portions of individual samples shall be mixed together to give a composite sample of mass 100 g. Composite sample also shall be treated as prescribed in B-2.1 for further analysis.

*Methods for random sampling.

10

IS : 6135 - 1981

C-4. NUMBER OF TESTS AND CRITERIA FOR CONFORMITY C-4.1 Test for total alkalinity shall be performed on individual samples. Tests for all the other characteristics shall be conducted on the composite sample. C-4.2 If a test result on total alkalinity is denoted by then the criteria for accepting the lot in respect of this characteristic ( — 0.4 R ) shall be greater than or equal to 96.0, where and R stand for the mean and range of test results. C-4.3 For all other characteristics mentioned in Table 1, the composite sample shall satisfy the corresponding requirements if the lot is to be accepted under this clause.

11

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