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IS 10468 (1983): 1, 3-phenylenediamine-4-sulphonic Acid

[PCD 9: Organic Chemicals Alcohols and Allied Products and
Dye Intermediates]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
( Reaffirmed 2002 )
 IS : 1046&C1943

Indian Standard
SPECIFICATION FOR
1, 3-PHENYLENEDIAMINE-4-SULPHONIC ACID

Dye Intermediates Sectional Committee, PCDC 11

Chairman Representing
DRP.V.SUBRAMANIAM Colour-Chem Ltd, Bombay

Members
DR K. S. VAJANDAR ( Alternate to
Dr P. V. Subramaniam )
DR S. C. AXIN UniversalDyestuff Industries Ltd, Vadodara
DR Y. B. DESAI ( Alternate )
SHRI S. D. BHARDWAJ Ajanta Chemical Industries, New Delhi
SHRI KAPIL DEV ( Alternate )
SHRII~.M. BRAHME Atic Industries Ltd, Bulsar
CHAIRMA& DYESTUFFS AND DYE Indian Chemical Manufacturers Association, Calcutta
INTERMEDIATESUBCOMMITTEE
PRESIDENT, ICMA ( Alternate )
SHRI M. V. DESAI Atul Products Ltd, Bulsar
DR J. M. TUREL ( Alternate )
SHRI S. N. DESAI Hickson & Dadajee Ltd, Bombay
SHRI N. S. MURTHY ( Alternate )
DR S. KALYANARAMAN SG Chemicals & Dyes Ltd, Vadodara
DR S. SID~HAN ( Alternate )
SHRI A. K. MANUAL Directorate General of Technical Development, New
Delhi
SHRI JASBIR SINGH ( Alternate )
SHRI V. K. MENON Amar Dye-Chem Ltd, Bombay
DR T. H. MAWAXK ( Alternate )
SHRI P. A. PATEL Indian Dyestuff Industries Ltd, Bombay
SEXRIB. M. NAIK ( Alternate )
SRRI K. L. RATHI Sudarshan Chemical Industries Ltd, Pune
DR A. S. GULATI ( Alternate )
SARI K. S. RINDANI Sandoz ( India ) Ltd, Bombay
SHRI M. M. GANDHI ( Alternate )
SHRI T. SADASIVAN Ciba-Geigy of India Ltd, Bombay
SHRI M. N. KHOPKAR ( Alternate )
SHRI G. G. SUTAONE Development~Commissioner, Small Scale Industries,
New Delhi
SHRI N. K. GUIIA ( Alternate )

( CWZtiaU6ci
Oa/kZg62 )

@ Copyright 1983
INDIAN STANDARDS lNSTITUTION
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 sbzll be deemed to be an infringement Df coovrieht under the said Act.
IS:10468 - 1983

( Continuedfrom page 1)
Members Rspresenting
SHRI V. G. UPADHYE Synthofine Chemicals of India Pvt Ltd, Bombay
SHKI H. K. VENKATARAMA~AXX Hindustan Organic Chemicals Ltd, Rasayani
( Maharashtra )
SHRI M. S. SAXENA, Director General, IS1 ( Ex-ojicio Member )
Director ( P & C )
Secretary
SHRI A. KAR
Deputy Director ( P & C ), ISI

Panel for Sulphonic Acid Dye Intermediates, PCDC 11 : P2

Conoener
DR P. V. SUBRAMANIAIV~ Colour-Chem Ltd, Bombay

Members
SERI M. V. DE~AT The Atul Products Ltd, Bulsar
DR S. R. G. SARMA (Alternate )
DR M. M. DESHPANDE SG Chemicals and Dyes Ltd, Vadodara
&RI B. M. NAIK Indian Dyestuff Industries Ltd, Bombay
SHRI J. K. DOSHI ( Alternate )
SRRISAN~OKH SINGH National Chemical Industries Pvt Ltd, New Delhi
SERI BRIJINDER PAL SINGES( Alternate I )
SRRI KULBIR SIN~H ( Alternate II )
SRRI R. K. TALPADE Hickson & Dadajee Ltd, Bombay
SHRI H. K. VEPTKATARAMAIAH Hindustan Organic Chemicals Ltd, Rasayani
( Maharashtra )

2
 18 : 10488- 1983

Indian Standard
SPECIFICATION FOR
1, 3-PHENYLENEDIAMINE-4-SULPHONIC ACID

0. FOREWORD

0.1This Indian Standard was adopted by the Indian Standards

Institution on 10 February 1983, after the draft finalized by the Dye
Intermediates Sectional Committee had been approved by the Petroleum,
Coal and Related Products Division Council.

0.2 1, 3-Phenylenediamine-4-sulphonic acid ( C&HsOsNsS ) is an

important dye intermediate for dyestuffs. The product is available in
the form of free acid. It is also known as m-phenylenediamine-4r-
sulphonic acid. It is represented by the following structural formula:

1, 3-Phenylenediamine-4Sulphonic Acid
( Molecular Mass 18EV2 )

0.3 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 3 1046S - 1983

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 sampl-
ing and test for 1, 3-phenylenediamine-4-sulphonic acid.

2. REQUIREMENTS

2.1 Description - The material shall be in the form~of yellowish-brown

to brown powder or paste.

2.2 The material shall also comply with the requirements given in
Table 1.

TABLE 1 REQUIREMENTS FOR 1, 3-PHENYLENEDIAMINE-

4-SULPHONIC ACID

CHARACTERISTIC REQUIREMENT METHOD OF TEST

I%. ( REF TO CL No.
IN APPENDIX )

(1) (2) (3) (4)

i) Matter insoluble in sodium hydroxide 0.25 A-l
solution ( on dry basis ), percent
by mass, Max

ii) Assay ( on dry basis ), percent by 85 A-2

mass, Mitz
iii) 1, 3-Phenylenediamine ( on 100 per- 0.5 A-3
cent basis ), percent by mass, Max
L

3. PACKING AND MARKING

3.1 Packing - The material shall be packed in steel drums ( see

IS : 2252-1970t ) lined with suitable polyethylene film or as agreed to
between the purchaser and the supplier. Each container shall be securely
closed.

*Rules for rounding off numerical values ( revised ).

tjpecification for steel drums ( galvanized and ungalvanized ) ( second revision ).

4
 IS : 10468 - 1983

3.2 Marking - Each container shall bear legibly and indelibly the
following information:
a) Name of the material;
b) Name of the manufacturer and his recognized trade-mark,
if any;
c) Gross, tare and net mass; and
d) Batch number.
3.2.1 The containers may also be marked with the IS1 Certification
Mark.
NOTE - The use of the IS1 Certification Mark is governed by the provisions of
the Indian Standards Institution ( Certification Marks ) Act, and the Rules and Regu-
lations made thereunder. The IS1 Mark on products covered by an Indian Standard
conveys the assurance that they have been produced to comply with the require-
ments of that standard under a welldefined system of inspection, testing and quality
control which is devised and supervised by IS1 and operated by the producer. ISI
marked products are also continuously checked by IS1 for conformity to that
standard as a further safeguard. Details of conditions under which a licence for the
use of the IS1 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 as prescribed
in 3 of IS : 5299-1969”.
4.2 Number of Tests
4.2.1 Assay content shall be tested on each of the individual samples.
4.2.2 The remaining requirements given in 2 shall be tested on the
composite sample.
4.3 Criteria for Conformity
4.3.1 The lot shall be declared conforming to the requirements for assay
content if each of the individual samples satisfies the corresponding
requirement given in Table 1.
.4.3.2 The lot shall be considered conforming to the remaining require-
ments if all the test results on the composite sample meet the relevant
specification requirements.

5. METHOD OF TESTS
5.1 Test shall be carried out according to the -methods prescribed in
Appendix A, as indicated in co1 4 of Table 1.

*Methods of sampling and tests for dye intermediates.

5
IS : 1046&- 1983

5.2 Quality of Reagents - Unless specified otherwise, pure chemicals

and distilled water ( see IS : 1070-1977” ) shall be employed in tests.
NOTE - ‘ Pure chemicals ’ shall mean chemicals that do not contain impurities
which affect the results of analysis.

APPENDIX A
( Table 1, and Clause 5.1 )
METHODS OF TEST FOR 1,3-PHENYLENEDIAMINE-I-
SULPHONIC ACID

A-l. DETERMINATION OF MATTER INSOLUBLE IN SODIUM

HYDROXIDE SOLUTION
A-l.1 Reagent
A-US Sodium Hydroxide Solution - Dissolve 5 g of caustic soda pellets
in water contained in 1 OO-ml measuring flask and make up to the mark.

A-l.2 Procedure - Weigh accurately 10 to 15 g thoroughly mixed

sample into a 1 OOO-ml beaker, add 300 ml water and sufficient 5 percent
sodium hydroxide solution to make the solution alkaline to brilliant yellow
paper. Heat the solution to 90°C until the m-phenylenediamine-4-
sulphonic acid is dissolved and filter it through counter poised filter
papers, wash residue well with hot water, dry at lOO”C, cool and weigh.
Reserve the filtrate and washings for assay determination ( seeA-2.2.1 ).
A-l.3 Calculation

Matter insoluble in sodium hydroxide solution,

LV, x 100
percent by mass =
442
where
Ml = mass in g of the residue, and L
M2 = mass in g of the sample taken for the test.

A-2. DETERMINATION OF ASSAY ( BY COUPLING )

A-2.0 Outline of the Method - The material is dissolved in water
adding dilute caustic soda solution. A known volume of the solution is
titrated against standard P-nitrobenzene diazonium chloride solution
and from the consumption of standard diazonium solution, assay is
determined.

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

6
 IS:10468-1983

A-2.1 Reagents

A-2.i.l Hydrochloric Acid - 50 percent ( see-IS : 265-1976* ).

A-2.1.2 Acetic Acid - 30 percent.

A-2.1.3 Sodium Acetate - crystals.

A-2.1.4 H Acid Solution - 1 percent faintly alkaline.

A-2.1.5 Standard p-Nitrohenzene Diazonium Chloride Solution

A-2.2 Procedure

A-2.2.1 Transfer the filtrate and washings reserved at the end of the
test for matter insoluble in sodium hydroxide solution ( see A-l.2 ) to
1-litre beaker, add 30 percent acetic acid until the solution is neutral to
brilliant yellow and congo red papers. Transfer the solution quantita-
tively to I-litre volumetric flask, make up to the mark with water and
mix well.

A-2.2.2 Pipette 50 ml of the above solution into a 500.ml beaker and

add 15 g of sodium acetate. Cool the beaker externally in an ice bath
and titrate with p-nitrobenzene diazonium chloride solution from an ice-
cold water jacketted burette. Stir mechanically, until- a’ faint purple
colour is developed on allowing the clear rim round a drop of the
titrated solution, spotted on filter paper to diffuse into a drop of faintly
alkaline 1 percent H-acid solution 3 minutes after the last addition of
diazo solution added in O-25 ml increments towards the end of the
titration.

A-2.3 Calculation

Assay, percent by mass ( calculated as V X N X 18.8

m-phenylenediamine-4-sulphonic acid ) =
M

where
V = volume in ml of p-nitrobenzene diazonium chloride
solution,
Jv = normality of p-nitrobenzene diazonium chloride solution,
and
M- mass in g of the sample taken for the test.

*Specification for hydrochloric acid ( second r&ion ).

7
IS:10468 - 1983

A-3. DETERMINATION OF m-PHENYLENEDIAMINE IN

m-PHENYLENEDIAMINE-4-SULPHONIC ACID BY PAPER
CHROMATOGRAPHY

A-3.0 General - Ascending paper chromatography has been prescribed

to determine m-phenylenediamine.

A-3.1 Reagents I

A-3.1.1 n-Probanol - distilled.

A-3.-1.2 Saturated Sodium Bicarbonate Solution

A-3.1.3 Sodium Carbonate Solution - 10 percent.

A-3.1.4 Whatman Paper - 3 mm thickness.

A-3.1.5 Hydrochloric Acid - ( see IS : 265-1976* ).

A-3.1.6 p-Dimethyl Aminobenzaldehyde

A-3.1.7 Rectified Spirit-Distilled - ( see IS : 323-19597 ).

A-3.1.8 Solvent Mixture - developing solvent ( n-propanol and saturated

sodium bicarbonate in 2:l ratio ).

-A-3.2 Apparatus

A-3.2.1 Chromatogaphic Tank - 27 x 40 cm size.

A-3.2.2 Sprayer

A-3.3 Preparation of Solution

A-3.3.1 Standard Sample Solution - Weigh exactly 1.0 g ( 100 percent )

of m-phenylenediamine-4-sulphonic acid, dissolve in 10 percent sodium
carbonate solution and make up to 100 ml with distilled water.
A-3.3.2 Standard m-Phenylenediamine Solution - Weigh 1 g ( 100 percent )
of above material, dissolve in distilled water and make up to 1 000 ml
with distilled water. From this pipette out 5 ml, 10 ml and 20 ml in
100 ml flask and make up to mark with distilled water. Call these
solutions A, B and C respectively.

A-3.3.3 Spots

A-3.3.3.1 Sample solution - 0.01 ml is equivalent to 100 micrograms,

*Specification for hydrochloric acid ( second revision ).

tSpecification for rectified spirits ( reuised ).

8
 IS : 10468 - 1983

A-3.3.3.2 m-Phenylenediamine solution

0.01 ml (A) = 0.5 ~percent

0.01 ml (B) = 1.0 percent
0.01 ml (C) = 2-O percent
A-3.4 Preparation of Tank

A-3.4.1 Place 200 ml of developing mixture into the chromatographic

tank and replace the lid. Allow to equilibrate for about an hour.
A-3.5 Development of Chromatogram

A-3.5.1 After spotting and drying, suspend the paper from the support-
ing rod by means of clips so that a lower edge of the paper is just
touching the surface of the developing solvent but is not supported on
the bottom of the tank. Allow the chromatogram to develop for about
16 hours. After developing and drying, it is sprayed with 1 percent
solution of p-dimethyl aminobenzaldehyde which is prepared as follows.
A-3.5.1.1 Weigh approximately 1 g of p-dimethyl aminobenzaldehyde
and dissolve it in 5 ml of concentrated hydrochloric acid. To this
95 ml of rectified spirit ( distilled ) is added and the solution is well
mixed.
A-3.6 Reagents

A-3.6.1 The following chromatogram develops:

pi1 m- PHENYLENE-
VIAMINE 0 l

ii1 MAIN. BAND OF

1.3. PHENYLENEDIAMINE- 0
L-SlJLPHONIC AC10 0

...
111J SPOT 0
0

A-3.7 Assessment - Compare the standard spot and evaluate m-pheny-

lenediamine content.

9
INTERNATIONAL SYSTEM OF UNITS ( SI UNITS )
Base Units

QUANTITY UNIT SYMBOL

Length metre In

M;lSS kilogram kg
Time second s
Electric current ampere A
Thermodynamic kelvin K
temperature
Luminous intensity candela cd
Amount of substance mole mol

Supplementary Units

QUANTITY UNIT SYMOOL

Plane angle radian rad

Solid angle steradian ST

Derived Units

QUANTITY UNIT SYMBOL DEFINITION

Force newton N 1 N = 1 kg.m/ss

Energy joule J 1 J = I N.m
Power watt W 1 W = 1 J/s
Flux weber Wb 1 Wb = 1 V.s
Flux density tesla T 1 T = 1 Wb/m
Frequency hertz HZ 1 Hz = 1 c/s (s-1)
Electric conductance siemens S 1 S = 1 A/V
Electromotive force volt V 1 V = 1 W/A
Pressure, stress Pascal Pa 1 Pa = 1 N/ma