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है”ह”ह

IS 15079 (2001): 2:4-Dinitroroaniline, Technical [PCD 9:Organic Chemicals Alcohols and Allied Products and DyeIntermediates]

2:4

IS 15079:2001

w’mrm%-

\ n n Y nW+ll$

Dyes lntcrmedititc ,’%ctional Committee, PCD I 1

t“ofWWoRD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Dyeslo(ermcdiate Sectional Committee had been approved by the Petroleum, Coal and Related Products Division

Council,

~ : 4. Dinitroaniline (CbH5NJO~) is an impofiant dye intermediate, used in the manufacture of disperse dyes. It is

represented by the following structural formula :NH ~

NO ~

2: 4-Dinitroaniline(Molecular Mass: 183)

[CAS Registry No. 97-02-9]

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

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 accordance with1S 2:1960 ‘Rules for rounding off numerical values (revi.re~’. The number of significant places retained in therounded off value should be the same as that of the specified value in this standard.

.

IS 15079:2001

Indian Standard

2: 4-DINITROROANILINE,TECHNICAL — SPECIFICATION

1 SCOPE

This standard prescribes the requirements andmethods of sampling and test for 2: 4-Dinitroaniline,technical.

2 REFERENCES

The following Indian Standards contain provisionswhich, through reference in this text constituteprovisions of this standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision and parties to agreement basedon this standard are encouraged to investigate the

possibility of applying the most recent editions ofthe standards given below:

IS No. Tide

107(!:1992 Reagent grade water (third revision)5299:2001 Methods for sampling and tests for

dye-intermediates (firsl revision)

3 REQUIREMENTS

3.1 Description

The material shall be in the form of yellow to yellowishbrown, moist or dry powder and shall be free from

visible impurities.

3.2 The material shall also comply with therequirements given under Table 1.

Table 1 Requirement for 2: 4-Dinitroaniline,Technical

S1 Characteristics Requirement Method ofNo. Test, Ref to(1) (2) (3) (4)

I) Assay, percent by mass 98.0 Annex A(on d,-ybasis), Mi/~

ii) Mel[ing point of dry 178 cl 9 of ISmalcrial, ‘C, kfin 5299

ii!) Matter insoluble in 0.2 clll of Ismethanol, percent by 5299

mass, Mm

ii ) 2 : 4- Dinitrochlorobenzene, 0.2 Annex B

percent by mass

(on 100(% basis), Max

4 PACKINGAND MARKING

4.1 Packing

The material shall be packed as agreed to betweenthe purchaser and the supplier.

4.2 Marking

Each container shall be securely closed and shall bearlegibly and indelibly the following information:

a) Name of the material;b) Indication of the source of manufacture;

c) Net mass;d) Lot or batch number; ande) Month and year of manufacture.

4.2.1 BIS Certification Marking

4.2.1.1 Each container may also be marked with theStandard Mark.

4.2.1.2 The use of the Standard Mark is governed by

the provisions of the Bureau of Indian Standards Act,1986 and the Rules and Regulations made thereunder.The details of conditions under which the licence for the

use of Standard Mark maybe granted to manufacturersor producers maybe obtained from the Bureau of Indian

Standards.

5 SAMPLING

5.1 The method of drawing representative samples ofthe material shall be as prescribed in 4 of IS 5299.

5.2 Number of Tests

Tests for assay, melting point and 2,4-

dinitrochlorobenzene shall be done on each sample.Tests for matter insoluble in methanol and description

shall be performed on the composite sample.

5.3 Criteria for Conformity

5.3.1 For Individual Samples

The lot shall be declared as conforming to therequirements of ’the assay, melting point and 2,4-

dinitrochlorobenzene, if each of the individual test results

satisfies the relevant requirements given at 3.1 and inTable 1.

5.3.2 For Composite Samples

For declaring the conformity of the lot to the requirementsof matter insoluble in methanol and description whiletested on the composite sample, the test result shall

satisfy the relevant requirements given in Table 1.

6 TEST METHODS

6.1 Tests shall be conducted according to the methodsprescribed and as indicatedinCO14 of Table 1.

1

IS 15079:2001

6.2 Quality of Reagents NOTE— ‘Pure chemicals’ shall mean chemicals that donot contain impurities which affect the results of analysis.

Unless specified otherwise, pure chemicals and distilled

water (.~ee IS 1070) shall reemployed in tests.

ANNEX A

[Table 1, SINO. (i) ]*.

DETERMINATION OF ASSAY

A-1 GENERAL

The content of 2: 4-dinitroaniline is determined by gas

chromatographic analysis. For detailed test procedure,reference may be made to IS 5299. However, the

conditions for a typical chromatographic analysis of2:4-din itroaniline is given below for guidance only.

A-2 APPARATUS

.4-2.1 Any suitable gas chromatography and columncapable of being operated under conditions suitablefor resolving the individual constituents into distinct

peaks may be used.

Sample

Injection quantity

Column

MaterialLength

Or@ce

Packing material

Carrier Gas

Conditions

CarrierJow rate

Oven temperature

[i~ection port

feulperature

2 : 4-Dinitroaniline (20percent solution in dimethyl

formamide)0.8 microliters

glass

2m0.3 cm ID10 percent OV 101

on Chromosorb WHP,80-100 Mesh

Nitrogen

30mhinljo”c

8 C~min programming to250 C hold 25 minutes330”C

Detector

Type F.I.D

Temperature 330°c

A-2.2 Interpretation of Chromatogram

The peak for 2: 4-dinitroaniline is shown at 14.33minutes. Atypical Chromatogram under the conditionsgiven above is shown in Fig. 1.

1

—FIG. 1 ATYPICALCHROMATOGRAMOF2:4-

DINITROANtLINE

A-2.3 Calculation

Follow the procedure given below for calculation when

internal standard method is employed:

Percent by massConcentration Area of peak Strength of

of standard x inthe sample x standardof2:4- ——

DinitroanilineConcentration Area of peak

of sample x of standard

Similarly other fraction can also be calculated.

2

IS 15079:2001

ANNEX B

[Table 1, SINO. (iv)]

THIN LAYER CHROMATOGRAPHIC ANALYSIS FOR 2: 4-DINITROCHLOROBENZENE

B-O GENERAL spot : 10microlitre of test

The content of 2 :4-dinitrochlorobenzene is determinedSample solution of sample A

by thin layer chromatographic analysis. Reference mayand 10 micro-litre

be made to IS 5299 for details of GC test method to beof test solutions of

followed. However, necessary details of test conditionsstandard solution B.

are given here for guidance only.Thin layer plate : Silica gel G

Developer : TolueneB-1 PROCEDURE

Run : 12 ems.

A typical condition for TLC analysis of 2 : 4- Detection : 0.5%p-Dimethylaminodinitrochlorobenzene is given below: benzaldehyde +

Test solution of : 1?4. (on 100’?4obasis) in 10?40stannous

2: 4-Dinitroaniline acetone chloride (1: 1).

Sample- A B-2 REPORT

Test solution of standard : 0.0025~0, 0.0050’?4.Report 2: 4-Dinitrochlorobenzene content as that which

and 0.007 5°/0is nearest in intensity to standard. In case the colour

2: 4-Dinitro- solution in acetone intensity does not come in the range of standard spots,chlorobenzene repeat the whole procedure using different percentageSample - B of standard 2: 4-Dinitrochlorobenzene.

IS 15079:2001

ANNEX C

(Foreword)

COMMITTEE COMPOSITION

Dyes Intermediate Sectional Committee, PCD 11

Organization

AIUI Limited, Valsad, Gajarat

Ajanla Chemical Irrdustrics, New Delhi

Colour-Chem Ltd, Mumbai

Clariant India Ltd, Mumbai

DeYclopment Comm Small Scale Industries, New Delhi

tlinduslan Ciba-Geigy India Ltd, Mumbal

!{industan organic Chemicals Ltd, Rasayani

Indian Dyestuff industries Ltd, Mumbai

Indian Chemical Manufacturers Association, Kollwta

Nnt]onal Chemical Laboratory, Pune

Sudarshan Chemical Industries Ltd, Pune

The Dyestuff Manufacturer’s Association of India, Mumbai

The Gujarat Small Scale Dyestuffs Manufacturer’sAssociation, Ahmedabad

BIS Directorate General

Represerrlative(s)

DR H. KMWAR (Chairman)SHRI H. B. DHUVAD (Alterrrate I)

DR J. G. DESAI (Alternate II)SHRI A. R. DESAI (Alternate 111)

SHRIS. D. BHARDWAJSHRI KAPIL DEV (Aherna/e)

DR S. SIDOHANSHRJA. K. CHAT-TERJEE(A/terna~e I)SHRI K. K. MEHTA (Affernate II)

DR J. N. SHAH

SHRI K. S. RINDANI (Alternate)

SHRIS. R. SI~GHDR J. S. REKHI (Alternate)

SHRIS. RAJAGOPALAN

SHRI D. K. MURTHY (A//ernate)

SHRIR. B. BHA~DARE

DR S. S. PATIL (A/fer-rrate)

DR S. R. DESHMLIKHSHRI S. D. PAWAR(Alternate)

SHRIG. C. DESAI

DR K. V. SRINIVASAN

SHRIR. SAnANARAYAN

SHRI P. K. PARAJJ(Alternate)

DR M. G. NARSIAN

DR S. C. AMIN (Alternate)

SHRJR. S. PATEL

SHIU R. R. SHAH (Alternate)

SHRJANJAN KAR, Director & Head (PCD)[Representing Director General ( E.-r-officio)]

Member-Secretary

DR SHRJMATIVIJAYMALIK

Director (PCD), BIS

4

L

Bureau of Indian Standards

BIS is a statutory institution established under the Bureazi of Indian Standards Act, 1986 to promoteharmonious development of the activities of standardization, marking and quality certification of goodsand attending to connected matters in the country.

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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 reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. PCD 11 ( 1301 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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