8/12/2019 is.4527.1968

1/20

Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to

information for citizens to secure access to information under the control of public authorities,in order to promote transparency and accountability in the working of every public authority,

and whereas the attached publication of the Bureau of Indian Standards is of particular interest

to the public, particularly disadvantaged communities and those engaged in the pursuit of

education and knowledge, the attached public safety standard is made available to promote the

timely dissemination of this information in an accurate manner to the public.

!"#$% '(%)

!"# $ %& #' (")* &" +#,-.Satyanarayan Gangaram Pitroda

Invent a New India Using Knowledge

/0)"1 &2 324 #' 5 *)6Jawaharlal Nehru

Step Out From the Old to the New

7"#1&"8+9&"), 7:1&"8+9&")Mazdoor Kisan Shakti Sangathan

The Right to Information, The Right to Live

!"# %& ;

8/12/2019 is.4527.1968

2/20

8/12/2019 is.4527.1968

3/20

8/12/2019 is.4527.1968

4/20

BIS 2005

B U R E A U O F I N D I A N S T A N D A R D S

MANAKBHAVAN, 9BAHADURSHAH ZAFARMARGNEWDELHI 110002

IS :4527 - 1968

(Reaffirmed 2000)

Edition 1.1

(2002-03)

Price Group 4

I nd i an StandardSPECIFICATION FOR

2-NITRO-4-CHLOROTOLUENE

(Incorporating Amendment No. 1)

UDC 668.811.2 : 668.741.1

8/12/2019 is.4527.1968

5/20

IS :4527 - 1968

B U R E A U O F I N D I A N S T A N D A R D S

MANAKBHAVAN, 9BAHADURSHAH ZAFARMARGNEWDELHI 110002

I nd i an Standard

SPECIFICATION FOR2-NITRO-4-CHLOROTOLUENE

Dye Intermediates Sectional Committee, CDC 46

Chai rm an Repr esen t i ng

DRB. D. T ILAK National Chemical Laboratory (CSIR), Poona

M ember s

DRL . K. BEHL Indian Drugs & Pharmaceuticals Ltd, New DelhiDRH. L . BAMI ( Alternate)

SHRI J OGINDERSINGH Directorate General of Technical Development,New Delhi

DRH. KAIWAR Indian Chemicals Manufacturers Association,Calcutta

DRG. R. N. SASTRY( Alternate)SHRI G. A. KULKARNI Amar Dye-Chem Ltd, Bombay

SHRIS. V. DESAI( Alternate)SHRI C. C. MANIAR Indian Dyestuff Industries Ltd, BombaySHRI K . C. MARFATIA The Dyestuffs Manufacturers Association of India,

BombaySHRIJ . C. ISSRANI ( Alternate)

SHRI S. M. MEHTA The Atul Products Ltd, AtulSHRIM. V. DESAI( Alternate)

DRR. J . RATHI Sudarshan Chemical Industries Private Ltd, Poona

SHRIK . L. RATHI( Alternate)SHRI L. J . RUNDLE I .C.I . (India) Private Ltd, CalcuttaSHRI SANTOKHSINGH National Chemical Industries, New Delhi

SHRIKULWANTSINGH( Alternate)DRH. A. SHAH Development Commissioner, Small Scale Industries,

New DelhiSHRIN. K. SEN( Alternate)

DRG. S. SIDHU Regional Research Laboratory (CSIR), HyderabadDRG. THYAGARAJ AN( Alternate)

SHRI B. SINGH Hindustan Organic Chemicals L td, BombaySHRIA. D. PATANKAR( Alternate)

DRD. R. SWAYAMPATI Suhrid Geigy Ltd, Baroda

DRO. P. M ITTAL( Alternate)SHRI D. DASGUPTA,Director (Chem)

Director General, I SI ( Ex-offi cio M ember)

Secretary

DRA. K. BHATTACHARYA

Deputy Director (Chem), ISI

( Conti nu ed on page2 )

8/12/2019 is.4527.1968

6/20

IS :4527 - 1968

2

( Conti nu ed from page1 )

Drafting Panel for Chloronitro Dye Intermediates, CDC 46 : P6

Convener Repr esen t i ng

SHRIG. A. KULKARNI Amar Dye-Chem Ltd, Bombay

M ember s

SHRISANTOKHSINGH National Chemical Industries, New Delhi

SHRIKULWANTSINGH( Alternate)

8/12/2019 is.4527.1968

7/20

IS :4527 - 1968

3

I nd i an Standard

SPECIFICATION FOR

2-NITRO-4-CHLOROTOLUENE0. F O R E W O R D

0.1This Indian Standard was adopted by the Indian StandardsInstitution on 9 J anuary 1968, after the draft finalized by the DyeIntermediates Sectional Committee had been approved by theChemical Division Council.

0.22-Nitro-4-Chlorotoluene (C7H6O2ClN) is used as diazo componentin the manufacture of dyestuffs of the azo series. It has the following

structural formula:

0.3This standard is one of a series of Indian Standards on dye inter-mediates. A complete list of such standards is given on page 15.

0.4This edition 1.1 incorporates Amendment No. 1 (March 2002). Sidebar indicates modification of the text as the result of incorporation ofthe amendment.

0.5For the purpose of deciding whether a particular requirement of thisstandard is complied with, the final value, observed or calculated,expressing the result of a test or analysis, shall be rounded off inaccordance with IS : 2-1960*. The number of significant places retainedin the rounded off value should be the same as that of the specified valuein this standard.

(CAS No. 89-59-8)

*Rules for rounding off numerical values ( r evi sed).

8/12/2019 is.4527.1968

8/20

IS :4527 - 1968

4

1. SCOPE

1.1This standard prescribes the requirements and the methods ofsampling and test for 2-Nitro-4-Chlorotoluene.

2. REQUIREMENT2.1Description The material shall be in the form of light yellowishgreen solid or pale yellowish liquid or a mixture thereof.

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

3. PACKING AND MARKING

3.1Packing Unless otherwise agreed, the material shall be packedin suitable drums ( seeIS : 2552-1963* ).

3.2Marking The containers shall be securely closed and shall bearlegibly and indelibly the following information:

3.2.1The containers may also be marked with the ISI Certification Mark.NOTE The use of the ISI Certification Mark is governed by the provisions of theIndian Standards Institution (Certification Marks) Act, and the Rules and Regulationsmade thereunder. Presence of this mark on products covered by an Indian Standardconveys the assurance that they have been produced to comply with the requirementsof that standard, under a well-defined system of inspection, testing and quality controlduring production. This system, which is devised and supervised by ISI and operatedby the producer, has the further safeguard that the products as actually marketed arecontinuously checked by ISI for conformity to the standard. Details of conditions, underwhich a licence for the use of the ISI Certification Mark may be granted tomanufacturers or processors, may be obtained from the Indian Standards Institution.

TABLE 1 REQUIREMENTS FOR 2-NITRO-4-CHLOROTOLUENE

SLNO.

CHARACTERISTIC REQUIREMENT METHODOFTEST,REFTOCLNO. OF

Appendix A IS : 548-1964*(1) (2) (3) (4) (5)

i) Crystallizing point, C, M i n 33 A-2

ii) Assay, percent by weight, M i n 99 A-3

iii) Moisture content, M ax 0.5 5.3

iv) Matter insoluble in methanol,percent by mass, M ax

0.2 when tested as perIS : 5299-2001

*Methods of sampling and test for oils and fats ( r evi sed).

Calculated on molecular weight 171.6.

*Specification for steel drums (galvanized and ungalvanized).

a) Name of the material;b) Name of the manufacturer;c) Batch number; andd) Net, gross and tare weight.

8/12/2019 is.4527.1968

9/20

8/12/2019 is.4527.1968

10/20

IS :4527 - 1968

6

A-2.1.1Ou ter Gl ass Test-T ube serves as an air jacket and is weightedwith lead shots or a similar loading material. I t is provided with a corkthrough which the inner tube ( seeA-2.1.2 ) is held in position.

A-2.1.2 I nn er Glass Test-Tu be fitted with a cork which carries astirrer in the form of a loop of glass with a glass stem and thethermometer placed centrally within the tube and the glass loop. Thebottom of the bulb of the thermometer shall be about 10mm from thebottom of the inner tube. The cork is so fixed that the immersion markon the thermometer is in level with the top of the cork.

A-2.1.3Cool in g Bath 1 000-ml beaker about 150 mm in height. Thelevel of the cooling liquid in the bath shall be at least as high as thelevel of the sample in the inner tube.

A-2.1.4Thermometer The dimensions of the thermometer* shall be asfollows:

*Thermometers with the mark F 75C/100 conform to these requirements ( seeB.S.593 : 1954 ).

Range 24 to 78CGraduation, at each 0.2CLonger lines, at each 1CPartial figuring, at each 2CFull figuring, at each 10CImmersion 100 mmThickness of graduation line,

M ax

0.10 mm

Overall length, M ax 385 mmLength of main scale, M i n 190 mmBulb length 15 to 20 mmStem diameter 6.0 to 7.5 mmDistance from bottom of bulb

to bottom of main scale,M ax

125 mm

Distance from bottom of bulbto top of contractionchamber,M ax

35 mm

Maximum error 0.2CMaximum error in an interval 0.2/10CBulb shape CylindricalBulb diameter Not to exceed, stem diameterExpansion chamber Elongated or pear-shaped with a

hemispherical topTop finish Ring

8/12/2019 is.4527.1968

11/20

IS :4527 - 1968

7

A-2.1.4.1 Any thermometer of similar range and accuracy may be used.

A-2.1.4.2The thermometer shall bear a certificate from the NationalPhysical Laboratory, New Delhi or any other institution authorized by

the Government of I ndia to issue such certificate.

All dimensions in millimetres.

F IG. 1 CRYSTALLIZINGPOINT(ASSEMBLYOFAPPARATUS)

8/12/2019 is.4527.1968

12/20

IS :4527 - 1968

8

A-2.2 Procedure

A-2.2.1Remove the inner tube of the apparatus from its jacket andintroduce about 20 g of the material. Immerse the tube partially in a

bath having a temperature of about 5C above the crystallizing point ofthe material so that the crystals melt, except for a trace necessary forseeding. Replace the inner tube in its jacket and assemble theapparatus as shown in Fig. 1, with the cooling bath between 6 and 8Cbelow the expected crystallizing point.

A-2.2.2Take the thermometer readings at intervals of half a minute,with continuous and gentle stirring. The highest temperature reachedduring solidification is regarded as the crystallizing point. Usualthermometer corrections shall be made.

A-2.2.3 I f supercooling should take place as shown by the rise intemperature, the constant temperature should be observedimmediately after the temperature-rise. A temperature-rise of 1Cshall be regarded as the maximum allowable.

A-2.2.4 I f a constant temperature is not obtained over the first fivereadings after the rise in temperature, six readings shall be takencommencing with the point at which the maximum temperature isfirst attained. The readings shall be plotted on a graph paper againsttime intervals and a straight line drawn to lie evenly between the first

and second and between the fifth and sixth of the six points justmentioned. This line shall be produced backwards until it intersectsthe portion of the curve before the temperature-rise. The point ofintersection shall in this case be taken as the crystallizing point.

A-3. ASSAY

A-3.0Outline of the Method The nitro group is reduced with zincand concentrated hydrochloric acid. The resulting amine is thentitrated (diazotized) with standard sodium nitrite solution, using

starch-iodide paper as an indicator.A-3.1 Reagents

A-3.1.1Aci t i c Aci d Analytical reagent grade.

A-3.1.2Concent r ated H ydr ochl or i c AcidseeIS : 265-1962*.

A-3.1.3Zi nc Dust

A-3.1.4Potassi um B r om id eseeI S : 2797-1964.

*Hydrochloric acid ( revised).

Specification for potassium bromide.

8/12/2019 is.4527.1968

13/20

IS :4527 - 1968

9

A-3.1.5Star ch-I odi de Test Paper s

A-3.1.6Standar d Sodi um N i t r i te Solu t ion0.2 N, freshly standardized.

A-3.1.6.1 Prepar ati on of t he sol ut i on Weigh accurately 13.8g of the

sodium nitrite, analytical reagent quality, and transfer into a 1000-mlvolumetric flask. Dissolve it in the requisite quantity of water bygently shaking and then make up the volume.

A-3.1.6.2 Standar di zat ion of the sodi um ni t r i t e

A-3.2Procedure Weigh accurately about 1.2 g of the material intoa 250-ml beaker. Dissolve completely in 40 ml of acetic acid, dilute with10 ml of distilled water. Cool to 0 to 5C by adding crushed ice. Add 5 gof zinc dust and 20 ml of concentrated hydrochloric acid and let thesample react for 30 minutes at this temperature. Stir frequently. Addanother 5 g of zinc dust and 15 ml of concentrated hydrochloric acid,reduce for 30minutes at the same temperature with frequent stirring.Repeat the above operation for the third time. Filter the reduced

solution through a filter paper into a 600-ml beaker and wash with

a) Weigh accurately 4.3 g of the sulphanilic acid, analytical reagentquality, and transfer into a 250-ml volumetric flask. Dissolve itin the requisite quantity of water by gently shaking and thenmake up the volume. Pipette 50ml of the solution into a beaker.Alternatively weigh out accurately 0.85g of the sulphanilic acidinto a beaker and dissolve in the requisite amount of water.

b) Add 25 ml of hydrochloric acid to the solution. Immerse the beakerin chopped ice and water until the temperature is about 5C. Thisis to lower the chances for loss of nitrous acid. While stirringmechanically, titrate with sodium nitrite solution which is addedthrough a thistle funnel the end of which is well inside the solution,as rapidly as the spot test will permit. The end point is reachedwhen an immediate blue coloured ring appears on a starchiodidetest paper which may be obtained repeatedly during the period of

10minutes without the further addition of sodium nitrite solution.c) Calculate the exact strength of the sodium nitrite by using the

following formula:

Normality of sodium nitrite solution

where

N=Normality of standard sulphanilic acid solution,

V=Volume in ml of sodium nitrite solution required for the

titration.

N 50V

-----------------=

8/12/2019 is.4527.1968

14/20

IS :4527 - 1968

10

water until a volume of 250 ml is collected. Add 5g of potassiumbromide and 20 ml of concentrated hydrochloric acid. Cool to about 0 to5C with crushed ice and titrate with standard sodium nitrite solutionwhich is added through a thistle funnel the end of which is well insidethe solution, as rapidly as the spot test will permit. The end point isreached when an immediate blue coloured ring appears on starchiodide test paper which may be obtained repeatedly during the periodof 10minutes without the further addition of sodium nitrite solution.

A-3.3 Calculation

where

A P P E N D I X B

( Clause4.1 )

SAMPLING OF 2-NITRO-4-CHLOROTOLUENE

B-1. GENERAL REQUIREMENTS OF THE SAMPLING

B-1.0 In drawing, preparing, storing and handling test samples, thefollowing precautions and directions shall be observed.

B-1.1Samples shall be taken at a place protected from damp air, dustand soot.

B-1.2Sampling instrument shall be clean and dry.

B-1.3Precautions shall be taken to protect the samples, the materialbeing sampled, the sampling instrument, and the containers forsamples from adventitious contamination.

B-1.4To draw a representative sample, the contents of each container,selected for sampling, shall be mixed, as thoroughly as possible, bysuitable means.

B-1.5The samples shall be placed in clean, dry and air-tight glass or

other suitable containers on which the material has no action.

Assay, percent by weight (calculatedon molecular weight 171.6) =

V = volume in ml of standard sodium nitrite solution,

N = normality of standard sodium nitrite solution, and

W = weight in g of sample taken for the test.

17.16 V NW

------------------------------------

8/12/2019 is.4527.1968

15/20

IS :4527 - 1968

11

B-1.6The sample containers shall be of such a size that they arealmost completely filled by the sample.

B-1.7Each sample container shall be sealed air-tight after filling and

marked with full details of sampling, the date of sampling, year ofmanufacture, and other important particulars of the consignment.

B-1.8Samples shall be stored in a cool and dry place.

B-2. SAMPLING INSTRUMENT

B-2.0The following forms of sampling instruments may be used:

a) Sampling bottle or can for taking samples from various depths inlarge tanks, and

b) Sampling tube.

B-2.1Sampling Bottle or Can It consists of a weighted bottle ormetal container with removable stopper or top, to which is attached alight chain ( seeFig. 2 ). The bottle or can is fastened to a suitable pole.For taking a sample, it is lowered in the tank to the required depth,and the stopper or top is removed by means of the chain for filling thecontainer.

F IG. 2 SAMPLINGBOTTLEORCAN

8/12/2019 is.4527.1968

16/20

IS :4527 - 1968

12

B-2.2Sampling Tube It is made of metal or thick glass and isabout 20 to 40 mm in diameter and 400 to 800 mm in length ( seeFig. 3 ). The upper and lower ends are conical and reach 5 to 10 mmdiameter at the narrow ends. Handling is facilitated by two rings atthe upper end. For taking a sample, the apparatus is first closed at thetop with the thumb or a stopper and lowered until the desired depth isreached. I t is then opened for a short time to admit the material andfinally closed and withdrawn.

B-2.2.1 For small containers, the size of the sampling tube may bealtered suitably.

F IG. 3 SAMPLINGTUBE

8/12/2019 is.4527.1968

17/20

IS :4527 - 1968

13

B-3. SCALE OF SAMPLING

B-3.1Lot All the containers in a single consignment of the materialdrawn from a single batch of manufacture shall constitute a lot. I f a

consignment is declared or known to consist of containers pertaining todifferent batches of manufacture, then the containers belonging to thesame batch of manufacture shall be grouped together and each suchgroup shall constitute a separate lot.

B-3.2For ascertaining the conformity of the lot to the requirements ofthis specification, tests shall be carried out for each lot separately. Thenumber ( n) of containers to be selected for drawing the samples shalldepend upon the sizes ( N) of the lot and shall be in accordance withTable 2 given below:

B-3.3These containers shall be selected at random from the lot and toensure the randomness of selection, random number tables shall beused. In case, such tables are not available, the following proceduremay be adopted:

Starting from any container, count them in one order as 1, 2,3, .................., up to rand so on, where ris the integral part of N/n( Nbeing the lot size and nbeing the number of containers to beselected ). Every rth container thus counted shall be withdrawn to

give sample for test.

TABLE 2 NUMBER OF CONTAINERS TO BE SELECTED FOR SAMPLING

LOTSIZE NO. OFCONTAINERSTOBE SELECTED

N n

(1) (2)

4 to 15 3

16 ,, 40 4

41 ,, 65 5

66 ,, 110 6

111 ,, 200 7

201 and above 8

NOTE When the size of the lot is 3 or less, all the containers shall be sampled.

8/12/2019 is.4527.1968

18/20

IS :4527 - 1968

14

B-4. TEST SAMPLE AND REFEREE SAMPLE

B-4.1From each of the containers selected as in B-3.2,draw with anappropriate sampling implement small portions of the material from

different parts of the container. The total quantity so drawn from eachof the containers shall be a little more than thrice the quantityrequired for testing purposes.

B-4.2Mix thoroughly all the portions of the material drawn from thesame container to give a representative sample for the container.

B-4.3From the samples ( seeB-4.2 ) representing different containersselected in B-3.2,a small but equal quantity of material shall be takenand thoroughly mixed to form a composite sample, which shall be dividedinto three equal parts, one for the purchaser, another for the supplier and

the third for the referee.B-4.4The remaining portion of the material in each sample ( seeB-4.2 )from each different container shall be divided into three equal parts, eachforming an individual sample. One set of individual samplesrepresenting thencontainers selected shall be for the purchaser, anotherfor the supplier and the third for the referee.

B-4.5All the individual and composite samples shall be transferred toseparate container. These containers shall then be sealed air-tight withstoppers and labelled with full identification particulars given in B-1.7.Care shall be taken not to expose the sample to acid and alkali fumes.

B-4.6The referee samples consisting of a composite sample and a setof nindividual samples, shall bear the seals of both the purchaser andthe supplier and shall be kept at a place agreed to between the two.This shall be used in case of any dispute between the two.

B-5. NUMBER OF TESTS

B-5.1Assay and test for the determination of crystallizing point shallbe conducted on each of the individual samples ( seeB-4.4 ) separately.

B-5.2Tests for the determination of moisture content shall beconducted on the composite sample ( seeB-4.3 ).

B-6. CRITERIA FOR CONFORMITY

B-6.1For Individual Samples The lot shall be declared asconforming to the requirements of assay and crystallizing point, if eachof individual test results as obtained in B-5.1,satisfies the correspondingrequirements given in Table 1.

B-6.2 For Composite Sample The lot shall be declared as conformingto the requirement of moisture content, if the test results as obtained

in B-5.2,satisfy the corresponding requirement given in Table1.

8/12/2019 is.4527.1968

19/20

I N D I A N S T A N D A R D S

ON

Dye Intermediates

IS:

2630-1964 Nitrobenzene, technical

2740-1964 Sulphanilic acid, technical

2741-1964 -naphthol

2744-1964 -naphthylamine

2833-1964 Aniline, technical

3229-1965 Naphthionic acid (sodium salt)

3242-1965 -oxynaphthoic acid (bon acid)

3562-1965 p-nitrotoluene, technical

4265-1967 4-4 diaminostilbene 2-2'disulphonic acid

4334-1967 o-chloroaniline

4335-1967 m-chloroaniline

4336-1967 p-choroaniline

4525-1968 p-aminoacetanilide ( under pr i n t)

4526-1968 2,5-dichloroaniline

4527-1968 2-nitro-4-chlorotoluene

8/12/2019 is.4527.1968

20/20

Bureau of Indian Standards

BI S is a statutory institution established under theBur eau of Indi an Standard s Act, 1986 to promoteharmonious development of the activities of standardization, marking and quality certification ofgoods and attending to connected matters in the country.

Copyright

BI S has the copyright of all its publications. No part of these publications may be reproduced in anyform without the prior permission in writing of BI S. This does not preclude the free use, in the courseof implementing the standard, of necessary details, such as symbols and sizes, type or gradedesignations. Enquiries relating to copyright be addressed to the Director (Publications), BI S.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are alsoreviewed periodically; a standard along with amendments is reaffirmed when such review indicatesthat no changes are needed; if the review indicates that changes are needed, it is taken up forrevision. Users of Indian Standards should ascertain that they are in possession of the latestamendments or edition by referring to the latest issue of BIS Catalogue and Standards : MonthlyAdditions.

This Indian Standard has been developed by Technical Committee : CDC 46 and amended by PCD 11

Amendments Issued Since Publication

Amend No. Date of Issue

Amd. No. 1 March 2002

BUREAU OF INDIAN STANDARDS

Headquarters:

Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002.Telephones: 323 01 31, 323 33 75, 323 94 02

Telegrams:Manaksanstha(Common to all offices)

Regional Offices: Telephone

Central : Manak Bhavan, 9 Bahadur Shah Zafar MargNEW DELHI 110002

323 76 17323 38 41

Eastern : 1/14 C. I. T. Scheme VI I M, V. I . P. Road, Kankurgachi

KOLKATA 700054

337 8499, 33785 61

337 8626, 337 91 20

Northern : SCO 335-336, Sector 34-A, CHANDIGARH 160022 60 38 4360 20 25

Southern : C. I . T . Campus, IV Cross Road, CHENNAI 600113 2350216, 235 04 42235 1519, 235 23 15

Western : Manakalaya, E9 MIDC, Marol, Andheri (East)MUMBAI 400093

832 9295, 832 78 58832 7891, 832 78 92

Branches : AHMEDABAD. BANGALORE. BHOPAL. BHUBANESHWAR. COIMBATORE.FARIDABAD. GHAZIABAD. GUWAHATI. HYDERABAD. J AIPUR. KANPUR. LUCKNOW.NAGPUR. NALAGARH. PATNA. PUNE. RAJ KOT. THIRUVANANTHAPURAM.VISHAKHAPATNAM