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.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 711 (1970): Ferric chloride, technical [CHD 1: InorganicChemicals]

IS: 711 -1970 ( Reaffirmed 1978 )

Indian Standard

SPECIFICATION FOR 17’ERRIC CHLORIDE, TECHNICAL

( First Revision )

Third Reprint AUGUST 1997

UDC 661.572.32

0 Copyright 1970

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

NEW DELHI 110001

Gr 4 October 1970

Indian Standard

IS : 711.1970 ( Reaffirmed 1978 )

SPECIFICATION FOR FERRIC CHLORIDE, TECHNICAL

( First Revision) -

Alkalis arid C3ilorino Sectiorml Committec~, CIX: 25

Chairman Rqmsenlin,q ,%rrt I h4 L. SFTU . , Thta l’kllli Cloth & Cknr~~al h4ills Co I,td. Sew l)rhi

Mmbm

SHI:I S. AIIU~~UG\X ‘I’hr ‘l’ravanrore Kayons Ltd, Rayonpuram SHRI P. S. HAI~THAI<AKKISITNAV

( .-4llcmnte j Snnr A. K. BHATTACHARYYA SHRI P. K. CIIAKRAVAIITY

S,lrionaI l‘tw House, Calcutta Directorate General of Supplies & Disposals, . _

New Delhi SHRI G. S. SAVKAR ( Alternate )

SHT~I R. M. DIKSHIT Ministry of Defence ( DGI ) SHEI K. L. GAM~HIR Salt Commissioner, Government of India, Jaipur

SIII:I B. K. ROY ( Alternnfc) SHRI CL A. GHAREKRAN The Ahmedabad Mfg & Calico Printing CO Ltd

( Calico Chemicals & Plastics Division ), Bombay SHRI K. I>. .JAIN Directorate General of Technical Development,

New Delhi SHI~I L. R. KIIISIINAMUJ~THY The Mettur Chemical & Industrial Corporation Ltd.

Mcttur Dam II. S. f Salem Distt ) SII RI M. P.\r)ua~.an,\~ ( Alternnte )

SHKI K. N. Mooni. Indiglz:;: 8 Toiletries Makers’ Association,

SHIU A. R. NAIUS~MHAN Indian ChemicalManufacturers’ Association, Calcutta; and Dhrangadhra Chemical Works Ltd,

SHRI P. 1). DESAI ( Ahnate ) Dhrangad hra

Indian Chemical Manufacturers' Association, Calcutta SWI JAI GOPAL JAIN (Allcrnalc)Dhrangadhra Chemical Works Ltd, Dhrangadhra

SHRI V. POD~ER Indian Paper Mills Association, Calcutta SHRI N. C. SEN GTJPTA ( Alfernatc )

REPRESENTATIVE DR K. SEBH~~~I

Tariff Commissioq, Bombiy Central Salt & Marine Chemicals Research Institute

SRRI D. R. BAXI ( AIfmotc) ( CSIR ), Bhavnagar

( Cimf~nued an pep 2 )

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

NEW DELHI 110002

IS: 711.1970

.4 Iembers Rekwntin,~

SIIRI H. I’. SIII:OPI Tata Chemicals Ltd, Bombay Stiar C. A. Josur ( Ahnalc)

SH~I A. SIII~XIZANTAN N.\IR Travancore-Cochin Chemicals Ltd, Udyogmandal ( Kerala )

SH I~I C. N. GOPINATHAS NMR ( Alternate )

Srrnr hf. S. TYA~I Indian Paper Makers’ Association, Calcutta SHliI S, K. VAKIL Saurashtra Chemicals, Porbandar

Snm B. R. W.~I.AVAI.Y.UI ( A~lcrnalc) SHRI D. DAS GUPTA, Director General, IS1 ( Ex-oj’icio Member )

Director ( Chrm )

Secretary

SHIU P. S. AROIL\

Assistant Director ( Chem ), IS1

Panel for Chlorine and Its Inorganic Products, CDC 25/P 2

Convener

Slll:I L. R,. GAITTAM D.C.M. Chemiral Works, New Delhi

Members

SHRI D. RAJAPPA ( ADernnre to Shri L. R. Gautam )

SHRI P. R. BAVDERAR Tata Chemicals Limited. Mithapur SHRI N. B. PATEL ( Alternate )

SFIHI A. K. BOSE Directorate General of Technical Development SRRI M. V. DES~I Atul Products Ltd, Atul

SI~RI B. V. SHAH ( Alternate ) SHRI L. R. KRIS~INAMURTHY The Mettur Chemical & Industrial Corporation Ltd!

Mettur Dam R. S. ( Salem Distt j SHRI M. PADNAN?\BAN ( Alternate )

Dn M. V. NIIURAR The Millowners’ Association, Bombay SHRI R. SUBR.ADlANYAM Kanoria Chemical St Industries Limited, Calcutta

IS:711-1970

Indian Standard SPECIFICATION FOR

FERRIC CHLORIDE, TECHNICAL

(First Revision)

0. FOREWORD

0.1 This Indian Standard (First Revision) was adopted by the Indian Standards Institution on 1 May 1970, after the draft finalized by the Alkalis and Chlorine Sectional Committee had been approved by the Chemical Division Council.

0.2 This standard was first published in 1955. The sampling scheme prescribed in the original standard has been modified in this revision.

0.3 Ferric chloride, technical, is produced generally in India by treating iron scraps with hydrochloric acid or chlorine. The material is obtained in the form of anhydrous powder, hydrated material as deliquescent crystal- line lumps, and liquid of varying concentrations.

0.4 Ferric chloride is used as a coagulant for sewage and industrial wastes, also in glycerine manufacture, in etching copper, in photo-engraving as a mordant, and to produce decorative surface effects on ceramics. It is also an oxidizing, chlorinating and condensing agent, a disinfectant, a pigment and a medicine.

0.5 This standard contains clause 4.1 which calls for agreement between the purchaser and the supplier.

0.6 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 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 ferric chloride, technical, chiefly used as coagulant in water purification, in the manufacture of glycerine, in etching glass plates and in photo-engravings.

*Rules for rounding off numerical values ( reuised ).

3

IS: 711- 1970

2. FORM

2.1 The material shall be in one of the following forms:

a) Anhydrous powder,

b) Hydrated, and

c) Liquid.

3. REQUIREMENTS

3.1 Description

3.1.1 Anh~dro~s Powder-The material of this form shall be greenish black, crystalline powder, extremely hygroscopic, becoming orange- coloured on hydration.

3.1.2 Hydrated-The material of this form shall be brownish yellow, deliquescent, crystalline lumps.

3.1.3 Liquid-The material of this form shall be a clear dark-brown, viscous liquid, free from sediments or suspended matter or other visible impurities.

3.2 The material shall also comply with the requirements given in Table 1, when tested according to the methods prescribed in Appendix A. Reference to the relevant clauses of Appendix A is given in co1 6 of the table.

4. PACKING AND MARKING

4.1 The material shall be packed in cont8inc:rs as agreed to between the purchaser and the supplier.

4.1.1 For anhydrous material, mild steel drums, for hydrated material, rubber and PVC lined drums, and for liquid material, carboys and stone jars, are recommended.

4.2 The containers shall be securely closed and marked with the name of the manufacturer; net weight and form of the material in the co.ntainer; recognized trade-mark; if any, and the year of manufacture.

4.3 BIS Certification Marking

The product may also be marked with Standard Mark.

4.3.1 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 may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards.

4

IS : 711- 1970

SL

No.

(1)

i)

ii)

iii)

iv)

v)

vi)

vii)

viii)

ix)

X)

xi)

xii)

TABLE 1 REQUIREMENTS FOR FERRIC CHLORIDE, TECHNICAL

(2) *Relative density at 25”/25”C,

Min

Ferric chloride ( as FeCl, ), percent by weight, MGz

Free acid ( HCl ), percent by weight, Max or

Basic1 ty ( as Fe,O, ), percent by weight, Max

Ferrous salts ( as FeCI, ), pcrcen t by weight, Max

Insoluble matter, percent by weight, Max

Free chlorine ( as Cl ), percent by weight, Max

Sulphates ( as SO, ), percent by weight, Max

Xtrates ( as NO, ), percent by weight, Max

Alkalis and alkaline earths ( ex- pressed as sulphates ), percent by weight, MUX

Copper as ( Cu ): percent by weight, MUX

Zinc ( as %n ), percent by weight, Max

Arsenic ( as AssO, ), percent by weight, Max

*Formerly ‘ specific concept, with water as Standardization ( IS0 ).

Liquid TO CL so. 1.x

.\l~I’l:sLlIs :\)

Anhydrous

(3)

-

98.0

-

--

0.10

0.50

0.01

0.30

0.05

0.3

0.015

0.01

o*ooo 5 ( 5 parts

per million )

Hydrated

(4)

-

59.0

0.03

0.03

0.10

0.20

0.01

0.30

0.05

0.3

0.015

0.01

(5) (6, 1.46 A-2

43.0

0.01

0.2

0.10

0.05

0.01

0.30

0.05

0.2

0015

0.01

A-3

A-4

A-4

A-5

A-6

A-7

A-U

A-9

A-10

A-11

A-11

0.000 3 0.000 2 ( 3 parts ( 2 parts

per per million ) million )

A-12

gravity ‘. ‘ Relative density ’ is the term adopted for this the refeTence substance, by the International Organization for

5. SAMPLING

5.1 The method of drawing representative samples of the material and the criteria for conformity shall be as prescribed in Appendix B.

5

IS : 711-1970

APPENDIX A

ANALYSIS OF FERRIC CHLORIDE, TECHNICAL

A-l. QUALITY OF REAGENTS

A-l.1 Unless specified otherwise, ‘ pure chemicals and distilled water (see IS : 1070-1960* ) shall be used in tests.

NOTE - ‘ Pure? chemicals ’ shall mean chemicals that do not contain impurities which affect the results of analysis.

A-2. DETERMINATION OF RELATIVE DENSITY

A-2.0 Outline of the Method-The sample is brought to the prescribed temperature and transferred to a hydrometer cylinder at approximately the same temperature. The appropriate hydrometer is lowered into the sample and allowed to settle. The hydrometer is read and the temperature of the sample noted.

A-2.1 Apparatus

A-2.1.1 Relatiae Density Hydromeler --of a suitable range. A relative density hydrometer calibrated at any temperature other than 25°C may also be used with appropriate correction (see Note under A-2.2.5).

A-2.1.2 I$drometer Cylinder- of clear glass or plastic, with a lip for convenience of pouring and having an inside diameter of at least 25 mm greater than the outside diameter of the hydrometer used. The height of the cylinder shall be such that the hydrometer floats in the sample with at least 25 mm clearance between the bottom of the hydrometer and the bottom of the cylinder.

A-2.1.3 Thermometer -of a suitable range and conforming to IS : 2480- 1964t.

A-2.1.4 Constant Temperature Batfl

A-2.2 Procedure

A-2.2.1 Adjust the temperature of the sample to 25°C and bring the hydrometer, cylinder and thermometer to approximately that temperature.

A-2.2.2 Pour the sample into the clean hydrometer cylinder without splashing in order to avoid the formation of bubbles and to reduce to a minimum the evaporation of the sample. Remove any air bubbles formed before inserting the hydrometer.

*Specification for water, distilled quality ( reuiscd ). $$ecification for general purpose glass thermometers.

6

IS : 711- 1970

A-2.2.3 Place the cylinder containing the sample in a constant tempe- rature bath to ensure that the temperature of the sample does not change during the test.

A-2.2.4 Lower the hydrometer gently into the sample and when it has settled, determine the temperature of the sample which is thoroughly but cautiously stirred with the thermometer, the whole of the mercury being immersed. Remove the thermometer and allow the hydrometer to resettle. Depress it about two scale divisions into the liquid and then release it. Keep the portion of the stem above the level of the liquid dry, since failure to do this changes the effective weight of the instrument and thus affects the accuracy of the reading. Allow sufficient time for the hydrometer to come to rest and for all air bubbles to come to the surface.

A-2.2.5 When the hydrometer has come to rest, floating away from the walls of the cylinder, and the temperature of the sample is constant, read the the hydrometer to the nearest 0*0005. The correct hydrometer reading is that point on the hydrometer seal e at which the surface of the liquid cuts the ‘scale. If a standardization certificate is provided, correct the hydrometer reading according to the data thereon. Report the value SO obtained, to the nearest O%Ol as the relative density at 25”/25”C.

NCWR - When a relative dtnsity hydrometer calibrated at a temperature other than 25°C is used, the correction for the hydrometer reading is calculated as follows:

where

A-= 0.00025 h (t-25)

X = correction factor,

A = relative density of liquid at t”C as indicated by the hydrometer, and

t = temperature at which the hydrometer is calibrated.

A-3. DETERMINATION OF FERRIC CHLORIDE

A-3.1 Reagents

A-3.1.1 Concentrated Hydrochloric Acid- conforming to IS : 265- 1962*.

A-3.1.2 Potassium Iodide - iodate-free.

A-3.1.3 Standard Sodium Thiosulphate Solution - 0.1 N.

A-3.1.4 Starch Solution-Triturate 5 g of pure starch and 0.01 g of mercuric iodide with 30 ml of water in a mortar. Pour the resulting paste into one litre of boiling water, boil for 3 minutes, allow the solution to cool and decant off the clear liquid.

*Specification for hydrochloric acid ( reoisad ).

7

IS :711-1970

A-3.2 Prepared Sample Solution- Weigh accurately about 10 g of the material and dissolve in 100 ml of 2 percent (zej/u) hydrochloric acid. If there is any insoluble matter, filter through a. sintered glass crucible or a Gooch crucible. Wash four times with 2 percent (W/U) hydrochloric acid and then with cold ~zater. blake up the volume of the filterate to 250 ml.

A-3.3 Procedure-Transfer 23 ml of the fiIepared sample solution into a 300-ml glass-stoppcred flask and dilute to 50 ml. Add 3 ml of concen- trated hydrochloric acid, 3 g of potassium iodide, a little solid cuprous iodide and allow to stand for 30 minutes. Then dilute with 100 ml of water and titrate with standard sodium thiosulphato solution using starch solution towards the end.

A-3.3.1 Carry out a blank test with all the reagents but without the material to be tested.

A-3.4 Calculation

Ferric chloride (as FeCl,), percent by weight= 162.22 ( Vi-VV,)N

W where

F, = volume in ml of standard sodium thiosulphate solution used in the test with the material,

V, = volume in ml of standard sodium thiosulphate solution used in the blank,

N -= normality of standard sodium thiosulphate solution, and

W = weight in g of the material taken under A-3.2.

A-4. DETERMINATION OF FREE ACIDITY OR BASTICITY

A-4.1 Reagents

A-4.1.1 Phenolphthalein Indicator -Dissolve 0.5 g of phenolphthalein in 100 ml of rectified spirit (conforming to IS:323-1952* ), 95 percent by volume, that has been previously neutralized to the indicator.

AAl. Standard Potassium Hydroxide Solution - O-5 N and O-2 N.

A-4.1.3 Standard Hydrochloric Acids -0.5 N and Q2 N.

A-4.1.4 Potassium Fluoride Solution -Dissolve 100 g of potassium fluoride in 120 ml of hot water, freshly distilled. Add 1 ml of phenolphthalein indicator and neutralize with standard hydrochloric acid (0,5 Iv) or standard potassium hydroxide solution (0.5 N), as the case may be. (One millilitre of potassium fluoride solution in 10 ml of freshly distilled water shall give a faint pink colour. ) Filter the solution, if necessary, and then dilute to 200 ml with freshly distilled water.

*Specification for rectified spirit ( revised ).

8

IS : 711- 1970

A-4.2 Procedure - Piprtte o1.11 4-O ml of standard hydrochloric acid (0*2N ) illto a 100-ml volumetric flask. Add to the flask about 10 g of the material, accurately weighed, and shake well to dissolve. Make up the volume to the mark. Pipette out 25 ml of this solution in a 250-ml conical flask. Add 50 ml of potascium fluoritlc sohition and 0.5 ml of phenolphthalein indicator, and cool the contents to 15°C. Titrate the solution with standard JlOtaSSiUm hydroxide solution (0.2 N) for one minute is obtained.

until a delicate pink colour persisting

A-4.2.1 Carry out a blank test using IO ml of standard hydrochloric acid and other reagents.

A-4.3 Calculation

Free acidity (as TIC1 ), percent by weight= 14.60 (A-B) J\r

IV

A -- volume in ml of stantlarrl notassium hydroxide solution used in the test with the material,

B -5 volume in ml of stantlard potassium hydroxide solution used in the blank,

.N = normality of standard potassium hydroxide solution, and

CV = weight in g of the material taken for the test.

A-4.3.1 In case A is less than B, therr is no free acid and the sample is basic. In such cases, calculate the I)asicity as under:

IO.646 ( B - A ).Af Rasicity (as Fe, o,), percent tJy weight .= -

w

A-5. DETERMINATION OF FERR’OUS SALTS (As FeCI,)

A-5.1 Rea$pnts

A-5.1.1 Concentrated Hydrochloric Acid-conforming to IS:265- I962*,

A-5.1.2 Potassium Ferricyanide Solutio?r - 5 percent (w/v), freshly prepared.

A-5.2 Procedure-Weigh accurately 0.5 g of the material and dissolve in water and make up the volume with water to 500 ml. Transfer 25 ml of this solution, add 1 ml of hydrochloric acid and one drop of potassium ferricyanide solution.

A-5.2.1 The limits prescribed in Table 1 shall be taken as not having been exceeded if no blue colour is produced.

*Specification for hydrochloric acid (revised).

9

IS:?ll-1970

A-6. DETERMINATION OF INSOLUBLE MATTER

A-6.1 Reagents

A-6.1.1 Dilufp f@drorhloir Acid- approximately 2 percent (v/l!).

A-6.2 Procedure--Weigh accurately about 20 g of the material and dissol\-c in 100 ml of dilute hydrochloric acid. Filter through a tared sintered glass crucible (G No. 4). Wash twice with cold dilute hydro- chloric acid and then thrice with water. Dry the crucible with its contents to constant weight at 105” to 110°C.

A-6.3 Calculation

Insoluble matter, percent by weight = 100 x $ 2

where

11/l - weight in g of the residue, and

11,‘s = weight in g of the material taken for the test.

A-7. TEST FOR FREE CHLORINE

A-7.1 Reagents

A-7.1.1 Starch Iodide Paper- Impregnate ordinary filter paper with muci- lage of starch, diluted with an equal volume of 0.4 percent ( w/u) solution of potassium iodide in water.

A-7.2 Procedure-Dissolve 0.5 g of the material in 10 ml of water in a conical flask. Boil the solution and place a moist starch iodide paper on the mouth of the flask.

A-7.2.1 Thcl limits prescribed in Table 1 shall be taken as not having been exceeded if no blue colour is produced on the starch paper.

A-8. DETERMINATION OF SULPHATES

A-8.1 Reagents

A-8.1.1 Dilute Hydrochloric Acid -approximately 10 percent (w/v).

A-8.1.2 Barium Chloride Solution - approximately 10 percent (w/v).

A-8.2 Procedure-Weigh accurately about 5 g of the material and add 100 ml of dilute hydrochloric acid. Filter, if necessary, and wash the filter paper thoroughly. Heat the solution to boiling and add drop by drop 10 ml of hot barium chloride solution. Boil the solution for 15 minutes and then allow to stand for 4 hours. Filter through a tared Gooch or a sintered glass crucible ( G No. 4). Wash the precipitate first with hot dilute hydrochloric acid and then with hot water till it is free from chlorides and dry to constant weight at 105” to 110°C.

10

IS : 711- 1970

A-8.3 Calculation

Sulphates (as SO.,), percent by weight=41*15 x $

\\vhere

A = weight of barium sulphate, and

W = weight of the material taken for the test.

A-9. TEST FOR NITRATES

A-9.1 Reagents

A-9.1.1 Dilute Sulphuric A&f-approximately 5 N.

A-9.1.2 Concentrated Hydrochloric Acid-conforming to IS : 265-1962*.

A-9.1.3 Standard Potassium Nitrate Solution - O*OO 1 molar.

A-9.1.4 Concentrated Sulphuric Acid- conforming to IS : 266-1961t.

A-9.1.5 Standard Indigo Carmine Solution-Dissolve 0.20 g of indigo carmine in 400 ml of dilute sulphuric acid, add 20 ml of concentrated hydrochloric acid and sufficient dilute sulphuric acid to produce 1000 ml. Standardize the solution so that 10 ml added to 3.3 ml of potassium’nitrate solution is just decolourized on adding 13 ml of concentrated sulphuric acid and heating to boiling. One millilitre of this solution is equivalent to 0.02 mg of nitrate (as NO, ).

A-9.1.6 Dilute Ammonium Hydroxide Solution -approximately 5 N.

A-9.2 Procedure -Weigh accurately 0.4 g of the material and dissolve in 100 ml of water. Add 50 ml of dilute ammonium hydroxide solution and filter by suction, To 15 ml of the filtrate, add 5 ml of dilute sulphuric acid, 1 ml of standard indigo carmine solution and 20 ml of concentrated sulphuric acid and heat to boiling.

A-9.2.1 The limits prescribed in Table 1 shall be taken as not having been exceeded if the blue colour produced does not entirely disappear.

A-10. DETERMINATION OF ALKALIS AND ALKALINE EARTHS

A-10.1 Reagents

A-10.1.1 Concentrated Hydrochloric Acid- conforming to IS : 265-1962*.

A-10.1.2 Hydrogen Peroxide -approximately 20 volumes. _________~ -.

*Specification for hydrochloric acid ( revised ). +Specification for sulphuric acid ( revised ),

11

.ts: 711- 1970

A-10.1.3

A-10.1.4

A-10.1.5

A-10.1.6

(w/u)*

A-10.1.7

Ether

Dilute Hydrochloric Acid- approximately 2 N.

Potassium Permanganate Solution -approximately 0.1 N.

Ammonium Thiocyanate Solution -approximately 10 percent

E.wtraction Mixture-a mixture of equal volumes of amyl alcohol and amyl acetate.

A-10.1.8 Sul~huric Acid- conforming to IS : 266-1961*.

A-10.2 Procedure

A-10.2.1 Weigh accurately about 10 g of the material and treat it with 10 ml of water. Add 17 ml of concentrated hydrochloric acid and two drops of hydrogen peroxide. Shake the solution with four successive 20-ml portions of ether in a separating funnel. Evaporate the acid solution, which will be almost colourless, to dryness. Dissolve the residue in 2 ml of concentrated hydrochloric acid and 10 ml of water. Filter, if necessary, and dilute with water to 100 ml.

A-10.2.2 Evaporate a 35-ml aliquot to about 10 ml. Add 1 ml of dilute hydrochloric acid and one drop of potassium permanganate solution and mix well. Add 5 ml of ammonium thiocyanate solution and extract with two IO-ml portions of extraction mixture. Separate the aqueous layer and evaporate to dryness preferably in platinum crucible of 30 ml capacity. Moisten with concentrated sulphuric acid. Ignite and weigh the residue to constant weight.

A-10.3 Calculation

Alkalis and alkaline earths ( expressed as. sulphates) =

10 000 A 35 w

where.

A=weight of the residue, and

W=weight of the material taken for the test.

A-11. TEST FOR COPPER AND ZINC

A-11.1 Apparatus

A-11.1.1 .Neder Cylinders -50 ml capacity.

*Specification for sulphuric acid (retied).

12

IS: 71X- 1970

A-11.2 Reagents

A-11.2.1 Citric Acid- solid.

A-11.2.2 Dilute Ammonium Hydroxide Solution - approximately 5 N.

A-11.2.3 Sodium Diethyl Dithiocarbamate Solution-Dissolve 0.1 g of the salt [ ( CsH,), NCS, Na] in 100 ml of water.

A-11.2.4 Carbon ‘Tetrachloride

A-11.2.5 Anhydrous Sodium Sulphab

A-11.2.6 Standard Copper Solution - Dissolve O-392 8 g of copper sulphate ( CuSO,, 5H,O) in 250 ml of copper-free water. Pipette out 25 ml of this solution and make up the volume to 100 ml. One millilitre of the resulting solution is equivalent to 0.1 mg of copper ( Cu ).

A-11.2.1 Resorcino.!

A-11.2.8 Thymol Blue Indicator- Warm 0.1 g of thymol blue with 4.3 g of 0.05 N sodium hydroxide solution and 5 ml of rectified spirit until dissolved. Dilute with ethyl alcohol, 20 percent by volume.

A-l 1.2.9 Chloroform

A-11.2.10 Dithizone Solution -Dissolve 0.1 g of diphenyl thiocarbazone ( C,H,NH NH CS N : NC,H,) in 100 ml of chloroform.

A-11.2.11 Standard Ilydrochloric Arid- 1 N.

A-11.2.12 Ammonium Chloride - solid.

A-11.2.13 Potarsium Ferroqanide Solution -approximately 1 percent freshly prepared solution in water.

A-11.2.14 Standard zinc Solution -Dissolve 1.000 g of ziuc in slight excess of hydrochloric acid and dilute with water to make up the volume to 1000 ml. Dilute 10 ml of this solution to 100 ml. One millilitre of this solution is equivalent to O-1 mg of zinc.

A-11.3 Prepared Sample Solution -Treat 10 g of the material with 10 ml ot‘water. Add 17 ml of concentrated hydrochloric acid and 2 drops of hydr ogen peroxide ( 20 volumes). Shake the resulting solution with four successive 20-ml portions of ether. Evaporate the acid solution to dryness. Dissolve the residue in 2 ml of dilute hydrochloric acid and 10 ml of water and filter if necessary. Dilute with water and make up the volume to 100 ml.

13

IS: 711-1970

A-11.4 Procedure for Copper- Transfer 20 ml of the prepared sample solution (A-11.3) in a separating funnel, and add 1 g of citric acid, 5 ml of dilute ammonium hydroxide solution and 1 ml of sodium diethyl dithio- carbamate solution. Shake this solution with three successive portions, 5 ml, 3 ml, and 2 ml, of carbon tetrachloride. Mix the carbon tetrachloride extracts and dry with a little anhydrous sodium sulphate. Transfer the dried carbon tetrachloride extract as completely as possible to a Nessler cylinder and dilute with dried carbon tetrachloride to 50 ml. Carry out a control test by treating 15 ml of water and 3 ml of standard copper solution in the same tiqnner.

A-11.4.1 The limits prescribed in Table 1, shall be taken as not having been exceeded if the colour produced in the test with the material is not deeper than that produced in the control test.

A-11.5 Procedure for Zinc-Transfer 10 ml of the prepared sample solution (A-11.3) and add 1 g of citric acid, 0.1 g of resorcinol and adjust the pH of the solution to approximately 9.0 using dilute ammonium hydroxide solution and thymol blue indicator. Shake vigorously with three successive 5-ml portions of dithizone solution. Mix the chloroform extracts, wash with 5 ml of water and then shake with 10 ml of standard hydrochloric acid. Separate and wash the acid with 5 ml of chloroform. Transfer to a Nessler cylinder, add 1 g of ammo&urn chloride and dilute with water to about 45 ml. Make up the volume with water to 50 ml and add 1 ml of potassium ferrocyanide solution. Carry out a control test in the other Nessler cylinder using 1 ml of standard zinc solution in place of the prepared sample solution and the same quantities of other reagents in the same total volume of the reaction mixture. Compare the turbidities after 15 minutes.

A-11.5.1 The limits prescribed in Table 1 shall be taken as not having been exceeded if the turbidity produced in the test with the material is not greater than that produced in the control test.

A-12. TEST FOR ARSENIC A-12.1 Procedure- Dissolve 1.000 g of the material in 10 ml of water and carry out test for arsenic as prescribed in IS: 2088-1962* using following amounts of arsenic trioxide ( As, 0,) for preparing the comparison stain:

Form of Material Arstnir Trioxide

mg Anhydrous 0.005

Hydrated 0.003

Liquid 0.002

*Modified Gutzcit method of trst for arsenic.

14

IS:711 - 1970

APPENDIX B ( Clause 5.1 )

SAMPLING AND CRITERIA FOR CONFORMITY OF FERRIC CHLORIDE, TECHNICAL

B-l. GENERAL

B-1.0 In drawing samples the following precautions and directions shall be observed.

B-l.1 Precautions shall be taken to protect the samples, the sampling imple- ments and the container for samples from contamination. If the material is in anhydrous form, the sampling shall be carried out with minimum amount of exposure to atmosphere.

B-l.2 The sampled material shall be placed in suitable, dry, clean container.

B-l.3 Each sample container shall be sealed air-tight after filling and marked with full details of sampling.

B-l.4 Samples shall be taken from different parts of the containers using suitable sampling implements in order that the collected material is truly representative of the container.

B-2. SCALE OF SAMPLING

B-2.0 All the containers in a consignment of ferric chloride of the same type and from a single batch of manufacture shall constitute a lot.

B-2.1 Samples shall be tested for each lot for ascertaining conformity of the material to the requirements of the specification.

B-2.2 The number ( n ) of containers to be selected from the lot shall depend upon the size of the lot (Jv) and shall be in accordance with co1 1 and 2 of Table 2.

TABLE 2 NUMBER OF CONTAINERS TO BE SELECTED FROM A LOT

LOT .%ZE

Jv

(1)

Up to 25

26 ,, 50

51 I, 100

101 and above

NUMBEROFCONTAINERS

TOBESELECTED IN

TIZR SAMPLE

"

V!

3

4

5

7

15

IS : 711- 1970

B-2.3 These containers shall bc sclectcd at random from the lot. For random selection procedures, guidance may I)e had from IS: 4905-1968*.

B-3. NUMBER OF TESTS

B-3.1 From each of the selected containers about 200 g of ferric chloride shall 1~ withdrawn with the help of a sampling implement. Out of the portions so collected equal quantity of the material shall be taken out and mixed together to form composite sample weighing about 300 g. The remaining portions corresponding to each of the selected containers shall be transferred to separate sample bottles and these sample bottles containing ferric chloride shall be termed individual samples.

B-3.2 Tests for ferric chloride content and relative density (in the case of liquid ) shall be conducted on individual samples. Tests for all other characteristics shall be made on the composite sample.

B-4. CRITERIA FOR CONFORMITY OF LOT

B-4.1 Ferric Chloride Content and Relative Density-From the individual test results, the mean (a) and range (R) of the values shall be calculated for each of the two characteristics (range being defined as the difference between the maximum and minimum values). The values of the expression ( x-- 0*6R) shall be greater than or equal to the correspond- ing value given in Table 1 if the lot is to be accepted under this clause.

B-4.2 For Other Characteristics-The test results for all other characterisiics tested on the composite sample shall satisfy the relevant requirements for the acceptance of the lot.

‘Methods of random aampliog.

16

BUREAU OF INDIAN STANDARDS

Headquarters Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 Telephones: 323 0131,323 3375,323 9402 Fax : 91 11 3234062, 91 11 3239399, 91 11 3239382

Telegrams : Manaksanstha

Central Laboratory : (Common to ail Offices)

Telephone

8-77 00 32 Plot No. 20/9, Site IV, Sahibabad Industrial Area, Sahibabad 201010

Regional Offices:

Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 323 76 17

*E&tern : l/14 CIT Scheme VII M, V.I.P. Road, Maniktola, CALCUlTA 700054 337 66 62

Northern : SC0 335-336, Sector 34-A, CHANDIGARH 160022 60 36 43

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

twestern : Manakalaya, E9, Behind Mar01 Telephone Exchange, Andheri (East), 632 92 95 MUMBAI 400093

Branch Officea::

‘Pushpak’, Nurmohamed Shaikh Marg, Khanpur, AHMEDABAD 360001 550 13 46

SPeenya Industrial Area, 1 st Stage, Bangalore-Tumkur Road, BANGALORE 560056

039 49 55

Gangotri Complex, 5th Floor, Bhadbhada Road, T.T. Nagar, BHOPAL 462003 55 40 21

Plot No. 62-63, Unit VI, Ganga Nagar, BHUBANESHWAR 751001 40 36 27

Kaiaikathir Buildings, 670 Avinashi Road, COIMBATORE 641037 21 01 41

Plot No. 43, Sector 16 A, Mathura Road, FARIDABAD 121001 6-26 66 01

S&ri Complex, 116 G.T. Road, GHAZIABAD 201001 0-71 1996

5315 Ward No.29, R.G. Barua Road, 5th By-lane, GUWAHATI 761003 541137

5-8-56C, L.N. Gupta Marg, Narnpally Station Road, HYDERABAD 500001 201063

E-52, Chitaranjan Marg, C- Scheme, JAIPUR 302001 37 29 25

1171416 B, Sarvodaya Nagar, KANPUR 208005 21 66 76

Seth Bhawan, 2nd Floor, Behind Leela Cinema, Naval ffishore Road, 2389 23 LUCKNOW 226001

NIT Building, Second Floor, Gokulpat Market, NAGPUR 440010 52 51 71

Patliputra Industrial Estate, PATNA 800013 262305

Institution of Engineers (India) Building 1332 Shivaji Nagar, PUNE 411005 32 36 35

T.C. No. 14/l 421, lhiwdty P. 0. Palayam, THIRW- 695034 621 17

*Sales Otke is at 5 Chowriie Approach, P.O. Princep Slreet, CALCLlTTA 700072

271065

tSti Office is at Novefty Chambers, Grant Road, MUMBAI 400007

*Sales Offkze is at ‘F’ Block, ‘Unity Building, Nareuhimaraja Square, BANGALORE 560002

309 65 28

222 39 71

Reprography Unit, BIS, New Dedhi, India