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 1050 (1984): Lime Sulphur Solution [FAD 1: Pesticidesand Pesticides Residue Analysis]

9

IS t 10% - 1984

Indian Standard SPECIFICATION FOR

LIME SULPHUR SOLUTION

( First Revision )

Pest Control Sectional Committee, AFCDC 6

Chairman

DR K. D. PAHARIA

Representing

Directorate of Plant Protection, Quarantine & Storage ( Ministry of Agriculture ), Paridabad

Members

DR P. K. AQQARWAL IDMA Laboratories, Chandigarh DR S. R. IYBNQAR ( Alternate )

DR H. L. BAMI Pesticides Residue Analysis Sectional Committee, ( AFDC 56 ), IS1

DR B. BANERJEE Tea Research Association, Jorhat DR G. SATYANARAYANA ( Alternate I ) SHRI S. C. DAS ( AZfcrnatc II )

SHRI N. S. BIRDIE Shriram Test H&se, Delhi S-1 R. K. BANERJEE ( Alternate )

Cmap &ANT PROTBCTION OFFICER Department of Agriculture, Government of Maharashtra, Bombay

CI.IBMIST INCHARGE, INSECTICIDES TXWIN~ LABORATORY ( Alternate )

DR M. S. DHAW National Malaria Eradication Programme, Delhi SHRI V. DORAIRAI Plastic Containers Sectional Committee ( MCPD

11 ), ISI SHRI 0. D. GOKHALB Bombay Chemicah Private Limited Bombay

SHRI V. V. KBTKAR ( Alteraate ) SHIU N. L. KALRA NatigetiInstitute of Communicable Diseases,

Sm G. C. JOSHI ( Afternate ) DR R. L. KALRA Pdab Agricultural University, Ludhiana

DR R. P. CMWU ( Alternate ) DR KALYAN SINQE Chander Shekhar Azad University of Agriculture

& Technology, Kanpur DR S. K. KAWYAP National Institute of Occupational Health

( ICMR ), Ahmadabad DR S. K. GUPTA ( Afternate )

( Continued on page 2 )

@ Copyright 1984

INDIAN STANDARDS INSTITUTION 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 &a11 be deemed to be an infringement of copyright under the said Act.

( Continuedfiom page 1 )

Members Represen eing

SHRI S. G. KRISHNAN Nqt’ nal Qqapic Chemical Industries Limited, Bombay

DR J. S. VERMA ( rilferm(e ) SHRI J. K. KHOSLA lviet~~ $rt;iners Sectional Committee ( MCPD

SHRI A. N. BHAT~ACHARYYA ( Alternate i DR S. LAKSHMANAN Pqper and B exible Packaging Sectional Com-

mittee ( nb CPD 14 ), ISI DR J. C. MAJUMDAR BASt- India Limited, Bombay

Dg R. P. CETAN~~BASEI(HA~ ( dlkw&e ) SHRI S. K. MAJUMDAR Central Food Technological Research Institute

( CSIR ), Mysore SHRI M. Muthu ( AIterrrate )

SHRI K. S. MEHT’A Bharat Pulverising Mills Private Limited, Bombay SHRI S. CHAITERJEE ( Akmate )

Agromore Limited, Bangalore

Pesticides Formulators Association of India ( S.S.I. 1. Bombav . _- ‘* DR S. R. BARQOAU ( &ernclte )

DR S. K. MUKHJ&UEE” Agricultural Chemicals Division, I dian A jcul- tural Research Institute ( ICA 2 *+ 1, Nqv

DR N. K. ROY ( AIterJtate ) ,J&b.j

SHRI K. R AJEND~A~ N+!R Central Iqpcticides Gel!, Directorate of_ Plant ProtectIon, Quarantme & Storage ( $4qstry of Agriculture ), Faridabad

DR R. C. GUPTA ( ~&?fute J ) SHRI S. K. GHOSH ( Afterndte r’1)

@RI p. V.-bj~R~y~Nbti SHRI K. B: &JPTA < &p?p 1

sWi;m !sstitpte c$ Pqlwpp, Bpnbp~

DR V. N. NIGAM SHRI M. M. PADALIA

Ministry of Dtfenqe ( DGI ) Department qf A ‘ iculture, Gpvern+xtt of

Gt$$t Ahmac&&d ., ./ * SHRI R. G. J.+rWJA ( 44

SHRI A. R. PANIC%R’ WwCr ).

DR S. N. DE%% Hin&s#n Insecticides Limited, New Delhi

SHRI Y. A. PRADHAN t&3 ( AWWtr )

SHRI M. L. S#+u ( A!WW ) Rallis India Limited, Rombay

DR R. L. RAJAK Cengal Insecticide Laboratory, Directorate of Plant Protectipqn, Quarantine & S&rage

SHRI V. C. BHARGAVA ( Alternate I ) ( Mini$ry of Agrrcuhure ), Fa&Iabgd

DEPUTY DIRECTOR ( P4 & QC ) ( &rnate II ) ._%,..._ REPRESENTATIVE !?3$ $m@rt of Agriculture, Government of

DR K. D. SHARMA Apdhra radesh, Hyderabad

D’ tqa e eueral of Technical Development, ’ %ew D$hl

SHRI S. C. BAJAJ ( Alternate ) _~. DR K. $9. SHR~WTA~A ’ Pesticides Association of India, New Delhi

Da J. C. MAJUMDAR ( Alternate )

( continued on puge 11 )

c

Indian Standard SPECIFICATIOti FOR

LIME SULPHUR SOLUTION

O.F’CIREWORD

0;f This k&b SMi&rd ( First Revision ) was adopted by the Indian Star&ids Institution on 29 June 1984, after the draft finalized by the Pest Control Seciional Committee had been approved by the Agricultural and Food Products Division Council and the Chemical Division Council.

0.2 Lime sulphur solution is a complex mixture of calcium fpolysulphides and thiosulphate and is produced by boiling a suspension of calcium hydroxide and sulphur. It is largely used ab a fungicide and to a certain extent also as an insecticide against pests of agriculture rind animal husbiilidry.

0.3 Tliis standard was first pliblishkd in 1957. Subsequenti$ tin axhendment was issued. It is being revised to update its requirements.

0.4 In the preparation of this standard, due f

onsideration has been given to the Insecticides Act, 1968 and Rule; raked tliereunder. However, this staodard is subject to the restrictions imposed under these, wherever applicable.

6.4 I& tki $$o& of dkidk$ tihkther a Ijartik&r requirement of this stindaid iS coriipli’ed with, the f&l Glue, observed or calculzlted expressing the result of a test or analysis, shall, be rounded off in accordance with IS : 2-1960*. The numbed- bf sigtlificant places retained in the rounded off value should be the same as that of the specified value in this’ standard.

1. SCOPE

l& TJlis staudakd @.e+skribes the -requirements &cl g@fho& of sampling and test for lime sulphur solution. I

*&pleS fat rg&didg off fiunietkal tilu@ ( rcVis@ti j.,

3

IS : 1050 - 1984

2. REQUIREMENTS

2.1 Description - The material shall ‘be a clear, deep yellow to deep orange red liquid, free from any extraneous impurities, scum, suspended matter, sludge and sediment.

2.2 Chemical - given in Table 1.

The material shall also comply with the requirements

TABLE 1 REQUIREMENTS FOR LIME SULPHUR SOLUTION ( Clauses 2.2 and 5.1 )

%. ckL4RACTERISTIC REQUIREMENT METHOD OF TEST, RBF TO

_----h- Appendix of Cl GF This standard IS : 6940-

1982* (1) (2) (3) (4) (5) i) Total sulphur content, percent 22.0 A

( m/v ), Min ii) Polysulphide sulphur content, 22.0 B

percent ( m/v ), Min iii) Thiosulphate sulphur content, 2’0 C -

percent ( m/v ), Max, iv) Sulphate sulphur content, percent 0.5 D -

( mlv ), Max v) Relative density at 27°C 1’26&0’01 - 5

*Methods of test for pesticides and their formulations (first revision ).

3. PACKING AND MARKING

3.1 Packing - The material shall be packed as per requirements given in IS : 8190 ( Part 2 > - 1980*.

3.2 Marking - The containers shall bear legibly and indelibly the following information, in addition to any other information required under Insecticide,y Act and Rules.

a) Name of the material; b) Name of the manufacturer; c) Date of manufacture; d) Batch number; e) Net mass of contents; f) Polysulphide sulphur content, percent ( m/v ); and g) Tt; $A&mum cautionary notice worded as in Insecticides ~~~

*Requirements for packing of pesticides : hrt 2 Liquid pesticides (first revision ).

4

Is : 1050 - 1984

3.2.1 The containers may also be marked with the IS1 Certification Mark.

NOTE - The use of the HI Certification Mark is governed by the provisions of the Indian Standards Institution ( Certification Marks ) Act and the Rules and Regula- tions made there under. 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 d:vised and supervised by IS1 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 Iicence for the use of the IS1 Certification Mark m+y 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 according to the method prescribed in IS : 10627-1983*.

5. TESTS

5.1 Tests shall be carried out by appropriate methods referred to in co1 4 and 5 of Table 1.

5.2 Quality of Reagents - Unless specified otherwise, pure chemicals and distilled water ( see IS : 1070-19773 ) shall be employed in tests.

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

APPENDIX A

1 Table 1, Item (i) ]

DETERMINATION OF TOTAL SULPHUR CONTENT

A-l. REAGENTS

A-l.1 Sodium Peroxide - solid.

A-l.2 Dilute Hydrochloric Acid - 1:4 (v/v).

A-l.3 Concentrated Hydrochloric Acid - r.d. 1’16.

A-l.4 Barium Cbloride Solution - 10 percent (m/v).

*Methods for sampling of pesticidal formulations. tSpecificatiou for water for general laboratory us ( sfccn$ r@$qq ),

5

Is : 1050 - 1984

A-2. PROCEDURE

A-2.1 Preparation of Sohtioa - Place the bottle containing the sample of the material in a thermostat maintained at 27’0” & 0’5°C. Pipette 10 ml of the material brought to 27’O”Cf 0’5°C into a 250 ml volumetric flask using a clean and dry pipette calibrated at 27°C and immediately make up the volume to mark with water. MIX this solution thoroughly. Take three or four bottles of convenient sizes and fill them completely with the solution, avoiding the contact of the solution with air as far as possible. Stopper the bottles, seal with paraffin and preserve them in a cool dark place.

A-2.2 Take 50 ml of cold water in a 250 ml beaker and dissolve in it 2 to 3 g of sodium peroxide. Open a bottle contaiuing the prepared solution ( see A-2.1 > and pipette* 10 ml of the prepared solution into the beaker containing sodium peroxide solution. While transferring the prepared solution, keep the tip of the pipette just under the surface of the liquid in the bearker and then raise the pipette to drain it. Cover the beaker with a watch glass and heat it on a steam bath occasionally stirring the contents of the beaker with a glass rod, until all the sulphur is oxidized to sulphate. ( The complete oxidation of sulphur to sulphate is indicated by the disappearance of the yellow colour. ) Wash the watch glass and the sides of the beaker with water into the beaker itself. Acidify the contents of the beaker with dilute hydrochloric acid and evaporate to complete dryness on a steam bath. Treat the residue with a small quantity of water acidified with hydrochloric acid, boil the filter to remove any stlica ( Si(& ) that may be present. Wash the beaker and the filter three or four times with small portions of water acidified with hydrochloric acid. Collect the filtrate and the washings in a one litre beaker. Dilute the filtrate to 300 ml with water, add 50 ml of concentrated hydrochloric acid and heat just to boiling. Add to the contents of the beaker the necessary quantity of barium chloride solution ( see Note 1 ) from a burette at such a rate that approximately 4 minutes are required to run in the necessary quantity ( see Note 2 ). Stir the contents of the beaker with a glass rod during the addition of barium chloride solution. Evaporate the contents of the beaker to dryness on a steam bath. Add hot water to the dry mass in the beaker and stir to make a suspension. Filter the contents of the beaker through a quantitative filter paper ( Whatman No. 42 ) or equivalent. Wash the last traces of the precipitate from the beaker on to the filter paper usmg water. Wash the filter with water until the washings are free from chlorides. Dry the precipitate for half an hour by placing the filter paper in an air oven. Transfer-the filter paper along with the precipitate to a tared

*A clean dry prpette shall be used.

6

porcelain crucible, carefully ignite to constant mass over a Bunsen burner. Cool the crucible with the contents in a desiccator and weigh.

NOTE l- The volume of barium chloride solution to be added is calculated.at the rate of 11 ml per gram of barium sulphite expected to be precipitate f&b the solution contained in the beaker.

NOTE 2 - The rate of addition of barium chloride solution may be regulated by attaching a capillary tube to the lower end of the burette.

A -3. CALCULATiON

A-3.1 Total sulphur content of the material, percent ( m/v ) = 34’34 m

where m = mass, in g, of barium sulphde.

APPENDIX B

[ Table 1, Item ( ii ) 1

DETERMINATION OF POLYSULPHIDE SULPHUR CONTENT

B-l. REAGENTS

B-l.1 Ammoniacal Zinc Chloride Solution - Dissolve 50 g of anhydrouj zinc chloride ( ZnCLa ) in about 500 ml of water, add 125 ml of ammonitim hydroxide solution ( r.d. 0’90 ) and 50 g of ammonium chloride and dilute to 1 000 ml.

B-1.2 Sodium Peroxide - solid.

B-l.3 Dilute Hydrochloric Acid - I:4 ( V/V ).

B-l.4 Concentrated Hydrochloric Acid - r.d. 1’16.

B-l.5 Barium Chloride Solution - 10 percent ( m/v ).

B-2. PROCEDURE

B-2.1 Take 10 to 15 ml of water in a small beaker. Open a fresh bottle containing the prepared solution ( see A-2.1 ) and prepared solution into the beaker containing water. V

j .ette* 1.0. 1p1 of the

prepared solufion, keep t tiilird irarisfeltiri’g the

liquid m the beaker and t ‘en raise the pihette to drain it. % e tip of the pipette just under the ii “t;f$?*ZQ

contents of the beaker a slight excess of ammoniacal zinc chloride s&&ii

*A dry and clean pipette shall pe used,

7

IS t 1050 - 1984

over the quantity required to precipitate all the sulphur present in the prepared solution taken for the determination. Stir the mixture contained in the beaker thoroughly with a glass rod and filter. Wash the beaker twice with cold water and transfer the washings along with any precipitate of sulphur remaining in the beaker on to the filter paper. Wash the filter paper twice with cold water. Transfer the filter paper along with the precipitate of sulphur to the same beaker. Add water sufficient to cover the filter paper and the precipitate, stir and disintegrate the filter paper with a glass rod. Add to the contents of the beaker about 3 g of sodium peroxide. Cover the beaker with a watch glass and heat it on a steam bath occassionally stirring the contents of the beaker with a glass rod, until all the sulphur is oxidized to sulphate. If the quantity of sodium peroxide is found insufficient, add more of it to complete the oxidation of sulphur. Wash the watch glass and the sides of the beaker with water into the beaker itself. Add dilute hydrochloric actd to make the contents of the beaker siightly acidic and filter to remove the shreds of filter paper. Wash the beaker and the filter three or four times with small portions of hot water. in a one litre beaker.

Collect the filtrate and the washings Dilute the filtrate to 300 ml with water, and 50 ml

of concentrated hydrochloric acid and heat just to boiling. Add to the contents of the beaker the necessary quantity of barium chloride solution ( see Note 1 ) from a burette at such a rate that approximately 4 minutes are required to run in the necessary quantity (see Note 2 ). Stir the contents of the beaker with a glass rod during the addition of barium chloride solution. Evaporate the contents of the beaker to dryness on a steam bath. Add hot water to the dry mass in the beaker and stir to make a suspension. Filter the contents of the beaker through a quantitative filter paper ( Whatman No. 42 or equivalent ). Wash the last trace of the precipitate from the beaker on to the filter paper <using water. Wash the filter with water until the washings are free from chlorides. Dry the precipitate for half an hour by placing the filter in an air oven. Transfer the filter paper along with the precipitate to a tared porcelain crucible, carefully ignite and heat to constant olass over a Bunsen burner. Cool the crucible with the contents in a desiccator and weigh.

NOTE 1 - The volume of barium chloride solution to be added is calculated at the rate of 11 ml per gram of barium sulphate expected to be precipitated from the solution contained in the beaker.

NOTES- The rate of addition of barium chloride solution may be regulated by attaching a capillary tube to the lower end of the burette.

B-3. CALCULATION

B-3.1 Polysulphide sulphur content of the material, percent ( m/v ) - 34’34 m

where m n mass, in g, of barium sulphate.

i

Its : 1050 - 1984

APPENDIX C

[ Table 1, Item ( iii ) 1

DETERMINATION OF THIOSULPHATE SULPHUR CONTENT

C-l. REAGENTS

C-l.1 Ammoniacal Zinc Chloride Solution - Dissolve 50 g of anhydrous zinc chloride ( Z&l, ) in about 500 ml of water, add 125 ml of ammonium hydroxide solution ( r.d. 0’90) and 50 g of ammonium chloride and dilute to 1 000 ml.

C-l.2 Methyl Orange Indicator Solution - 0’05 percent ( m/v ). Dissolve 0’5 g of methyl orange in water and dilute to 1 000 ml.

C-l.3 Methyl Red Indicator Solution - 0’5 percent ( m/v ) in methyl alcohol ( 95 percent by volume ).

C-l.4 Dilute Hydrocblorrc Acid - approximately 0’1 N.

C-l.5 Mucilage of Starch - About one percent ( m/v ), freshly prepared. Triturate one gram of starch with 5 ml of cold water, and add this with constant stirring to sufficient quantity of water to produce 100 ml. Boil for a few minutes, cool and filter.

C-l.6 Standard Iodine Solution - Approximately 0’05 N. Mix 6’35 g of iodine with 12’7 g of potassium iodine and dissolve in a small quantity of water. Filter the solution through a plug of glass wool, collect the filtrate in a one litre volumetric flask and make up the volume to mark with water. Standardized the iodine solution using arsenious oxide ( AsaOa ) dried at 105°C f 2°C.

C-2. PROCEDURE

C-2.1 Take 50 ml of water in a 200 ml of volumetric flask. Open a fresh bottle containing the prepared solution ( see A-2.1 ). and pipette* 50 ml of the prepared solution into the volumetric flask containing water. While transferring the prepared solution, keep the tip of the pipette just under the surface of the liquid in the volumetric flask and then raise the pipette to drain it. Add to the contents of the volumetric flask a slight excess of ammoniacal zinc chloride solution over the quantity required to precipitate all the sulphur present in 50 ml of the prepared solution. Dilute the contents of the volumetric flask to mark with water and shake thoroughly. Filter through a dry filter paper. Collect the filtrate in a clean dry beaker. Using a pipette, transfer 100 ml of the filtrate to a 250

*A clean, dry pipette shall be used.

9

ml of conical flask, add a few drops of methyl orange or methyl red indi- cator solution and exactly neutralized with drlute hydrochloric acid. Titrate the nuctral solution with standard iodine solution using a few drops of mucilage of starch. After titration, reserve the contents of the conical flask for the determination of sulphate sulphur content ( see D-2.1 >

C-3. CALCULATION

C-3.1 Thiosulphate sulphur content, fiercent ( m/v ) = 6’413 vN where

V- ,voh.&e, in ml, of standard iodine s&ion iequired for titration of 100 ml of the filtrate; and

N = normality of standard iodine solution.

APPENDIX D 1 Table I, Item (iv) j

DETERMINATlON OF tiLfiti:hTE SbL+Htik CdNTEN+

D-i. REAGENTS

D-l.1 Dilute Hgdiochloric Acid - 1 : 4 ( v/v )

D-l.2 Barium Chloride Solution - 10 percent ( m/v ).

D-2. PkociXiukE

D-2.1 Quantitatively transfer the contents of the conical flask after coin- pleting the titration with standard iodine solution ( see C-2.1 ) to a 400 ml beaker, slightly acidify with dilute hydrochloric acid and heat to boiling. Add slowly and with constant stirring a slight excess of barium chloride solution to the contents of the beaker and boil for 30 minutes. Allow the contents of the beaker to stand over night and then f&r through a quantitative filter paper ( Whatman No. 42 or equivalent ). Wash the last traces of the precipitate from the beaker on to the filter paper &Gig water. Wash the fiber with water uutil the washings are free from chlorides. Dry the precipitate for half an hour by placing the filter in a“ a$ oven. Transfer the filter &.$r along with the precipitate to a porcelain, crucrble, carefully rgn te and heat to constant mass I&n$n burner. Cool the cruci ‘le with contents in a desiccator b

.

i-3. CALCUL~T;[‘ON

I%%1 @@hate sulbhur content of the material, percent ( d/v ) = 13’74 3 where

m = mass, in g, of barium sui&&

ld

li3 t 10&i - l!iti

( Continued from page 2 1

iUembers Representing

DR K. N. SHRIVASTAVA Shaw Wallace & Co Limited, Calcutta SHRI R. N. ROYCHOWDHXJRY ( AIternare )

SHRI A. C. SEROFF Excel Industries Limited, Bombay SHRI P. V. KANGO ( Alternate )

DR K. SIVASANICARAN Union Carbide ( India ) Limited, NewDelhi DR U. V. SINGH ( Alternate )

SHRI N. S. VENKATARAMAN Department of Agriculture, Government of Tami Nadu, Madras

DR R. V. VENKATARATNAM Regional Research Laboratory Hyderabad

( CSIR ,)

DR NAOABHUJHAN RAO ( Alternate ) DR SANTOSH YELLORE Analytical Testing Services Pvt Ltd, New Delhi

DR D. B. ANANTI-IA NARAYANA ( Alternate ) SHRI T. PIJRF~ANAN~AM. Director General, ISI ( Ex-oficio Member )

Director ( Agri & Food )

Secretary

SHRI LAJINDBR SIN~H Deputy Director ( Agri & Food ), IS1

11