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IS 2316 (1990): Methods of preparation of standard
solutions for colorimetric and volumetric analysis [CHD 1:
Inorganic Chemicals]

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Satyanarayan Gangaram Pitroda
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IS 2316 : 1999 ( Reaffirmed 2001 ) Indian Standard METHODSOFPREPARATIONOFSTANDARD SOLUTIONSFORCOLORIMETRICAND VOLUMETRICANALYSIS f Second Revision First Reprint JANUARY 1993 UDC 543-4 : 543. 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 December 1990 Price Group 4 .24+543*43 @ BIS 1990 BUREAU OF INDIAN STANDARDS MANAK BHAVAN.

observed or calculated. New salts have been prescribed in many cases deleting the conventional salts for preparing the standard solutions. . This standard was first issued in 1963 and revised in 1968. more standard solutions have been incorwrated. if the final value. CHD 01 FOREWORD This Indian Standard ( Second Revision ) was adopted by the Bureau of Indian Standards on 28 February 1990.Chemical Standards Sectional Committee. In this second revision. is to be rounded off. it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )‘. al’ter the draft finalized by the Chemical Standards Sectional Committee had been approved by the Chemical Division Council. In reporting the result of a test or analysis made in accordance with this standard.

742 7 g of potassium antimony1 tartrate Dissolve 1 *OOOg of bismuth metal in nitric acid.Cl ) in a vacuum dessicator using 100 ml of water.O ) in water and dilute to 1 000 ml.1 This standard prescribes the methods of pre. One nitrogen ( as N ) per ml. One ml of this solution con- tains 1. chemicals of analytical reagent grade and distilled water ( se8 3 GENERAL IS 1070 : 1977 ) shall be employed in preparing 3.1 Preparation percent sulphuric acid. One ml of this 6.0 mg of arsenic ( as As ). Dissolve 1. All volumetric titra- tions shall be carried out in duplicate.O mg of barium( as Ba ).1 The following Indian Standards have been referred to in this standard : 3. Dissolve 1 *OOOg of pure aluminium foil in 40 ml of ( 1 : 1 ) hydrochloric acid and dilute to 100 8 STANDARD ARSENIC SOLUTION ml with water. material per litre contains 1.2 Unless specified otherwise.1 Preparation 10. 3 deals with secondary standards which require 2 REFERENCES standardization before use. 2. 4 QUALITY OF REAGENTS tion solution for volumetric analysis ( jrst revision ) 4. millilitre of this solution contains 1 .1 Preparation 1 0 mg of aluminium ( as Al ).2 A solution containing 3. Neutralize with dilute sulphuric calcium chloride as dessicant. 9.140 9 g of dried material in water and 9 STANDARD BARIUM SOLUTION dilute to 1 000 ml. One ml of this solution contains 1-O mg of antimony ( as Sb ). 1. ( second revision ) 2263 : 1979 Methods of preparation of indica. One ml of this solution contains 8. all chemicals IS No.778 7 g of barium chloride ( BaCIs.1.0 mg of ammonia ( as NHs ).] in 300 ml of 10 Add 50 ml of 1 : 1 sulphuric acid and evaporate 1 . Dilute to 1000 ml with 10 5.1 Keep overnight about 5 g of pure ammonium solution containing 4 g of sodium hydroxide in chloride ( NH.1 Preparation 6. Dilute with water containing 10 ml concent- rated sulphuric acid to 1 000 ml. l62316: l- Indian Standard METHODSOFPREPARATIONOFSTANDARD SOLUTIONSFORCOLORIMETRICAND VOLUMETRICANALYSIS (Second Revision ) 1 SCOPE given in Section 1 and solutions for volumetric determinations are given in Section 2 and 3. 7 STANDARD ANTIMONY SOLUTION lo STANDARD BISMUTH SOLUTION 7. Section 2 deals with primary standards which paration of standard solutions for the common require no further standardization while Section calorimetric and volumetric determinations.1 Solutions for calorimetric determinations are solutions and in tests.0 mg ammonical 2H.1 Preparation Dissolve 2. [ K (SbO ) C1 HI 0s 4 Hs 0 .320 3 g of arsenious trioxide ( A& 0s ) 6 STANDARD AMMONIUM SOLUTION in minimum volume of dilute sodium hydroxide 6. Title which do not contain water of crystallization shall be dried in an oven at 105 f 2°C until free from 1070 : 1977 Water for general laboratory use moisture. acid.819 0 g of dried Dissolve 1.1 Preporation solution contains I. SECTION 1 COLORIMETRIC SOLUTIONS 5 STANDARD ALUMINIUM SOLUTION percent sulphuric acid.1. Dissolve 3.1 Unless specified otherwise.

One millilitre of this 1.000 g pure manganese metal in 30 ml solution. Dilute to 1 litre with dilute to I ~00 ml.1 Preparation 19 STANDARD LEAD SOLUTION Dissolve 1. Dissolve 5. weigh 1. One millilitre of this solution contains 1 . 19.658 3 1 000 ml. [ ( NH4 )* SO1 Fe SO1.000 g of copper wire in minimum quantity of dilute nitric acid Dissolve 1. Dilute to 1 COO ml with 1 percent nitric acid.. Dissolve 1.1 Preparation in a polyethylene bottle. 7HsO ) in water and dilute to Dissolve I*000 g of magnesium turnings or 1.0 mg of Boron (as B ). 16. .7 19 9 g of boric acid ( Hs BOs ).2 Alternatively. 12 STANDARD CADMIUM SOLUTlON previously dried at 110 f 5°C to constant rnasg. One millilitre ol this solution contains 1 0 mg of iron ( as Fe’+ j.0 mg of cobalt ( as Co ). pre- viously dried to constant mass at 105 * 5”C.Cr. Heat to expel brown fumes. ( K.000 g ot pure cobalt metal in minimum contains l-0 mg of lead (as Pb ).648 5 g of sodium chloride in water and dilute to 1 000 ml. One millilitre of this solution contains 1 000 ml with water.000 g of pure cadmium metal chippings 18 STANDARD IRON SOLUTION in minimum volume of dilute nitric acid.O mg of cad. One millilitre of this solution contains 1 ‘II contains 1. Add 40 ml of 1 : 1 sulphuric acid. One millilitre of this solution water. volume of 1 : 1 nitric acid. Dilute to with water. Cool and dilute to 1 000 ml and evaporate to dense white fumes. Heat to dense white fumes.2 Alternatively. One millilitre 0: 12.929 1 g of CUPI.O. One milli- 14. Add 50 ml of 1 : 1 sulphuric acid and evaporate to dense 18. Dissolve 1. One millilitre of this solution contains g of magnesium oxide ( MgO ) in minimum 1-O mg of cobalt ( as Co ). Dissolve 7.1 Preparation litre of this solution contains 1. dissolve 3.0 mg of chromium ( as Cr+a ). 13. ) at 110” f 5°C to constant mass. One millilitre of this solution contains 1*Omg of copper ( as Cu ). One mi!lilitre of this SOIU- tion contains 1.835 8 g of lead acetate [ Pb 15. mg of lead ( as Pb >.1 Preparation 15. in 17 STANDARD IODINE SOLUTION warer and dilute to 1 000 ml.1 Preparation 21 STANDARD MANGANESE SOLUTION Clean the surface of an unenamelled copper wire 21.1 Preparation with a sand paper. in water and dilute to 1 000 ml. 5Ha0 ) in water and dilute to 11.IS 2316:1990 to dense white fumes. 20.1 Preparation ( CHs CCs )a 3 H. One millilitre of this solution contains 1-O mg of chloride ( as Cl ). amount of dilute hydrochloric acid and dilute to 1 000 ml.2 Alternatively dissolve 1 000 g of pure lead Dissolve 2 828 9 g of dried material in water and in 40 ml of 1 : 1 nitric acid. Add about 40 ml of 1 : 1 sulphuric acid of 1 : 1 nitric acid._ sulphate ( CuSO.1 Preparation this solution contains 1 0 mg of iodine ( as I ). Dissolve 1 a308 1 g of potassium iodide ( K1 ).3 If lead is to be determined by turbidimetric procedure.0 mg of copper ( as Cu ). 11 STANDARD BORON SOLUTION 16. 15 STANDARD COBALT SOLUTION 19. 19. dissolve 4.769 8 g of cobalt sulphate ( CoSO.1 Preparation 1 000 ml. Dilute 20 STANDARD MAGNESIUM SOLUTION to 1 000 ml with water.1 Preparation Dissolve l-598 5 g of lead nitrate [ Pb ( NOs )r ] 14 STANDARD CHROMIUM SOLUTlON in 200 ml of 1 percent nitric acid solution.1 Preparation white fumes.O ] in 200 ml water containing 10 ml concentrated sulphuric acid 13 STANDARD CHLORIDE SOLUTION Dilute with water to 1 000 ml.0 mg of lead ( as Dry about 4 g of pure potassium dichromate Pb ).C 1 and dilute to 1 000 ml with water. store 17. One millilitre of this solution contains 16 STANDARD COPPER SOLUTION 1-O mg of magnesium ( as Mg ). solution contains 1.021 5 g of ammonium ferrous sulphate mium ( as Cd ). One millilitre of this solution contains 1.0 mg of bismuth ( as Bi ). One millilitre of this solution Dissolve 1.. 6H. Dilute to 1 000 ml with water.

Warm to expel Dry about 2 g of potassium nitrate ( KNOs ) to brown fumes.0 mg of sodium ( as litre‘ of this solution contains 1. 30. ( NH.1 Preparation 24.2 Alternatively dissolve l-574 8 g of silver nitrate ( Ag NOs ) in water and dilute to 1 000 25 STANDARD NITRITE SOLUTION ml.542 1 g of dried mate- lvater. num ( as MO). x HsO ) at 5000 f 10% to constant mass. 25. Draw a 50 ml aliquot litre of this solution contains 1-O mg of nickel ( as acidify with hydrochloric acid and determine Ni ).99 percent pure silver foil in about 30 ml of 1:l nitric acid. 28 STANDARD SODIUM SOLUTION 22.1 Preparation Fuse 0. Dissolve Mn ). One millilitre of sunlight during weighing.748 5 g of anhy. Dilute to 1 000 ml with water.1 Preparation 31.. rial in water and dilute to 1 000 ml One millilitre chloric acid and make up to 1 000 ml. One millilitre of this solution contains 22 STANDARD MOLYBDENUM SOLUTION 1 . l-906 8 g of dried material in water and dilute to 1 000 ml. percent by mass in precipitated ammonium sulphate [ NiSO. hour and leach the melt with water. Boil to expel brown fumes.ofmanganese nnd dilute to 1 000 ml. One millilitre of this soluc ( as Mn ). then one millilitre of this solution con- 0 ] in water and dilute to 1 000 ml. Filter and Cool and dilute to 1000 ml with water. One millilitre of Dry about 3 g of potassium chloride ( KC1 ) at this solution contains l-0 mg of manganese ( as 105 f 5°C to constant mass and cool. 1 000 ml. One milli.1 Preparation 23. Dissolve store in amber coloured bottle.1 Preparation 28. 6Hs silica is X. Dilute with mass and cool.499 7 g of sodium nitrite ( NaNO.0 mg.630 6 g of dried material in water and dilute to this solution contains 1*Omg of silver ( as Ag ). One milli.2 Alternatively dissolve 6. 21. Na). One millilitre of 1. One millilitre of this solution contains 1-0 mg of nitrate ( as NOs ).478 7 g of 3 . 29 STANDARD SILICA SOLUTION 23 STANDARD NICKEL SOLUTION 29. Suppose silica con- 23.1 Preparation drous material in 50 ml of 10 percent nitric acid.1 Preparation Dry about 3 g of potassium dihydrogen phosphate ignite about 5 g of sodium sulphate ( NapSOl ) at ( KHsPO( ) at 105 & 5°C to constant mass and 500 f 20°C to constant mass.Cool and dilute with water to 1 000 ml.9 percent pure nickel in 30 sodium carborate in a platinum crucible for one ml of 1: 1 nitric acid.0 mg of nitrite ( as NOs ).O mg of potassium ( as K ). 2 All apparatus should be careYully washed with chloride free distilled water before use. silica content gravimetrically. tion contains 1. 26 STANDARD PHOSPHATE SOLUTION 31 STANDARD SULPHATE SOLUTION 26.1 Preparation NOTES 1 Care should be taken that there should be Dissolve 1.500 0 g of pure precipitated silica ( SiOs ) previously dried at 110 f 5°C with 5 g anhydrous Dissolve l*OOOg of 99.728 8 g of nickel tent ( as SiOs ).500 3 g of the dried material in a few ml of 500 f 20°C in a platinum crucible to constant dilute sodium hydroxide solution.0 mg of phosphate ( as PO.1 Preparation Dry about 2 g of molybdenum trioxide ( Moos ) at 105 f 5°C to constant mass and cool. this solution contains 1. One millilitre of this solution contains l-0 mg of silver ( as Ag ). Store in of this solution contains l-0 mg of nickel ( as a polyethylene bottle. Dissolve l-432 9 g of dried material in water litre of this solution contains I. Dilute to 1 000 ml with water and 105 & 5°C to constant mass and cool. of this solution contains 1. render slightly acidic with dilute hydro. )s SO. ). Then dissolve 2. 30 STANDARD SILVER SOLUTION 24 STANDARD NITRATE SOLUTION 30. One milli- dilute to 500 ml with water. Dissolve 2..1 Preparation Dissolve l-000 g of 99. ) minimum exposure of silver metal or its salts to direct in water and dilute to 1 000 ml. Dissolve Dry about 4 g of sodium chloride ( NaCl ) at 1. Ni ). 27. One millilitre tains l-0 x X/100 mg of silica ( SiOs ). Take 1.2 Alternatively heat about 5 g of manganese 27 STANDARD POTASSIUM SOLUTION sulphate ( MnSO. cool.0 mg of molybde.

If the colour returns.946 g of pure arsenious oxide ( AssOs ) 39 STANDARD OXALIC ACID in 30-40 ml of warm water containing 2-3 g of sodium hydroxide.1 Preparation Dissolve l*OOO g of 99. ( dihydrate ) in about 2C0 ml of water and dilute Add 500 ml of a 5 percent solution of sodium to 1000 ml.95 percent pure metallic tin in lC0 ml of 1:l hydrochloric acid and dilute zinc in 40 ml of 1: 1 hydroclllcric acid and dilute with the same acid to 1 000 ml.1 Preparation 36. One millilitre of thic NOTE. Dilute the solution to about 39. One millilitre of to 1 000 ml with water. 33 STANDARD TIN SOLUTOIN 36 STANDARD ZINC SOLUTION 33. solution into 500 ml dilute ( 4 N \ sulphuric acid metric flask. Pipette out 25 ml of this solution in and dilute to 1 000 ml.6 ml of hydrochloric dilute to 1 000 ml. cator to a colourless and point. 2HsO ] into a Kjeldahl flask. in calcium chloride as dessicant.1 N iodine be estimated for TiOs. if necessary.95 percent pure metallic Dissolve 1. add a few . volumetric flask.1 Preparation of 0. Dissolve 4.603 date ( NH‘ VOs ) in a vacuum dessicator usi. x V/25 mg sulphide per millilitre.1 Preparation of@1 N Solation -250 ml.1 Preparation content in 25 ml solution 1 ml of 0.3965 g of potassium titanyl oxalate 32 STANDARD SULPHIDE SOLUTION [ KsOTi ( C&O.the anhpdrous material and dissolve in water and 34 STANDARD TITANIUM SOLUTION dilute to 1 000 ml.4liquot of :he solution ma\ a conical flask and add 50 ml of 0. add 8 g of ammonium sulphate and 50 ml of 32. Similarly titrate 50 ml of blank iodine solution with sodium thio. cool and add 10 ml concentrated nitric acid and then dilute to 1 000 ml. solution contains 1. Dilute 40 STANDARD POTASSIUM BROMATE the solution with water to 1 000 ml.1 N sodium thiosulphate using starch as indi. minimum content of concentrated nitric acid.1 Preparation concentrated sulphuric acid.783 3 g of the dried material in water and 50 ml of water containing 10. Ti ). Gradually heat the Dissolve about 15 g of sodium sulphide ( NasS. Keep for 5 minutes and titrate with of this solution contains 1. tains l-0 mg of‘ sulphide ( as S ). pour the 9HsO ) in water and dilute to 500 ml in a volu.Os ) at 38.0 mg of titanium ( as 0.000 g of 99.1 Preparation of O-1 N Solution water. 34. When the effervescence ceases. The difference of two readings gives the volume of 0.1 N iodine equivalent to sulphide 35. )s. tion contains l-0 mg of zinc ( as Zn ). One millilitre of this solution contains l-0 mg of sulphate ( as SO. One millilitre solution to it. a volume of sodium sulphide solution containing 1 g of sulphide to 1 000 ml Dissolve 2. One millilitre of this solu- this solution contains 1 *O mg of tin ( as Sn ). SOLUTION 38 STANDARD CALCIUM SOLUTION 40. . SECTION 2 PRIMARY STANDARD VOLUMETRIC SOLUTIONS 37 STANDARD ARSENIOUS OXIDE ( OR acid. 35 STANDARD VANADlUM SOLUTION sulphate. Dissolve Dissolve 2. 4 . ). One millilitre of this solution con. Thus this solution (A) contains 1.1 Preparation Weigh 7. Neutralize the excess alkali with dilute sulphuric acid ( approximately 2 N ) until a few Dissolve 6.296 3 g of ammonium vanadate in with water. Dilute. Cool to room temperature and dilute to 1 000 ml with 37.502 2 g of pure calcium carbonate in 2. boil the solu- SODIUM ARSENITE SOLUTION ) tion to remove dissolved carbon dioxide. bicarbonate.0 mg of vanadium ( as V ). contents and boil for 10 minutes. This solution is unstable and shall be pre- pared fresh before use.1 N Solution Dry about 4 g of potassium bromate ( KB.drops of sulphuric acid to decolourize it. Cool. Heat.303 3 g of crystallized oxalic acid drops of phenolphthalein are just decolourized.1 Preparation of O-5 N Solution 150 f 5°C to constant mass and cool.1 N iodine solution consumed corresponds to l-603 mg of Keep over night about 5 g of ammonium vara- sulphide.

1 N Solution PHTHALATE SOLUTION The sodium chloride may be further purified ( if necessary ) by precipitating the sodium chloride 42.1 Preparation of O-1 N Solution 41. The end point is with water to 1 COOml in a volumetric flask.1 N portions of silver nitrate solution. dried material in water and dilute to 1 000 ml. Weigh 5.1 Preparation of 0.2 Alternatively. material in water and dilute to 1 000 ml. reached when one drop of the thiocyanate solution produces a faint brown colour. solution. Dissolve 4. ). add 56 ml of fills in. 5.700 0 g 01 1 000 ml. which 48.The strength of the standard solution thus Pipette 25 ml of standard 0.1 Preparation of O*l N Solution from a nearly saturated solution by passing hydro- gen chloride gas into the solution through inverted Dry about 25 g of potassium hydrogen phthalate funnel. dissolve in carbon dioxide free from water and is transferred to platinum crucible and ignited at dilute to 1 000 ml. Titrate with ammonium thiocyanate or potassium thiocyanate solution 48. Dry at 120 & 5°C to constant of dried material.1 Preparation of Approximate 0.ml.1 Preparation of Approximate O-1 N from a burette. ( It cer ic ammonium sulphate [ Ce ( SO. 45 STANDARD SODIUM CHLORIDE SOLUTION 42 STANDARD POTASSIUM HYDROGEN 45.CsHIJOI ) at 105 & 5°C for 2 hours and ted on a sintered crucible or other suitable filter cool.1 Preparation of O*l N Solution 105 f 5°C to constant mass and cool. Weigh 20. which 1 : 1 sulphuric acid and stir with frequent addi- quickly disappears on shaking. ] into a solution prepared by adding 5 . Individual Solution titrations should agree within 0. The precipitated sodium chloride is collec- ( HK. 260 f 10°C for 1 hour and cool.. add 5 ml of 6 N nitric acid ( 1 : 3 ) and 48 STANDARD CERIC SULPHATE 1 ml * of ferric alum indicator solution ( see SOLUTION IS 2263 : 1979 ).CrsOr ) . the precipitate becomes material is dissolved.566 7 g of dried material in water and dilute to constant mass and cool. Deter- mine the reagent blank. SECTION 3 SECONDARY STANDARD VOLUMETRIC SOLUTIONS 47 STANDARD THIOCYANATE SOLUTION titration in order to obtain correct results ). As the end tions of water and gentle warming until the point approaches.1 Preparation of 091 N Solution Dry about 10 g of sodium carbonate ( NasCOs) at Carefully pulverise about 6 g of potassium dichro.1 N silver nitrate prepared remains the same for a long period of rva- poration is prevented.CNS ) or 10 g of potassium thiocyanate basis of normality of standard silver nitrate ( KCNS ) in water and dilute to 1 000 ml.299 4 g mate ( K. Repeat the titration with two other 25 ml 47. 500 & 20°C. and as each drop of thiocyanate ( So4 )2 ] into a GCC-m 1 beaker. weigh out 66 g of pure no longer disappears on vigorous shakng. Calculate the Dissolve about 8 g of ammonium thiocyanate normality of the thiocyanate solution on the ( NH. solution ( see 54 ) into a 250-ml conical flask.1 ml.1 Preparation of O-1 N Solution SOLUTION Dry about 5 g of potassium iodate ( KIOs ) at 46. At first a white precipitate Solution is produced imparting a milky appearance Weigh out 36 g of pure ceric sulphate [ Ce to the solution.903 1 g of dried 1 000 .2 is essential to shake vigorously during the ( NH‘ )s SO. IS 2316 t 1990 41 STANDARD POTASSIUM 44 STANDARD SODIUM CARBONATE DlCHROMATE SOLUTION SOLUTION 44.422 3 g of dried material and About 7-8 g of this material medium and dried. Dissolve 6.04 ) at 1CO f 5°C to 3. Standardize the solution as follows: NOTE . SOLUTION 46 STANDARD SODlUM OXALATE 43. it’ produces a pink colour. Cool the solution and dilute flocculent and settles easily.834 3 g of ignited and cooled material is then dissolved in waters and diluted 43 STANDARD POTASSIUM IODATE to 1 000 ml. dissolve in water and dilute to weight and cool. Dissolve Dry sodium oxalate (CsNa.

add 25 ml of t N sulphuric acid.15 g of arsenious oxide ( EDTA ) SOLUTION ( AsrOB 1.CHs. how dilute.O. Now heat the solutibn to about.C. From the sodium thiosulphate solution into a 500-ml total volume of dichromate used.946 mg of As&. add the dichromate one drop at a time until the tinge of purple colour Transfer a 25 ml portion of standardized 0. At this point. 20 ml 0. Add 15 ml of sodium 49. calculate the normality of ferrous ammonium dilute to 50 ml and titrate with ceric sulphate sulphate solution on the basis of standard solution till the blue colour persists for 1 minute.3 With Sodium Thiosulbhate grey.2HB0 in water and 0.7 ). tion till the final blue colour is obtained. Diluteto Sohtion 100 ml and add 2’5ml of iodine monochloride solution and one drop of ferroin indicator. phate crystals [ Fe Sod-( NH. Stir the mixture until the material is tions of standardized 0. 6 .5 ml permanganate ( see 53 ) solution to the appear- of iodine monochloride solution as catalyst ( see ance of permanent pink colour. Titrate until the orange coloir begins to fade and returns only slowly Transfer about 40 g of ferrous ammonium sul- after the addition of each drop of ceric suIphr+te solu. Add 0 5 g of potassium iodide.84 ) to 500 ml Repeat the titration with two other similar por&- of water.1 Preparation of Approximate 0*05 M hydroxide solution ( 2 N ) and heat gently to Solution ( O-1 N ) hasten solution. Transfer to a 1 OOO-ml volumetric flask solution. Add 75 . Calculate the normality of the ceric 28.3 ml of 0. Heat to about 50°C and titrate with ceric sulphate solution potentiometrically using Alternatively. gr. 0. 570 ml of ammonium hydroxide and diluted to 1 litre ). Do not sodium salt of diphenylamine sulphuric acid.2. ( CHICO0 )* ] Na2.05 ml as a blank on the indicator and of O-2 percent freshly prepared starch solution. standard sodium thiosulphate solution.50°C and a 1 000-ml volumetric flask.756 g of zinc sulphate in water and made sulphate solution on the basis of arsenious oxide up to 1 litre.1 N sodium thiosulphate dissolved. Standardize the solution as of arsenious oxide taken. retroxide solution ( 0. Note above ). and dilute to about 300 ml.In place of osmium tetroxide. Titrate with late the normality of ceric sulphate solution on standard 0. Each 4. pipette 25 ml of the solution to platinum electrode or visually with 2 to 3 drops a conical flask.28 ml of stilphuric acid ( sp. ( Na.01 M solution of the remains pale blue for at least one minute. ). iodine mono.S04*6Ha0 ] to tion. pale blue. rulphuric acid ) as a catalyst ( set Note ) and one Standardize the solution as follows: drop of ferrc-pinindicator solution. ( see 40 ) slowly while stirring until the origi- nal pure green colour change to a greenish 48. ) into a 250-ml beaker.1 N appears and remains on stirring.01 N prepared by dissolving CH. NH. add 5 ml of phosphoric acid of ferroin indicator solution..1 Preparation of Approximate O-1 N add 20 ml of concentrated hydrochloric acid. Standardize sulphate solution on the basis of normality of the solution as follows. follows: 48.2 With Sodium Oxalate Transfer 25 ml of the solution to a 250-ml Weigh accurately O-15 to 0. allow the temperature to fall below 45°C.20 g of sodium oxalate conical flask. Cool to room temperature and add 25 ml of sulphuric acid ( 1 : 3 ). potassium dichromate solution.111of and titrate with standard 0. Shake until the contiune the addition of ceric sulphate solution drop by drop until the colour is completely discharged and material has dissolved in water containing 20 ml does not return within one minute. prepared by dissolving . 1. subtract conical flask.611 9 g of disodium ethylene diamine to 100 ml with water and add 3 drops of osmium tetraacetate dihydrate [ ( OOCCHs )s. Calcu. previously dried at 100°C for 1 hour into a 250-ml conical flask. 48. 20 ml of 12 N-hydrochloric acid and 1.1 With Arsenious bxide 49 STANDARD DISODIUM ETHYLEhE DIAMINE. until the solution ( sp gr 1. Store in a polyethylene bottle.1 N zinc orange colour changes sharply to colourless or sulphate solution.1 N potassium water. TETRAACETATE DIHYDRATE Weigh accurately 0’ 10 to 0.2. Calculate the normality of the ceric and make up to the mark with water. Finally titrate this solution with ceric sulphate solution until the Transfer 10 ml of the standard 0.1 N potassium dichromate solution the basis of sodium oxalate taken.5 g of ammonium chloride dissolved in 1 ml of 0 1 N ceric sulphate. Add 50 ml of buffer solution taken. Titrate it against the EDTA solu- NOTE .2. chloride (prepared by adding 25 ml of 0’04 M potas- sium iodide solution and 40 ml of 12 M hydrochloric 50 STANDARD FERROUS AMMONIUM acid to 20 ml of 0’025 M potassium iodate solution ) may be uaed as a catalyst as follows: SULPHATE SOLUTION Dissolve the arsenious oxide as described above and 50. Dissolve 18.255 g of osmium tetroxide in 100 ml of 0 1 N dilute to 1 000 ml. is equivalent to ( 67. Calculate the concentrated sulphuric acid and make up to the normality of the ceric sulphate solution on the basis mark with water.NH.

ric acid and add 3 ml exci .m Dilute to about Standardize the solution as follows: 200 ml with water. Titrate the sodium carbonate Repeat two more titrations. About 0’51. blue colour is develooed after adlitloq of a (b7.1 Preparation of Approximate @I N Solution Solution Dissolve 21. Titrate against standard 0. vigorously titrate with flask.1 N 52 STANDARD IODINE SOLUTION Solution 52. Allow to stand for 2-3 days in an amber-coloured Transfer 12.ml beaker about 0. Add 20 ml of potassium per- Transfer 25 ml of iodine solution to 250-ml manganate solution from a burette while conical flask and dilute to about 100 ml with shaking till the solution is decolourized and water.1 N sodium then heat to 55 f 5°C. At this temperature thiosulphatt solution from a burette until the complete the titration stirring gently with a colour is reduced to pale yellow. 53 STANDARD POTASSIUM FERROCYA.tandardized before use. persistent faint yellow. Af’ter thyl orange becomes orange or faint pink.987 3 g of silver nitrate ( Ag KOs ) in t KJe (CN)s 3HsO 1 and 0.1 ml.1 N sodium oxalate solution as follows: solution ( see 45 ) and add 50 ml of 10 percent sulphuric acid. Standardize the Pipette out 25 ml of 0. Heat LU . the colour chaogcs to purple.l Preparation of Approximate O-1 N Solutien Take into a 400. and potassium ferrocyanide to the colour change add 2 drops of methyl orange indicator ( see from purple to persistent yellowish green.1 Preparation of Approximate 0~1 N Carefully dissolve 3’2 g of potassium permanga- Solution nate ( KMn04 ) in water and dilute to 1 000 ml. 55 STANDARD SILVER NITRATE NIDE SOLUTION SOLUTION 53. The this. Add 2 ml of thermometer and allowing time for each drop starch solution and continue titration until the to be decolourized before adding the rest. Individual titration should agree within 0. Calculate the normality of the iodine volumes of sodium oxalate solution.pure potassium water and dilute to 1 000 ml. Add ( HCl ) into a 1 OOO-ml volumetric flask containing 15 ml of ammonia. Run a solution on the basis of standard sodium blank determination using 50 ml of 10 percent thiosulphate solution. Filter off any manganate 250-ml beaker containing 25 g of iodate free hydroxide through glass wool. It shall alwaya be c. add 2 drops of dipherlylamine indicator carbonate solution ( see 43 ) to 250-m] conical solution. Standardize the all iodine is dissolved and dilute with water to solution as follows: 1 000 ml. The solution shall be allowed to free distilled water before use. IS 2263 : 1979).1 Preparation of Approximate 0*05 M 55. A solution is just colourless. Repeat the titration with two more 0.The true end point is sharp.7 g of resublimed iodine ( Is ) to a glass stoppered bottle. Store in an amber 7 . Boil the solution and cool again.1’25 g of potassium ferrocyanide Dissolve 16. Stir unitl coloured glass-stoppered bottle. 54.1 ml.35 g accu- rately weighed metallic zinc ( 99.0 :nl wise and carefully until the colour of the me- before end point. The titration should agree within point. Initially a Continue the titration by adding the acid drop. Standardize the solution as follows: 51. neutralize with hydrochlo- about 500 ml of water cool and dilute to 1 000 ml. of standard sodium oxalate solution. Preserve in an amber-coloured glass stoppered bottle in a cool place.The strength of iodine solution deteriorate8 potassium permanganate based on the strength on keeping. Calculate the normality of NOTE . continue the addition until the and then calculate the normality. colour due to methyl orange becomes a very NOTE .5 g of. change from purple to a yellowish green. Whi!e stirritl:.1 Preparation of Approximate 8. titration should be performed dropwise far a titration is repeated with two other portions of sharp end point.v drons of potakum ferrocyinide solution. sodium carbonate solution.1 N sodium ly. IS 2316 J 1990 51 STANDARD HYDROCHLORIC ACID stand for four weeks before using. Calculate zinc solution against the hydrochloric acid to be equivalent of potassium ferrocyanide solution standardized. sulphuric acid. dilute to 50-75 ml with water.O”C approxirnatc- Transfer 25 ml of standard 0. All apparatus should ferrocyanide in previously boiled water and dilute be thoroughly washed with absolutely chloride to 1 000 ml. Calculate the 54 STANDARD POTASSIUM PERMANGA- normality of the hydrochloric acid on the basis NATE SOLUTION of standard carbonate solution. Repeat the titration faint pink colour which persists for 30 second with two more 25 ml portions of iodine after the addition of last dropshall be the end solution. Store in an amber- potassium iodide and 25 ml of water.95 percent Transfer by means of graduated cylinder or a pure ) cover with water and add 10 ml con- burette 9 ml of concentrated hydrochloric acid centrated hydrochloric acid to dissolve.

Calculate sharply from blue to light green. ( Na. not amount to more than 0.coloured glass-stoppered bottle. The nue the titration until the colour changes titrations should agree within 0. Store in a polyethylene bottle.O ).ml of the blank matches that of the solution conical flask. barium hydroxide and dilute to 1 000 ml with Standardize the solution as follows: water.1 ml. The normality of sulphuric acid solution on the various titrations should agree within 0. The indicator blank correction should and 8 ml of concentrated hydrochloric acid. When cold. Pipette out 25 ml of standard O-1 N sodium chloride solution (see 27) into a 250-ml conical flask resting on a white porcelain tile.1 ml of Mix thoroughly and titrate with sodium silver nitrate.03 to 0. Standardize the solution as follows: adding 1 ml of the indicator to a volume of’ water equal to the final volume in the titration Transfer 25 ml of the standard 03 1 N potassium and then silver nitrate solution until the colour dichromate solution ( see 46 ) into a 250. .1 N Solution Solution Dissolve 5 g of sodium hydroxide ( NaOH ) in Transfer 3 ml of sulphuric acid ( sp gr l-84 ) lU0 ml of boiled and carbon-dioxide free water into a 1 OOO-ml volumetric flask containing about in an Erlenmeyer flask. Calculate the normality of silver nitrate solution on the the normality of sodium thiosulphate solution basis of normality of sodium chloride.1 Preparation of Approximate O-1 N against silver nitrate until a faint but distinct Solution reddish-brown colour persists after vigorous Weigh 25 g of sodium thiosulphate crystals shaking. Add about O-5 g of 500 ml of water. basis of standard sodium hydroxide solution.S. 56 STANDARD SODIUM HYDROXIDE SOLUTION 58 STANDARD SULPHURIC ACID 56.1 Preparation of Approximate 6. Repeat the hydrogen phthalate solution ( see 41 ) using titration with two more 25 ml portions o: phenolphthalein as indicator. Titrate with sulphuric acid solution this solution against 0.1 ml. Add 2 ml of starch solution and conti- portions of sodium chloride solution. on the basis of normality of potassium dichromate.5H.1 N standard potassium using phenolphthalein indicator. thiosulphate. Standardize the Calculate the normality of sodium hydroxide solution as follows: solution on the basis of standard potassium hydrogen phthalate solution.1 N sodium hydroxide solution . Calculate the portions of sodium hydroxide solution. Add a 57 STANDARD SODIUM THIOSULPHATE few drops of potassium chromate indicator SOLUTION solution ( see IS 2263 : 1979 ‘Methods of preparation of indicator solutions ) and titrate 57. dilute to 1 000 ml. Standardize this solution as follows: Transfer 25 ml of standard 0. dissolve in water and dilute Determine the indicator blank correction by 1 000 ml.1 Preparation of Approximate O-1 N 58.Os. sodium hydroxide solution The various titra- Repeat the titration with two further 25 ml tion should agree within 0. Add 2 g of potassium iodide titrated. swirling the liquid constantly until the brown colour changes to yellowish Repeat the titration with two further 25 ml green.( see 55 ) into 250-ml coni- Determine the normality by titrating 25 ml of cal flask.1 ml.

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