L Matta MettataRetetaRaaMaReReMe! 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 accets 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. ear a afirare, aft a attrac” oqce & ae Mazdoor Kisan St than Jawabarlal Nehru Ete Right to information, The Right to Live” Step Out From the Old to the News Satyanarayan Gangaram Pitroda ‘Bhartrhari—Nitisatakam oo Oo OO O&O oO Oo Oe @ @ @ 4BLANK PAGE PROTECTED BY COPYRIGHTIS : 252-1991 (Reaffirmed 2010) aredta ara after ast, Te att aH — fafafce ( atterer qardteror ) Indian Standard CAUSTIC SODA, PURE AND TECHNICAL — SPECIFICATION ( Third Revision ) Third Reprint MAY 2007 (including Amendment 1) UDC 661.322.1 © BIS 1991 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 October 1991 Price Group 6Acids, Alkalies and Halides Sectional Committ CHD 002 FOREWORD This Indian Standard ( Third Revision ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Acids, Alkalies and Halides Sectional Committee had been approved by the Chemical Division Council. The specifications for caustic soda, technical (IS 252 ) and caustic soda, pure (1S 1021 ) were first issued in 1950 and 1956, respectively. These specifications were later revised in 1962 and 1964, respectively modifying the limits for iron, chlorides, sulphates, silicates and manganese. During the second revision in 1973, IS 1021 was amalgamated with IS 252 and requirements for caustic soda lye and caustic soda solid were also included, The method of sampling and tests were also modified during the course of the second revision. In the present revision, requirements for chlorates, perchlorates and matter insoluble in water along with the relevant test methods ave been incorporated for pure grade of caustic soda, Methods of test for determination of silica, carbonates, sodium hydroxide, chlorides, iron and copper have been suitably modified. 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, ‘Rules for rounding off numerical values ( revised ). The number of significant places retained in the rounded off value should be the same as that of the specified value in this standardAMENDMENT NO. 1 FEBRUARY 1995 TO IS 252 : 1991 CAUSTIC SODA, PURE AND TECHNICAL — SPECIFICATION (Third Revision) [ Page 2, Table 1, SINo. (x). col $ and 6 | — Substitute '0.2' for'0.02" (CHD 002) 114 ISNDAOTGMCIPX—14 BISIND/O—100I 252 : 1991 Indian Standard CAUSTIC SODA, PURE AND TECHNICAL — SPECIFICATION (Third Revision ) 1 SCOPE, J. This standard prescribes the requirements and the methods of sampling and test for caustic soda, pure and technical. 1.1.1 It covers the material in the solid and lye form, 2. REFERENCES ‘The Indian Standards. listed below are necessary adjuncts to this standard: the IS. No. Title 265; 1987 Hydrochloric acid (third revision) 296: 1986 Sodium carbonate, anhydrous (third revision ) 323: 1959 Rectified spirit ( revised ) 1070: 1977 Water for general laboratory use ( second revision ) 1260 Pictorial marking for handling (Partt) + 1973 and labelling of goods : Part | Dangerous goods (first revision ) 4264:1967 Code of safety for caustic soda 3 GRADES There shall be two grades of the material, namely: a) Pure — suitable for use in rayon and cosmetic industries, and b) Technical — suitable for use in textile, soap, vegetable oil refining paper and other industries. 4 REQUIREMENTS 4.1. Form and Description The material shall be supplied in the form of lye or solid (including flakes, blocks, sticks and pellets). 4.1.1 The material shall be. free from foreign matter, dirt or other visible impurities. 4.2. Relative Density of Canstic Soda Lye ‘The relative density of caustic soda lye shall be subject to an agreement between the purchaser and the supplier. 4.3 The material shall comply on dry basis, with the requirements given in Table T, when tested according to the methods prescribed in Annex A. Reference to the relevant clauses of ‘Annex A’is given in col 7 of the table. 4.4 For Technical Grade Chlorides (as NaCl) and sulphates (as Na,SO; together shall be 3.5 percent. The value for sulphate content shail also be reported. 45 Calculation of Results on Dry Basis In AB to A-12, results have been calculated on the basis of the material as received. To calculate the results on the dry basis as speci- fied in Table 1, the method given in A-I3 st be adopted. 5 PRECAUTION IN HANDLING AND STORING The precautions in handling and storing as given in IS 4264 ; 1967 shall be observed. 6 PACKING AND MARKING 6.1 Packing The material shall be packed. in polyethylene bags or polyethylene Iimed gunny bags or steel drums, or as agreed to between the purchaser and the supplier, The solution shal be supplied in tankers or tank cars. 6.2 Marking Each container shall be securely closed and shall bear legibly and indelibly the following information: a) Name and grade of the material; b) Indication of the source of manufacture; ©) Net mass of the material; and ) Lot or batch number, in code or other-IS 252: 1991 ‘Table 1 Requirements for C: ‘austic Soda, Pure and Technical ( Clause 4.3) 8 Characteristic Requrenent on Dry Basis Method of ‘0. Test Ref To a Teale CL No. In Lye Solid Lye Solid Ammer A 1 2 ; ‘ 5 Fi fi 1) Sodium carbonates Nas COs), 04-040 «2002.00 a pore bys sae iy Sodium hydrondefas Naot), 995099509500 98.0 a4 peveent by assy Ain tu) Chlondgy a NACH, percent by 0108.40 As . 3.50 3.50 iv) Sulphate (as Na:S00), percent by 010 0.10 AG w Slices (as Si0%), percent oom - 8 a ying. May vi) Tron (es Fe), ppm, Mar 2 30 AS wil) Copper (as Cu), pom, Mar 2 2 _ ao vii) Manganese (as Mt). ppm, Max 1 a io 1x) Chiorates and perchlorates (as 10 10 — at NaciO', pom. Hee sy Matter insoluble in'water percent 005 005-02 ap nase Nae 6.2.1 The containers shall be marked with the 7 SAMPLING following caution note: ‘CORROSIVE - HANDLE WITH CARE! and appropriate label to. indicate the possible corrosion hazards [see TS 1260 (Part 1) : 1973 J. ‘The procedure for drawing _ representative samples ofthe material and their criteria for conformity shall be as prescribed in Annex B. ANNEX A (Clauses 4.3, 4.4, 4.5 and Table 1) METHODS OF T Ac] QUALITY OF REAGENTS AcLI Unless specified otherwise, cals and distilled water (see IS shall be used in tests. NOTE — Pure chemicals) do not contain impurities analysis, yure_chemi- (070: 1977) i aH Te aah oF A-2 PREPARED SAMPLI A-2.1 Ina weighing bottle with a ground-glass stopper, weigh to the nearest 0.01. g, of the material (solid or liquid ), equivalent to a little less than 50 g,. of caustic soda. SOLUTION FOR CAUSTIC SODA A2L1 Solid Material Dissolve the material (see A-2.1 ) in approxi- mately 200 ml of water and. cool it to room temperature; transfer the solution quantitatively toa 500-mi_one-mark volumetric flask and dilute nearly to the mark, recool, then dilute to the mark and mix thoroughly. ‘The solution thus prepared shall be used for the subsequent tests, A-212 Liquid Material Transfer the material ( see A-2.1 ) directly to a 500-ml one-mark, volumetric flask and dilute nearly to the mark; cool to room temperature, then dilute to the mark and mix thoroughly.A.3 DETERMINATION OF CARBONATES A-3.0 Two methods, namely, Method 4 Double Indicator Method and Method 8 Gascometric Method have been prescribed. Method 4 shall be used for routine analysis and Method B shall be used as a referee method. A-3.1 Method A (Double Indicator Method ) 1 Reagents A.A Standard hydrochloric acid — 1 N. A-34L1.2 Standard hydrochloric acid — 0.1 N Ac3.1.13 Methyl orange indicator solution — Dissolve 0.1 gof methyl orange in 100 ml of water, A-3.1.1.4 Phenolphthalein indicator solution — Dissolve 0. g of phenolphthalein powder in 60 ml of rectified spirit (sec IS 323 : 1959 ) and dilute with water to 100 ml A Pipette out 25_ ml of the prepared sample solution ( see A-2 ) into a conical flask and add 2 to 3 drops. of phenolphthalcin indicator, Titrate it against standard hydrochloric acid solution (1.V) up to a little before the end point. Take this reading as A. Further titrate it against standard hydrochloric acid (0.1 N) till the pink colour just disappears. Take this reading as B. ‘Then add 2 to 3 drops of methyl orange indicator and continue titration against standard hydrochloric acid (0.1.N) to a reddish orange colour. Take this reading as C. 3.1.3 Calculation Carbonates (as Naz COs ), 212 (C—B)xN 2( CT BIAN 1.2 Procedure Percent by mass, A = where N = normality of standard hydrochloric acid (0.1N) and, M = mass of the material taken for test. A-3.2 Method B ( Gascometric Method ) AS 0 Principle Measurement of the volume of carbon dioxide evolved from a portion of the test sample by reaction with a hydrochloric acid 1 Reagents 21-1 Distilled water, or water of equivalent purity—Free from carbon dioxide at room tem- perature. Eliminate any carbon dioxide present In water either by boiling for 10 minutes. and IS 252 : 1991 cooling it in the absence of atmospheric carbon dioxide or, more simply, by bubbling at free from carbon dioxide through it for 15 minutes. The air is freed from carbon dioxide by passing it through a column containing pellets of sodium hydroxide, Store it in the absence of atmos- pheric carbon dioxide AB2A2 Hydrochloric acid— 12.N. A33.2.1.3 Sodium chloride, coloured acid solution Dissolve 26 g of sodium chloride in water. Add 5 ail of sulphuric acid, solution (01.83) Dilute it to 1000 ml, add a_small amount of 0.05 percent methyl orange indicator solution and mix thoroughly A-3.2.14 Sodium hydroxide solution — 6 N. A3.2.2 Apparatus — Apparatus as assembled is shown m Fig. | A323 Procedure 3.23.1 Weigh, to the nearest 0.01 g, the test sample ( solid or lye ) corresponding to approximately 10 g of caustic sod: 2.3.2 Assembly of the apparatus the Fill coloured acid solution through leveling bottle F. Pour into absorber C some of the sodium burette B of the apparatus with hydroxide solution. (Renew this solution after 100 determination. ) With burette B and absorber C filled up to cock R, and graduation mark a, respectively, and cocks R; and R: closed, place the test portion in flask 4 and, in the case of solid material, dissolve it’ in approximately 30 ml of water. Dilute to approximately 40 ml so as to reduce the dead space to a volume slightly greater than 100 ml (volume above the level of the Tiguid in flask A plus the volume of condenser tube D up to cock R ). Place in the flask three porcelain or glass balls, about 2 mm in diameter, and a few pieces of pumice having a total volume approximately equal to that ofthe balls. Stopper the flask and close cock R, Connect flask A with burette B through cock Ry and lower the leveling bottle F. Check the tightness of the apparatus by appropriately handling the cocks and the leveling bottle. A-3.2.33 Evolution and measurement of carbon dioxide By means ofa separating funnel, pour 35 ml of hydrochloric acid into flask 4 taking care to avoid loss of gas. ‘The acidity of the solution in the flask is thus approximately 2 NV after the evolution of carbon dioxide. Heat the flask and maintain the solution at boiling point forIS 252: 1991 COMPRESSED AIR FOR Shianine tHe warew Eoutaime am THe. FRermostatie vacker TE |Mosratic iener water AOEOS gs souution aeoirED wit fasvano Covdu- Reo ey meine ‘Onance: FG 1 5 minutes while running cold water through the condenser. Then stop heating and add more of the coloured acid solution by means of the separating funnel, lowering the leveling bottle F still further to make the solution in the flask 4 rise in the condenser tube up to cock Ry. Then close the latter and wait for S$ minutes to allow the gas to reach the temperature of the water jacket. Measure the volume of gas V at atmos- pheric pressure P and at the temperature 1 of the vter in the jacket, For this purpose move the leveling bottle F to bring the coloured acid solution to the same level both in the flask and capacity ‘SBOUT Wom RUBBER TUBE 0 HERMOMETER aabUaIEO mW Oe Pieces oF agour THE SAME VOLUME ASSEMBLY OF APPARATUS FOR DETERMINATION OF CARBONATES in the burette B; read the volume of the latter. Adjust the cocks Ry and Rz so that burette B absorber Care connected, then raise the leveling bottle F’so that the gas is transferred to the absorber where the carbon dioxide is absorbed. Then transfer the non-absorbed gas back to burette B by lowering the leveling bottle Fand, after adjusting the level of the hydroxide solution to the gauge mark a on absorber C, close cock Ry and read the volume of the residual gas. Repeat. these operations until a constant volume Vi is obtained, The difference in the volume, V— Vj, representsthe carbon dioxide contained in the test portion, measured at atmospheric pressure and at the temperature of the water jacket. A324 Calculation Carbonates ( as Na; CO; ), percent = v-" by mass, A = 0170 oP =n PGP where P = atmospheric pressure in mm, Hg at the time of determination, vapour pressure, in mm, Hg of the coloured acid solution at the tempera- ture of the water contained in the jacket, jemperature in degrees centigrade of the water contained in the water jacket, volume, in ml, of gas before absorption of carbon dioxide, V;: = volume, in ml, of gas after absorption of carbon dioxide, and ‘M = mass, in g of the material taken for the test A4 DETERMINATION OF SODIUM HYDROXIDE Acd.I Reagents AALLI Standard Hydrochloric Acid — 1 N. ‘A-4.1.2 Methyl Orange Indicator Solution — Dissolve 0.1 g of methyl orange in 100 ml of water, pe v AA4.2 Procedure Transfer exactly 20 ml of the sample solution (see A-2) to a 500ml conical flask. Add approximately 80 ml of water and 5 drops of methyl orange indicator solution and titrate it against standard hydrochloric acid until the colour of the indicator changes from yellow to orange. ‘A-43- Calculation Total alkalinity (as NaOH ), percent by mass B where V = volume in ml of standard hydrochloric acid used for titration, N = normality of standard hydrochloric acid, and M = mass in g of the material taken for the test. 244 BISNDOT IS 252 : 199 Sodium hydroxide (as NaOH), percent by mass ~ B-(4 x 40/53) where B = total alkalinity (as NaOH ), and 4 = carbonate content ( as Na;CO; ) as culated in A3.3 or A-3. A-5 DETERMINATION OF CHLORIDI 5.1 Reagents AS. Concentrated Nitric Acid AS5.1.2 Standard Silver Nitrate Solution —0.1 1.3 Nitrobenzene A-S.1.4 Standard ‘Solution’ — 0.1 N. Ammonium — Thiocyanate A-S.L5 Ferric Ammonium Sulphate Indicator — saturated solution, A-8.1.6 Diluted Sample for Testing Chlorides in Technical Grade Pipette out 50 ml of the sample solution ( see ABT Sto 2 250 standard messing Mask and make up the volume to 250 ml_mark with water. This solution shall also be used for the determination of iron content. A-5.2 Procedure AS.2.1 For Caustic Soda, Solid Transfer exactly 50 ml of the sample (see A-5.1,6) solution to a conical flask, neutralize it with concentrated nitric acid and then add 5 ml of the acid in excess, Add 5 ml of nitro- benzene and shake vigorously; pipette out into this 20 ml of standard silver nitrate. solution, Titrate it’ against standard ammonium thiocyanate solution using ferric ammonium sulphate indicator, A522 For Caustic Soda, Lye Weigh accurately a quantity of the material containing not more than 0.05 g of chlorides (as NaCl) and carry out the test as prescribed in AS.2L A-5.2.3 For Caustic Soda, Pure Grade Weigh accurately about IS g of the material, dissolve it in about 50 ml distilled water and carry out the test as preseribed in A-§.2.1 A-5.3 Calculation A-S3.1 For Caustic Soda, ( Solid Technical ) Chlorides (as NaCl), rent by mass = 3 (20M oV Ms pe1S 252: 1991 where Ny = normality of standard silver nitrate solution, V ~ volume in ml of standard ammonium thiocyanate solution used in A-§.2.1 Ny = normality of standard ammonium thiocyanate solution, and M = mass in g of the material taken in AQL. A.5.3.2 For Caustic Soda, Lye Chlorides ( as NaC), 5 (20 NV Na) S045 (20 N= Na) percent by mass where N, and Nz are the same as specified in ASB V = volume in ml of standard ammonium thiocyanate solution used in A.8.2.2, an M = mass in g of the material taken for the test in A-5.2.2. A-53.3 For Caustic Soda, Pure Grade Chlorides ( as NaCl ), where Ny and AS3.1 V; = volume in ml of standard ammonium thiocyanate solution used in A- and ‘M = mass in g of the material taken for the test in A-5.2.3. A-6 DETERMINATION OF SULPHATES A-6.1 Reagents A611 Concentrated see IS 265 : 1987. A-6.1.2 Barium Chloride Solution — 10 percent. are the same as. specified in Hydrochloric Acid — A-6.2 Procedure Weigh accurately about 10g ofthe material and dissolve it in 100 ml of water. Add sufficient quantity of concentrated hydro- chloric acid to neutralize and leave an excess of acid in the solution. Boil it to. decompose the carbonates. Filter the resulting solution through a folded filter paper thoroughly, collecting both the filtrate and washing in a 500-ml beaker. Dilute it to 250 ml, boil and add 10 ml of hot barium chloride solution to the boiling solution. Boil it again for 2 minutes; let it stand for 4 hours, and then filter through a tared sintered glass crucible (G No. 4) or a tated Gooch crucible. Wash the precipitate to free it from chlorides, and dry to constant mass at 105 to 110°C A+6.2.1 Excess barium chloride is necessary to reduce the solubility of barium sulphate, Precipitation. in hot solution by the addition of barium chloride in a slow stream with. stirring minimizes the mechanical occlusion of barium chloride and gives a coarse precipitate which is less soluble in acids. A-6.3 Calculation Sulphates ( as Na,Sos ), 60-86 percent by mass = sous M. where ‘M, = mass in g of the precipitate, and M = mass in g of the material taken for the test. <7 DETERMINATION OF A-7.0 Outline of the Method Silica is determined colorimetrically by_ visual CATES comparison or by spectrophotometer as molybdenum blue. 1 Apparatus ACTALL Nessler Cylinders — 100-ml capacity. ACT. Reagents AeT2A Dilute Sulphuric Acid — approximately A722 Ammonium Molybdate Solution — Dissoive 10 g of ammonium molybdate in 100 ml of dilute sulphuric acid (1 N ), A123 Sodium Citrate Solution — Dissolve 8 g of Sodium citrate (as NasCeHsOr, 2H,0 ) in 100 mi of water. A124 Reducing Solution — Dissolve 7 g of anhydrous sodium sulphite in 100 ml of water and add 1.5 g_ of l-amino-2-naphthol-4-sulph- onic acid. When this is dissolved, add to. this solution, a solution containing 90 g of sodium bisulphite in 800 ml of water, and dilute to 1.000 mi ATS Sodium see IS 296 : 1986 Carbonate, Anhydrous —A7.2.6 Standard Silicate Solution — Fuse 0.1 g of pure precipitated silica with anhydrous sodium carbonate ina platinum crucible and Teach the melt with water, neutralise with dilute sulphuric acid and dilute to 1 000 ml Dilute 10 ml of this solution to 100 ml. One ml of the diluted solution contains 0.01 mg of silica (as SiO; ). Store the solution in a polyethylene bottle. A-73 Procedure Dissolve 5g of the sample ( 10 g in case of caustic soda in lye form) in water in a polyethylene beaker and make upto 250 ml in a standard flask. Transfer 10 ml of the solution into a polyethylene beaker, neutralise with dilute sulphuric acid and add excess of acid to bring the pH of the solution to 15 to 16 Transfer toa 100ml Nessler cylinder, add 2 ml of ammonium molybdale solution and allow to stand for 5 minutes, Then add 5 ml of sodium citrate solution, followed by 2 ml of reducing solution ( see A-7.2.4), Dilute to 100 ml and stir well Carry out a control test in another Nessler cylinder, using 4 ml of standard silica solution in place of the sample and the same quantities of other reagents in the same total volume of reaction mixture. Allow the two Nessler cylinders to stand for 30 minutes and compare the colour developed in the two cylinders A-7.3.1 The limit prescribed for silicates shall be faken as not having been exceeded if any blue colour produced in the test with the material is not deeper than that produced in the control test. A-T.4 The colour produced can also be ‘measured on a spectrophotometer by measuring the absorbance at 820 nm and compared with a standard graph drawn as given below: A standard graph is drawn by measuring the absorbance of 2 ml, 4 ml, 6 ml, 8ml and 10 ml of standard silica solution treated with the above reagents in the same way and plotting the absorbance against the silica content. AS DETERMINATION OF IRON A-8.1 Apparatus ABA A-8.2 Reagents Nessler Cylinders — 100-ml. capacity, A821 Concentrated see IS 265 : 1987, Hydrochloric Acid — A8.2.2 Ammonium Persulphate 1S 252: 1991 A-8.2.3 Potassium — Thiocyanate Solution — approximately 5 percent, OR Ammonium Thiocyanate Solution — approximately $ percent. A-8.24 Standard Iron Solution Dissolve 0.702 g of ferrous ammonium sulphate [ FeSo,. (NH; }:S04 6H;0 ] in 100 ml of distilled water and 10 ml of concentrated sulphuric acid, add dilute potassium perman- ganate solution dropwise (0.2 percent, m/v ) Until a slight pink colour persists after stirring, and then dilute with water to 1 000-ml_ mark. Transfer 100 ml of this solution to 1 000-mi volumetric flask and dilute again to 1 000-ml mark. One millilire of this solution is equivalent to 0.01 mg of iron ( as Fe ), A-83 Procedure AB31 For Caustic Soda, Solid Transfer by means of a pipette 25 ml of the sample solution ( see A2.1) for pure grade, or 10. ml of the diluted sample solution (‘see A-5.1.6 ) for technical grade, dilute to 50 ml ‘and make acidic with concentrated bydro~ chloric acid, Add 30 mg of ammonium” per- sulphate and boil to oxidize the iron. Cool and wansfer to a Nessler cylinder, add 2 ml of potassium thiocyanate solution ( or ammonium thicoyanate solution ) and dilute to 100ml mark with water. In another Nessler cylinder, take the same amount of concentrated hydrochloric acid, ammonium — persulphate and potassium "thiocyanate solution (ammonium thiocyanate solution), as used with the material and dilute to about 85 ml Prom a burettc add standard iron solution in small portions at a time so that after dilution to 100 ml, the colour obtained matches with that obtained with the material AB3.2 ‘or Caustic Soda, Lye Weigh accurately an amount of the material containing not more than 0.035 mg of iron (as Pe) and carry out the test as in A-B.3.1 A-84 Calculation ABA For Caustic Soda, Solid ( Technical) 2500 Iron (25 Pe), ppm = 250¥ AcRA2 For Caustic Soda ( pure ) 200 ¥ Iron (a8 Pe) ppm = (as Pe). ppm =— 200IS 252: 1991 where V = volume in ml of standard iron solution used in A-8.3.1, and ‘M = mass, in g of the material taken for the test ( see Ae2.1 and A-5.1.6 ). A843 For Caustic Soda, Lye lov. Iron (as Fe ), ppm = —57 where V= volume, in ml, of standard iron solution used in’A-8.3.2, and M = mass in g of the material taken for the test in A-8.3.2 A DETERMINATION OF COPPER A091 Apparatus A-9.1.1 Nessler Cylinders — 100-ml capacity. A092. Reagents A921 Concentrated Sulphuric Acid A922 Litmus Paper A-9.2.3 Ammonium Chloride A-9.2.4 Concentrated Ammonium Hydroxide — sp a 0.92, Citric Acid Solution — Dissolve 100 cid (monohydrate) crystals in 100 ml of water. ‘9.2.6 Dilute Ammonium Hydroxide — approxi« mately 3 N. A927 Gum Acacia Suspension — Dissolve 0g of gum acacia in’ 100 ml of boiling water, filter and dilute to 200 ml. ( This solution shali be prepared fresh.) A-9.28 Tetrasodium Pyrophosphate Solution — Dissolve 4 g of tetrasodium pyrophosphate in 100 ml of water, A-9-2.9 Sodium Diethyl Dithoicarbamate Solution — Dissolve 0.2 g sodium diethyl dithoicarbamate in water and make up the volume to 100 mi. A-9.2.10 Standard Copper Solution — Dissolve 0,392'8 g of copper. sulphate pentahydrate (CuSO, SH;0 ) in slightly acidulated “water and make up the volume to 1 000 ml in a volumetric flask. Pipette out exactly 10 ml of the solution ina 100-ml volumetric flask and make up the volume to 100-ml mark. One milli- litre of this solution is equivalent to 0.01 mg of copper. A92I1 pH-Meter A9 3 Procedure A-93.1 Weigh about 10g of material, to the nearest 01g, and transfer it into a 400-ml beaker. Dissolve it in about 20 ml of water and then neutralize with concentrated sulphuric acid using litmus paper. To the neutralized solution add ammonium chloride and concen- trated ammonium hydroxide to precipitate out iron, Heal the solution to coagulate the precipitate, Filter the precipitate through a Gooch crucible with an asbestos mat and wash the residue twice with water. Collect the filtrate and the washing in a beaker. Cover the beaker with a watch glass and, then evaporate to a volume of about 70 ml. Transfer the solution to 100-ml Nessler cylinder, To this add 2 ml citric acid solution’ and add dilute ammonium hydroxide (till pH 85). Mix the solution thoroughly and then add 10 ml of gum acacia suspension, 5 ml of tetrasodium pyrophosphate solution and 10 ml of the sodium diethyl dithiocarbamate solution and dilute to 100-ml mark with distilled water. To another Nessler cylinder add 2 ml of citric acid solution dilute ammonium hydroxide ( till pH 8.5 ), 10 ml gum acacia suspension, 5 inl of tetrasodium pyro- phosphate solution, 10 ml of sodium diethyl dithiocarbamate solution and then 2 ml of standard copper solution. Make up to, 100-ml mark with distilled water and mix well. Compare the colour produced in the two cylinders after 10 minutes. A93.11 The limit prescribed shall be_ taken as not having exceeded if the intensity of colour produced in the test with the material is not greater than that in the control test. A-l0 DETERMINATION OF MANGANESE, ‘A-10.1. Apparatus — Nessler 100-mi capacity. cylinder, A102 Reagents A-10.21 Phosphoric Acid — 85 percent (manga- nese free ), A-10.2.2 Potassium Periodate A10.2.3 Standard Manganese Solution—Dissolve 03077 g of manganese sulphate, monohydrate (Mn$0j, HO.) in water, add 1’ml of concen- trated sulphuric acid and make up the volume to 1 000-ml in a volumetric flask. Pipette out 10 ml of this solution in a 100ml volumetric flask and dilute to the mark. One ml of this solution is equivalent to 0.01 mg of manganese.A103 Procedure A-10.3.4 Weigh about 10g of the material to the nearest 0-1 g and transfer it to a 400 ml beaker and dissolve in about 40 ml_water. To this solution, add 10 to 15 ml of phosphoric acid and 06 to 0.8 g potassium periodate, Heat the solution to boiling. Boil for 20 minutes. Cool the solution ‘to room temperature. Transfer the solution to a 100 ml Nessler cylinder. “Make up to the mark with distilled water and mix well. Compare the colour with that in the other Nessler cylinder containing 1 ml of standard manganese solution in. place of the test solution treated. similarly under similar conditions with the same amounts of reagents for the same time as in the test solution, and make up to 100 ml mark 10.3.2 The limit prescribed shall be taken as not having exceeded if the intensity of colour produced in the test with the material is not greater than that in the control test. Acll DETERMINATION OF CHLORATES AND PERCHLORATES (AS SODIUM CHLORATE ) A-1LO Two methods, namely. Method A and Method B have been’ prescribed. Acl1L Method A A-IL1.0 Outline ofthe Method A little excess of ferrous ammonium sulphate added to the slightly acidified solution of caustic soda is oxidized quantitatively by the chlorate present in caustic soda. The chlorate is estimated by back titrating the excess ferrous ammonium sulphate with potassium — per- ‘manganate, ACILLA Reagents ALL Ld Ferrous ammonium sulphate solution — 0.02 N Dissolve 3.92 g of ferrous ammonium sulphate crystals in’300 ml of water. Add 1 ml of concentrated sulphuric acid and make up to 500 ml AALLA.2 Sulphune acid — 11 (wv). ACILLL3 Potassium permanganate solution — O.1.N Weigh about 40—3.25 of potassium permanganate into a beaker, add a little of ‘water and boil it gently for iS minutes. After cooling, filter the solution through fumel with a plug of glass wool and dilute to 1 000 ml Collect the filtrate in a brown-coloured bottle and standardize with sodium oxalate solution. 18252: 1991 ACILI.L4 Potassium permanganate solution — 002 NV Dilute 50 ml’ of 0.1 0 potassium per- manganate solution ( see A-IL1.1.3) to 250 ml in a volumetric flask. A-111.2 Procedure A-ILL.21 Weigh accurately about 50 g of caustic soda sample in.a beaker and neutralize it with sulphuric “acid carefully after_ placing the beaker in cold water. Add 5 ml of the in excess and dilute to 250 mi. Transfer_the contents of the beaker to a 500 ml-conical flask add 25 ml of ferrous ammonium sulphate solution, close the flask with a bunsen valve and boil the contents gently for 15 minutes. Allow the flask to cool to room temperature. ‘After cooling, titrate the contents of the flask ‘with 0.02 NV potassium permanganate, solution slowly with stirring till a pink colour’ persists. Note the volume V AAL122 Runa blank by titrating 25 ml of ferrous ammonium sulphate containing 5 ml of sulphuric acid and 200 mt of water against 0,02 N potassium permanganate, proceeding in the same way as that of test. Note the volume as V1 AALL3 Calculation Chilorates ( as NaCl0s, ) ppm = (Yar Va) Nx 17-14>. 10" where ¥, = volume, in ml, of standard permanganate ‘solution Use lank; yotassium in the Vs — volume, in ml, of standard potassium permanganate Solution used in the test; N= normality of standard potassium per- ‘manganate solution; and M = mass, in g, of the material taken for the test. AAL2 Method B AAL20 Outline of the Method A little excess of ferrous sulphate added to a slightly acidified solution of caustic soda is oxidized quantitatively by the chlorate in caustic soda, The chlorate is estimated by back titrating the jexcess ferous ammonium sulphate with standard potassium dichromate solution, AAL2A Reagents 1.2.1.1 Ferrous ammonium sulphate—0.02N Dissolve 3.92 g of ferrous ammonium sulphate crystals in 300 ml of water. Add I ml of con- centrated sulphuric acid and dilute to 500 ml,IS 252: 1991 A-IL.2.1.2 Dilute sulphuric acid — 1:1 (v/v) AAI 1.3 Phosphoric acid— 1:1 (v/v), Ac112.14 Sodium diphenyl amine sulphonate solution — Dissolve 0.2 g of sodium diphenyl amine sulphonate in 100ml of water. A-112.15 Potassium dichromate solution — 0.02N." Powder finely about 2 g of potassium dichromate (AR grade ) and dry in an air oven at 140-150 C for one hour and cool in a desiccator. Accurately weigh 0.98 g of the dried potassium dichromate and dissolve in 1 000 ml of water ina volumetric flask. A-11.2.2 Procedure AcI122.1 Weigh accurately about 50_g of caustic soda in a 500 ml-beaker. Neutralize it with dilute sulphuric acid (I: ) carefully, keeping the beaker in cold water. Add an excess of 20 ml of dilute sulphuric acid. Transfer the contents of the beaker into a 500 ml conical flask. Pipette out 25 ml of ferrous ammonium sulphate solution into the flask, Close the flask with a Bunsen valve, boil the contents for 15 minutes and allow to cool to room temperature. After cooling, add 20 ml of phosphoric acid (1:1) and 0.5 ml Sodium diphenyl amine sulphonate solution into the flask. Titrate the solution with potassium dichromate solution to a violet colour. Note the volume as V>. AA122.2 Run a blank by titratin, ferrous ‘ammonium sulphate, 20 ml of dilute sulphuric acid, 20 ml_of phosphoric acid and 0.5 ml of sodium diphenyl amine sulphonate against potassium dichromate solution by proceeding in the same way as in the test, Note the volume as V1. A-11.23 Caleulation Chlorates (as NaClO; ), (A= Va) x Nx ITT4 x 108 ~ aM 25 ml of ppm wher ¥, = volume, in ml, of standard potassium chromate “solution used’ in the V2 = volume, in ml, of standard potassium dichromate solution used in the test N = normality of standard potassium dichromate solution; and ‘M = mass, ing, of the material taken for the test, 10 ‘AcI2 DETERMINATION INSOLUBLE IN WATER Ad12.1 Reagent OF MATTER A-12.1.1 Concentrated Hydrochloric Acid — See 1S 265:1987. A-12.2 Procedure Weigh accurately about 50 g of the material and transfer it into a 600-ml beaker, add 300 ml of water and stir until dissolved. Add concen- trated hydrochloric acid till the solution is just alkaline to phenolphthalein. Bring to boil ‘and allow the solution to settle on the hot- plate for 15 minutes. Filter through a weighed Gooch crucible or tared sintered glass crucible (G No, 4) and wash with hot water to tree it from alkali allowing water to drain completely after each washing. Dry it in an oven for one hour at 105 to 110°C, Cool it in a desiccator and weigh AcI2.3 Caleulation Matter insoluble in water, M, percent by mass = 100 57 where ‘M, = mass, in g, of the insoluble residue, and M = mass, in g, of the material taken for the test, Ac13 CALCULATION OF RESULTS ON THE DRY BASIS A-I3.1 For the purpose of this standard add the percentage of sodium hydroxide, carbonates, (as'NagCOs5, chlorides (as NaCl), sulphates (as NazSOq ) and silicates (as SiO; ) and treat the total as_the total dry solid content of the solution, On this basis calculate the content of the different components on the dry basis AAR Example AA3.LL1 If the total percentage of the determined components of a solutionis 50.4 and the percentage of sodium hydroxide content is 50.2, the percentage of sodium hydroxide on dry basis will be 502 x 100 _ go. 7 Again the above example, if the iron, content is.10 ppm, the content ‘ofiton on dry basis 100 10 x ra = 198 ppm.A13.1.1.2 If the total percentage of the deter- mined ‘components of the solid is 99.5 and the percentage of sodium hydroxide content is 99.1, the percentage of sodium hydroxide on IS 282: 1991 ary basis will be 99-1 x 100 te 996 ANNEX B ( Clause 7.1) SAMPLING OF CAUSTIC SODA, PURE AND TECHNICAL B-l GENERAL, SAMPLING Bel. Precautions shall be taken to protect the samples, the material being sampled, the sampling instrument and the containers for samples” from adventitious contamination, particularly from absorption of water and carbon dioxide. REQUIREMENTS OF B-l2 To draw a representative sample, the contents of each container selected from sampling shall be mixed thoroughly by suitable B13 The sample shall be placed in clean, dry and air-tight alkali resistant glass containers, B-l4 Each sample container shall be_ sealed airtight after filling, and marked with full ciails of sampling, the date’ of sampling. and the batch number. R2 SCALE OF SAMPUNG B21 Lot All the containers in a single consignment of the material drawn from “a single batch of manufacture shall constitute the lot, Tf a consignment is declared to. consist of different batches of manufacture, the batches shall be ‘marked separately and the groups of containers in each batch shall constitute separate lots. B22 Samples shall be tested from each lot separately for judging the conformity of the material to the specified requirements. The number of container (n) to de selected at random from lots of different sizes (V) shall be in accordance with Table 2. B23 The container shall be drawn at random from the lot, and to ensure randomness, the following procedure may be adopted; Arrange all the containers in the lot in a systemiatic manner, and starting from any i one, count them as 1,2... up tor, where r is the integral ‘part of Nin. Every rth container thus counted shall be included in the sample till the required number of containers specified in col 2 of Table 2 is taken out. Table 2 Number of Containers to be Selected for Sampling (Clause B22) ine ‘Number of Containers to be Selected N ” @ ste 50 3 sito 200 4 201 0400 5 401 to 650 6 SI t0 1 000 1 B3 TEST SAMPLES AND REFEREE, SAMPLE. B-3.1 Caustic Soda, Solid B43.11 Scrap off 50mm of the material from ‘the top centre and then take the sample, ‘The quantity of the material so drawn shall be not Tess than 200 g and the mass of the total mate- rial taken out shall not exceed 1 kg. The number of portions to be collected and the quantity of material taken from each portion may. be suitably reduced in of big containers to keep the size of the material taken out at 1 kg. Mix rapidly the material so collected from any particular container on a clean dry surface after scrapping off the surface carbonate that may be formed during sampling B-3.1.2 From each of the portions representing the Containers selected, take out 600 g and mix thoroughly the material collected. This shallIs 252 : 1991 constitute the composite sample. Divide this composite sample into three parts, transfer each part to a sample container which shall then be sealed air-tight with well-fitting corks coated with paraffin wax. B-3.1.3 The portion of the material left (after the quantity for the preparation of the composite sample has been taken out) in respect of each container shall also be divided into three parts Each such part shall constitute an_ individual test sample and shall be transferred to a sample container which shall then be closed as in B-3.1.2 and labeled giving full identification particulars, One of these three sets shall be marked for the purchaser, another for the supplier and the third for the referee B-3.2 Caustic Soda Lye B-3.2J From Tank Cars or Tank Wagons Draw samples from cach tank car or tank wagon fom different levels by means of a suitable sampling instrument, Mix the material so collected and transfer about 5 litres of it to a clean resistant glass bottle. Divide the mate rial into three parts and transfer each part to a sample container which shall then be closed as in B-3.1.2 and labelled giving full identifica lion particulars. Each such bottle shall consti- tute an individual sample; one of these shall he marked for the purchaser, another for the supplier and the third for the refere B-3.2.2 For Containers B-3.2.2.1 Draw representative portions from each container selected from sampling after thoroughly mixing the container; take out about 2 litres from each selected container. B-3.2.2.2 From cach of the portions represen- ting the selected containers, take out about 1200 ml and mix the material so obtained, This shall constitute the composite sample. Divide this composite sample into three parts, one for the purchaser, another for the supplier and the third for the referee. Transfer each part to a sample container which shall then. be closed as in B-3.1.2, B-3.2.3 The portion of the material ( after the quantity required for the preparation of the composite sample has been taken out) in respect of each container shall also be divided into three parts, Each such part shall constitute an individual sample and shall be transferred to sample container which shall then be closed as in B-3.1.2 and labelled giving full identifica tion particulars, One of these three sets shall be marked for the purchaser another for the supplier and the third for the referee. B-3.3 Referee Sample The referce sample (see B-3.1.2, B.3.1.3, B-3.2.1, B-3.2.2.2 and B-3.2.3 ) shall bear the names of the purchaser and. the supplier and shall be used in case ofa dispute between the two. It shall be kept at a place agreed to between the purchaser and the supplier. B44 NUMBER OF TESTS Ba.1 For Tank Car or Tank Wagons Tests for all the characteristics prescribed in 4.3 shall be carried out on the individual samples, B-42 For Containers B-4.2.1 Tests for the delermination of iron shall be conducted on each of the individual samples, B-4.2.2 Tests for the remaining characteristics prescribed in 4.3 shall be conducted on the composite sample, BS CRITERIA FOR CONFORMITY B-S.1 For Tonk Cars or Tank Wagons ‘The tank car or tank wagon shall be declared: as conforming to the specification if the indivi- dual sample” satisfies all the requirements prescribed B-S.2 For Containers BS. The lot shall be considered conforming to the requirement for iron if each of the individual samples satisfies the tests in A-8, 1 For tron B-S.2.2 For Composite Sample The test results on the composite sample shall meet the specified requirementsBureau of Indian Standards BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote harmonious development of the activities of standardization, marking and quality certification of goods and attending to connected matters in the county. Copyright BIS has the copyright of all its publications. No part of these publications may be reproduced in any form without the prior permission in writing of BIS, This does not preclude the free use, in course of implementing, the standard, of necessary details, such as symbols and sizes, type or grade designations. 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