इंटरनेट मानक 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. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 44 (1991): Iron Oxide Pigments for Paints [CHD 20: Paints, Varnishes and Related Products] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 44 : 1991 (Reaffirmed - 2012) Indian Standard IRON OXIDE PIGMENTS FOR PAINTS — SPECIFICATION ( Second Revision ) First Reprint MARCH 2000 UDC 667.6221 : 661.872.2 © BIS 1991 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 December 1991 Price Group 5 Raw Materials for Paint Industry Sectional Committee, CHD 021 FOREWORD This Indian Standard ( Second Revision ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Raw Materials for Paint Industry Sectional Committee had been approved by the Chemical Division Council. The standards IS 44 : 1950 'Specification for black oxide of iron for paints', IS 45 : 1950 'Specification for manufactured red oxide of iron for paints', IS 46 : 1950 'Specification for natural red oxide of iron for paints', IS 47 : 1950 'Specification for ochre for paints', IS 48 : 1950 'Specification for natural sienna ( raw and burnt ) for paints' and IS 49 : 1950 'Specification for natural umber ( raw and burnt ) for paints' were first issued in 1950. These were based on the interim co-ordinated drafts produced with the assistance of the representatives of manufacturers and of various departments, and authorities of the Government of India by the Coordinating Subcommittee of No. 5 Standing Committee on specification for paints and allied stores of the General Headquarters, India ( now Army Headquarters ). In 1969, all the above standards were amalgamated into IS 44 : 1969 'Specification for iron oxide pigments for paints ( first revision )'. The revised specification stipulated requirements for 6 classes of the material corresponding to the materials covered in the earlier set of six standards ( IS 44 — IS 49 ). The requirement for sulphur and sulphur compounds for class 2 material ( manufactured red oxide ) was made more stringent. Besides, requirements for volatile matter and water soluble matter had been modi fied and unified for class 3 to 6. The method of determination of carbonates as carbon dioxide was also modified. New requirements for limits for ferrous iron and calcium compounds were also introduced for class 2 material. Limits for manganese content had also been fixed for classes 5 and 6. The standard had also been aligned with IND/ME 38 (a) 'Red oxide of iron, dry, lead-free' issued by the Department of Standardization, Ministry of Defence, Government of India. In this second revision, classes have been designated as grades. Requirements for in additional grade, namely, iron oxide yellow, have been added. Requirements for total iron ( as Fe O ) for the Grades 2, 3 2 3 and 4; volatile matter for Grade 4 and matter soluble in water for Grade 1 have been modified. Three new requirements (a) sum of water soluble chloride and sulphate, (b) pH of aqueous extract, and (c) loss on ignition have been added. The requirements for sulphur and compounds of sulphur have been deleted. In preparing this standard, assistance has been derived from the following standards: 1) ISO 1248-1974 'Iron oxide pigments for paints', issued by International Organization for Standardization ( ISO ) 2) ASTM D 768-81 'Standard specification for yellow iron oxide hydrated', issued by American Society for Testing and Materials ( ASTM ) 3) ASTM D 769-81 'Standard specification for black synthetic iron oxide', issued by American Society for Testing and Materials ( ASTM ) 4) ASTM D 3721-78 'Standard specification for synthetic iron oxide pigments', issued by American Society for Testing and Materials ( ASTM ) 5) ASTM D 3722-82 'Standard specification for natural red and brown iron oxide pigments', issued by American Society for Testing and Materials ( ASTM ) 6) ASTM D 3724-82 'Standard specification for synthetic brown iron oxide pigments', issued by American Society for Testing and Materials ( ASTM ) 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 accodance 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 SEPTEMBER 2000 TO IS 44 : 1991 IRON OXIDE PIGMENTS FOR PAINTS — SPECIFICATION ( Second Revision ) ( Para 2, Table 1, col 11 ) — Substitute 'Ref to Cl No. in IS 33 : 1992' for 'Ref to Cl No. in IS 33 : 1991'. [ Page 2, Table 1, Sl No. (iii) ] — Substitute '± 10% of approved sample' for '± 10 of approved sample'. [ Page 2, Table 1, Sl No. (iv)(a), col 11 ] — Substitute '11' for '—'. [ Page 2, Table 1, Sl No. (iv)(b), col 11 ]— Substitute '11' for '—'. ( CHD 21 ) Reprography Unit, BIS, New Delhi, India IS 44 : 1991 Indian Standard IRON OXIDE PIGMENTS FOR PAINTS — SPECIFICATION ( Second Revision ) 1 SCOPE 4.2.2 Grade 5 and 6 material shall have two types: This standard prescribes requirements and Type C — Raw methods of sampling and test for natural and synthetic iron oxide pigments. Type D — Burnt 2 REFERENCES 5 REQUIREMENTS 5.1 Composition The Indian Standards listed below are the neces sary adjuncts to this standard: 5.1.1 Grade 1 IS No. Title The material shall be synthetic ferro-ferric oxide 33 : 1991 Methods of sampling and test and shall be free from added colouring matter for inorganic pigments and and water soluble iron salts. The colour shall be extenders for paint ( third entirely due to inorganic iron compounds. revision ) 5.1.2 Grade 2 1070 : 1977 Water for general laboratory use ( second revision ) The material shall consist of wholly manufactured oxide of iron and shall be free from added colour 1303 : 1983 Glossary of terms relating to ing matter and water soluble iron salts. The paints ( second revision ) colour shall be entirely due to inorganic com 2263 : 1979 Methods of preparation of pounds of iron. indicator solution ( first revision ) 5.1.3 Grade 3 2316 : 1968 Methods of preparation of standard solutions for colori- The material shall be a natural product, the metric and volumetric analysis colour of which shall be entirely due to inorganic ( first revision ) compounds of iron. 3 TERMINOLOGY 5.1.4 Grade 4 For the purpose of this standard, definitions given The material shall be a naturally available under 2 of IS 33 : 1991 and IS 1303 : 1983 shall hydrated oxide of iron. It shall be free from added apply. colouring matter and impurities. The colour shall be entirely due to inorganic compounds of iron. 4 GRADES AND TYPES 5.1.5 Grade 5 and Grade 6 4.1 Grades 5.1.5.1 Type (C) material shall be a hydrated There shall be seven grades of material, namely, oxide of iron together with the manganese salt Grade 1 Black oxide, that is naturally associated with it. The colour of Grade 2 Synthetic red oxide, the material shall be entirely due to inorganic compounds of iron and shall contain no organic Grade 3 Natural red oxide, colouring matter. Grade 4 Ochre, 5.1.5.2 Type (D) material shall be produced by Grade 5 Natural sienna, calcination of type (c) and shall be free from Grade 6 Natural umber, and admixture of any other substance. Grade 7 Synthetic iron oxide yellow hydrated. 5.1.6 Grade 7 4.2 Types The material shall consist of synthetic oxide of iron by chemical reaction and shall be free from 4.2.1 Grade 4 shall have two types: salts. The colour shall be entirely due to inorganic Type A — Red compounds of iron and shall be free from admix Type B — Yellow ture of any other substance. 1 IS 44 : 1991 5.2 Form and Condition 6 TEST METHODS The material shall be supplied in the form of dry 6.1 Quality of Reagents powder or in such a condition that it may be Unless specified otherwise, pure chemicals and reduced to powder form by crushing, without distilled water ( see IS 1070 :1977 ) shall be em grinding action, under palette knife. ployed for tests. 5.3 All grades and types of the material shall conform to the requirements given in Table 1. NOTE – 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the results of analysis. 5.4 Lead Free Material When lead free material is required, it shall not 7 PACKING AND MARKING contain more than 0.03 percent of lead or com 7.1 Packing pounds of lead or a mixture of both, calculated as metallic lead ( Pb ), when tested as prescribed The material shall be suitably packed as agreed under 25 of IS 33 : 1991. to between the purchaser and the supplier. Table 1 Requirement for Iron Oxide Pigment for Paints ( Clause 5.3 ) Sl No. Characteristic Requirements for Grade Method of Test 1 2 3 4 5 6 7 Annex Ref to Cl No. in IS 33 : 1991 (1) (2) (3) (4) (5) (6) (7) (8) (9) (10) (11) i) Volatile matter, percent 2.5 0.5 0.5 1.0 0.5 0.5 1.0 — 7 by mass, Max ii) Residue on sieve, per 0.5 0.5 0.5 0.5 0.5 0.5 0.5 — 8 cent by mass, Max iii) Oil absorption — 9 iv) Colour a) Staining power — — b) Undertone — Close match to the approved sample — — — v) Matter soluble in water, 1.0 0.5 0.5 0.5 0.5 0.5 0.3 — 17 percent by mass, Max vi) Sum of water soluble – 0.1 — – – – 0.1 A – chloride and sulphate expressed as Cl and SO, 4 percent by mass, Max vii) Acidity ( as H2SO4 ) or 0.1 0.1 0.1 0.1 0.1 0.1 0.1 — 18 alkalinity ( as NaOH ), percent by mass, Max viii) pH of aqueous extract — Within ± 1 of approved sample — — ix) Total iron ( as Fe2O3 ), 79 94 80 45 — — 83 B — percent by mass, Min – – – – x) Ferrous iron ( as FeO ), 20 1.5 — C — percent by mass, Min Max xi) Carbonates ( as CO2 ), 0.5 — — — — 0.5 — D — percent by mass, Max xii) Calcium compounds ( as — 2.25 — 5.0 2.5 2.5 — E — CaO ), percent by mass, Max xiii) Manganese content ( as — — — — 1 15 — F — MnO ), percent by mass, 2 Max xiv) Loss on ignition, percent – – – – – 13 G — by mass, Max 2 IS 44 : 1991 e) Batch No. or Lot No. in code or otherwise; 7.2 Marking and 7.2.1 The containers shall be marked with the f) Month and year of manufacture. following information: 7.2.2 The containers may also be marked with the a) Name of the material; Standard Mark. b) Grade and type of the material; 8 SAMPLING c) Indication of the source of manufacture; 8.1 Representative samples of the material shall d) Net mass of the material; be drawn as prescribed under 4 of IS 33 : 1991. ANNEX A [ Table 1, Sl No. (vi) ] DETERMINATION OF WATER SOLUBLE CHLORIDE AND SULPHATE A-0 PREPARATION OF AQUEOUS Ignite it gently, and then at red heat. Cool it in a EXTRACT desiccator and weigh to the nearest 1 mg. Weigh about 5 g of pigment in a beaker. Add A-1.3 Calculation 200 ml of water and stir and boil for 5 minutes. Cool rapidly to room temperature and transfer to Calculate the water soluble sulphate content 250 ml volumetric flask and dilute to mark with ( as SO4 ) percentage by mass, as given below: water. Mix thoroughly by shaking and inver Water soluble sulphate sion. Filter it through filter paper and preserve content, percent by mass = the solution for determination of sulphate and chloride. where A-1 DETERMINATION OF SULPHATE M = mass in g, of barium sulphate precipi 1 tate; and A-1.0 Outline of Method M = mass in g, of pigment in the aliquot. 2 The solution is heated and barium chloride is added to the solution. The barium sulphate preci Report the result in two decimal places. pitate, thus obtained, is dried and weighed. A-2 DETERMINATION OF CHLORIDE A-1.1 Reagents A-2.0 General A-1.1.1 Hydrochloric Acid — concentrated. A-2.0.1 Outline of the Method A-1.1.2 Barium Chloride Solution — 5 percent. Weigh about 25 g of barium chloride into a The aqueous extract is titrated with silver nitrate beaker. Add about 200 ml of water and stir and solution using potassium chromate solution as boil for 5 minutes. Cool to room temperature and indicator. transfer to 500-ml volumetric flask and dilute to A-2.1 Reagents mark with water. Mix thoroughly by shaking and inversion. A-2.1.1 Silver Nitrate Solution — 0.01 N ( see IS 2316 : 1968 ). A-1.2 Procedure A-2.1.2 Potassium Chromate Solution — 5 percent. Take 50 ml of the clear aqueous extract obtained A-2.2 Procedure in A-1.0, in a beaker, acidify with 3 ml of the hydrochloric acid and boil the solution vigorously, Take 50 ml of the clear aqueous extract obtained taking care to avoid loss of solution by splashing. in A-0, in a beaker and add 1 ml of 5 percent Add 5 percent barium chloride solution drop by potassium chromate solution. Titrate with 0.01 N drop, to the hot solution until in slight excess, and silver nitrate solution, slowly and with vigorous allow the solution to stand overnight. Decant the shaking, until a faint reddish brown colour per supernatant liquid through a tared sintered cruci sists. Carry out a blank determination by adding ble ( P 10 or P 16 ). Wash it free from chlori de. 1 ml of 5 percent potassium chromate solution to 3 IS 44 : 1991 50 ml of water and titrate with silver nitrate V = the volume, in millilitres of 0.01 N silver 2 solution until the colour matches to that of the nitrate solution required for the blank previous titration making due allowance for any determination; and opalescence or turbidity. M = the mass in g, of pigment in the ali NOTE — Alternatively the end point of the titration quot. may be determined by potentiometric indication. A-2.3 Calculation Report the result in two decimal places. Calculate the water soluble chloride content expressed as Cl, percentage by mass, as given A-3 SUM OF WATER SOLUBLE CHLORIDE below: AND SULPHATE Water soluble chloride Add the water soluble sulphate content and content, percent by mass = 0.177 5 × chloride content, percent by mass Sum of water Water soluble Water soluble where soluble chloride = sulphate, per- + chloride, per- V = the volume, in millilitres of 0.01 N silver and sulphates, cent by mass cent by mass 1 nitrate solution required by the test percent by portion; mass ANNEX B [ Table 1, Sl No. (ix) ] DETERMINATION OF TOTAL IRON B-0 GENERAL B-1.1.5 Potassium Ferricyanide Indicator — ( see IS 2263 : 1962 ). Two methods of determination, Method 1 — ex ternal indicator method and Method 2 — internal B-1.2 Procedure indicator method; have been prescribed In case of dispute, Method 1 shall be used. B-1.2.1 Weigh accurately 0.25 to 0.40 g of the material, dried as prescribed under 6 of IS 33 : B-1 METHOD 1 — EXTERNAL INDICATOR 1990 and transfer to a 500-ml conical flask. Add METHOD 25 ml of the hydrochloric acid and warm gently until clear solution is obtained. The addition of a B-1.0 Outline of the Method few drops of stannous chloride solution after The ferric iron is reduced to ferrous state by adding the acid gently assists dissolution of iron. stannous chloride and solution titrated against If the solution of the sample is still not clear, standard potassium dichromate solution using digest the solution on a hot-plate, a evaporate to potassium ferricyanide as external indicator. dryness and redissolve in hydrochloric acid as above. Filter into a long necked flask and dilute B-1.1 Reagents the solution to about 50 ml. Bring the solution to boil and keeping the solution hot, add stannous B-1.1.1 Hydrochloric Acid — concentrated. chloride solution in drops until the solution is B-1.1.2 Standard Potassium Dichromate Solution — colourless. It is best to keep a watch-glass on the 0.1 N ( see IS 2316 : 1963 ). flask while adding the stannous chloride solution with agitation of the hot solution after each addi B-1.1.3 Stannous Chloride Solution tion. If too much stannous chloride is added by mistake, add potassium permanganate to the Dissolve by heating 60 g of pure stannous chloride solution until a yellow colour appears, then adding in a mixture of 400 ml of concentrated hydro one or two drops in excess. chloric acid and 600 ml of water until the solution is complete. Cool, add a few pieces of granulated NOTE — Only a very slight excess of stannous chloride tin and preserve the solution in an air-tight solution should be added to form a slight silky white amber-coloured bottle to prevent oxidation. precipitate with mercuric chloride solution added sub- sequently. Reduction should be repeated if a black or B-1.1.4 Mercuric Chloride Solution — saturated. grey precipitate is obtained. 4