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Bs 1014 1975

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7 BS 1014 : 1975 iy eee se Specification for 9d Pigments for Portland cement and Portland cement products British Standards Institution ‘This Beith Standard, Raving besa approved by the Pmenis, Pins and Vannes Industry Standards Comite, was published under the authority of the Heute hardin 29 August 1975 © Writish Standards tostitution, 1975 rst published Apsil 1942 fevision Apa 1961 Second revision August 1975, ISHN: 0 50 OHS 9 Copyright Users of British Standards are reminded that copyright subsists in all SI publications. No part of this publication may be ‘eroded in any form without the prior permission ia writing oF BSI. This does not preclude the fee wwe in the course of Implementing the standard, of ncrssary details such as symbols and size, type or grade designations, Enguiies should Be addressed to the BSI Sceretariat. Contract requirements Auention is drawn to the fact that tis British Standard does not purport o include all the necessary provisions of a coatract. Revision of British Standards In oder to keep abreast of progress in the industries concerned, Britis Standards are subjetto periodical review, Sugerstions {or improvements will be recorded and in due course brought to the nti of tae committees cbarued with the tvisen oft standards to which they rele, British Standards are revised, when necesary. by the issue either of amendment slips or of revised editions ts important that ‘srs of British Standards should ascertain tha they are in pessession ofthe latest amendments or edions all aformacon os ail £81 publications, numbering over 9000 wil be found in the BST Catalogue. This information is supplemented by details published ‘eich month in 8/ News of new publications, revisions nd amendments, ‘BSI Nes is avilile to Subscribing Members of the Institution. All other publications may be purchased direct fom Sales Department. Enquiries concerning subseribing membership, which bas considerable advantages, willbe welcomed, and should Se made to Subsritions Department. Both departments ae located at Linford Wood, Milion Keynes MK14 6LE (Telephone 0908 220022; Telex 825777). The flowing BSI reference relate the work on this standard Committe ference PVC/I/2 Draft for comment 72/30536 DC Co-operating organizations ‘hs Mements, Paints and Varnishes Industry Standards Committe, under whose supervision this British Standacd was preparsd, ‘consists of representatives from the following Goverement sopartments id smtife ad industri ongansatone tush ¢ Asvciation “Oil and Colour Chemists’ Asiacition Department ofthe eavironment Paigt Rewsreh Asscistion *Defarinent or the Environment, Building Research =Paintmakers Assocation of Great Britain Limited Felaiient, Post Once Depron of Indastey Royal lnsttue of batish Architects Depactnent of Indust, Laboratory of the Royal Instat of Publi Health and Hygiene ‘Govecnent Chen Society of Chemical Industry Greater Landon Count ‘Titanium Pigment Monufacttrers Technical stare ot Carrnin Telnalony Comte Usndon Transport Hoenn *White Lead Manufacturer Association Ministry af eters ‘Zine Development Association Natoma Federation of Yad’ and Phamber “Zine Piment Development Association Meri "he Government deparinints snd sient nd indus organizations marked with an asters i the above lt, togethor with Ihe follwing. wore dicetly reprexcnied on the counts entasted with te preparation of thi itsh Standen BatshPrect Console Concrete Sacity eaten and Concrete Associaton oiniless Flooring Assocation (Coment Mokere Panel of Independent Consatants ‘Chenel insti Association B008-6—0.24-8 S| BS 1014 : 1975 ES. Specification for Pigments for Portland cement and Portland cement products Amendments issued since publication Amd. No. Date of issue | Text affected British Standards Institution 2 Park Street - London W1A 2BS Telephone 01-629 9000 Tolex 268993 BS 1014: 1975 Contents Page Inside front cover Cooperating organizations 2 Foreword Specification Scope References Sampling Agreed sample 5. Description Composition Required characteristies Effect of pigment on Portland cement products 9. Packaging 3 Appendices ‘A. Method for the determination of chromium ‘compounds content, expressed as Crz03 6 B. Method for the determination of iron ‘compounds content, expressed us Fe; Oy 6 Foreword ‘This British Standard provides specifications for a ‘ange of pigments suitable for the colouring of Portland cement and Portland cement produets. The Pigments specified may also be suitable for use with ‘other hydraulic cements but the use of the pigments in these vements has not been covered in this British ‘Standard because experience in the use of these ‘cements with pigments is limited. The pigments specified ure manufuctured efther synthetically or from naturally oceurring mineral ores ‘This revision differs from the 1961 edition with regurd to the following matters: (a) owing to the decline of the magnesium oxy- cloride flooring trade, reference to the use of the pigments in this material has been replaced by feference to their usage in mortar compositions and ceinent products generally: (b) because information on the previse content of ‘metal oxide ina pigment is not necessarily # guide to its tinting stiength or hue, itis, therefore, per mitted that materials with metal oxide contents ‘outside those specified may be supplied by agree- ‘ment between the contracting parties (©) the section covering brown iron-manganese oxide pigments has been widened to include the ‘how aanganese brown iron oxide pigments; Page . Method for the determination of titanium dioxide content, expressed as TiO, 7 . Method of tes for the comparison of colour and staining power 9 E. Method of test for effect on the setting times of Portland cement 10 F. Method of test for effect on the strength evelopment of Portland cement products 10 G. Notes on pigment dispersions 10 H. Notes on incorporation of pigments " Tables 1. Required characteristics 4 2. Methods and masses of pigment to be used 9 Figure 1. Nakazono reductor for determination of titanium dioxide content 7 (@) the section relating to zine sulphide pigments hhas been excluded because their use with cement nas ceased to be significant; () the section relating to mineral black pigments hhas boen deleted because these pigments are no longer available; (D) neve clauses relating to phthalocyanine pigments, blended pigments, and pigment dispersions have been introduced; notes on pigment dispersions are siven in appendix G; (® the chemical methods of testing have been ‘revised and where possible are identical with those in the specifications already published for pigments for paint; (a) appendices ae included for the first time to cover respectively 2 comparative test for effect on the setting times of Portland cement and a com- parative test for effect on the strength development of Portland cement; notes on the incorporation of pigments in Portland cement and Portland cement products are given in appendix H. QO BS 1014 : 1975 ee British Standard Specification for Pigments for Portland cement and Portland cement products —— 1. Scope This British Standard specifies the requirements for pigments for colouring Portland cement and Portland ‘cement products NOTE 1. [eis chought that plement found wuiable for Portland cement wil algo be suiable for supersiphate and big alumina cements bat thei wages for sich porpote e ‘not coveted by this standard because of the limited experience in the us of pizments with those coments should net be Inferred, however, tat the pigments specified in this standard not be satisfactorily used with coments ther than land coment. should be noted that certain cadmium pigments, Pe NOTE 2. cobalt bue pigments and titan complex pigments ae sso suitable for use wih Portland cement but bocaute oftheir ost they wre generally not used for thie purpose, 2, References ‘The titles of the British Standards referred to in this standard are listed on the inside back cover. 3. Sainpling For the purpose of testing a pigment in accordance with this standard, a sample of not less than 100 g shall be taken and packed according to the method described in BS 4726, 4, Agreed sample ‘The agreed semple referred to in table 1 and appen- dix D shall be one and the same and shall comply in all respects with the other relevant requirements of this standard. The sample shall be packed in the ‘manner described in BS 4726 and shall be not less than 100 g. 5. Description 5.1 Powders. The pigment shall be in the form of dry. soft powder or in such a condition that it may be readily reduced thereto by crushing it under a palette knife without any grinding action being necessary. 5.2 Dispersions. By agreement between the contract- ing parties the pigment may be inthe form of a slow settling suspension of the pigment in water. Any dis- persion which settles in storage shall be readily re-dispersable by simple stirring or shaking, 6. Composition ‘The pigment shall consist essentially ofthe chemical ‘compound or compounds shown in table | and shall ‘ot contain compounds or other impurities, such at Jead or zinc compounds, capable of affecting adversely the setting and development of strength of Portland cement. By agreement between the contracting parties, limits for metal oxide content ather than those given in table 1 may be specified 7. Required characteristics ‘The pigment shall have the characteristics and require: ‘ments specified in the appropriate column of table 1 8. Effect of pigment on Portland cement products, 8.1 Setting time. The pigment, when used in the maximum proportions recommended by the manufac- turer, shall not be regarded as significantly affecting the setting time of Portland cement products if, when. tested in accordance with appendix E, the inital set- ting time isnot les than 45 mia, the final setting time ‘not move than 10 hand the difference for both setting times between the mixes with and without added pigment not more than 36 min, 8.2 Strength development. The pigment, when used in the maximum proportions recommended by the ‘manufacturer shall not be regarded as significantly affecting the strength development of Portland cement Products if, when tested in accordance with appen- dix F, the mean compressive strength of the mix containing the pigment does not differ by moze than 20 % from the mean compressive strength of the mix without pigment 9. Packaging Al packages containing the material shall be clearly ‘marked with the number of this British Standard, BS 1014 :1975 1 3 06 Fou | 246s sane sn $86 seu zoo | wu eso pony BL | 28a oemeue “90 Sots | at i fod! tram ono aot sxcunsttuou z01 FORE] ons un spso say nwa 0% Pouon sot | i ag foes oon wa 0b Soy seep] opremey | wma eg sew st a0 | optus pose _ on nus see 54 Poa | ropuon au) ogi sot Epon 1 snousioue ] “a 08 totes em wnat rer toes ea smu 20 seu yore epowaN | pouen | -puode sg mpleday t26e | aprv0 won po TUTTE zor uw x56 | use p10 sous 50 epomen | poMAW | pasties y upubdsy to 2ruasy | a Doma: cares suomednp 104 | smpKod oa 19130 power noun 21810 po ei (¢arou sep men Susuannbeg [SARE 70 tp wood agnor oe sopseroeieyo pauinbay “| aigey BS 1014 : 1975 ey suo ka 2 ‘puns si Jo swusuayn 1b 00g Ar |. cae Men OT | yds paste | on opus | ony seu B07 seu gor, epomsn | zpomen on suuesooreniga oO oS : BS 1014 : 1975 Appendix A Method for the determination of chromium compounds content, expressed as Crs, AL Apparatus. The following apparatus is required. Ad Zirconium orci, 60 A.L.2 Onemark volumetric flak, 500 mi, complying ‘withthe requirements of BS 1793, ALS Meker or Teo burner. A2 Reagents. The reagents ued shal be of recog ved analytical reagent quality, Distilled water of vnior of equal purity complying with the require ments of BS 3978 shall be used A2A Sodium peraxile, 22 Sulphuricorthophosphoric acid mixture. Mix three parts by volume ofa 50 % (fs) sulphuce acid solution with one pat by volume of orthophosphorc acid (2 1.75). 2.3 Ammonium ferrous sulphate solution. Dissolve 80 of FeSO4(NI,), 80 6th O in water containing 50 ml of $0 (9) sulphorie acid and make ap to 1000 ml with wat A.24 Potassium dicnomate solition, Dissolve 9.8715 gof KyCraOy in water and make up to 1000 ra with water A2S Barium diphenylamincsulphonate indicator. Dissolve Ig ofthe solid n 100 mi of sulphuric add = 18, AA3 Procedure. Weigh. tothe nearest milligram, about 2.9 g of the pigment previously dried at 105 °C into tho siren eruible containing about 7 fof the souiun peroxide and then adds Further similar quan- tity of the latter. Mix the two components thoroughly ‘witha hss rod and then brush any adhering partes fn the fod back into the erucible Heat the erucble in the flame of a Meker of Telu burner and maintain the contents ina molten sate fr I min with constant swing of the melt. Allow to cool for 2 min, then nmerse the hot erie in about 250 ml of water in 31400 ol beaker snd iomedistely cove the bear wth watchs. Gently wace the beaker and con tents until vigorous reation ceases, then remo the eeibieand wish any soltion back into the beaker. Gover the beakee witha watlvgass and boi! the contents of te beaker fr 10 mi Filler through an epen-textured filter paper an wish the fier thoroughly with hot water Cool the flats transfor it to the 800 ml one-mark volumetric flask and makeup to the mack with water Pipette 50 lof this solution into» 500 ml conte! flask Dilute this sap to 100 ml, bol for 20 min and ‘hen coo, Dilute to about 250 mi, aif with 30 ml ofthe sulphucisthophosphorie aed mixture, coo! toa temperature between 10 °C and 15 °C and add by means of a pipette 50 ml of the ammonium ferrous sulphate solution; then add 15 to 20 drops of the barium diphenylarsinesulphonate indicator an titrate with the potasium dichromate solution to purple ‘end: point lstng at lest 30 s,Carty outs blank determination using a 30 l portion of the ammonium fercous sulphate solution using the same conditions without the addition ofthe chromium oxide sample ‘Ad Caleulation of Cras. Calculate the chromium compounds content, expressed as Crg0y 28a percent- age by mass, by meats ofthe formula Gan) sin =") where V1 isthe volume, in miliitres, of the potassium dichromate solution required for titration of the sample, ¥ isthe volume, in millilitres, of the potassium dichromate solution required for the blank, and ‘mis the mass, in grams, of sample taken, Appendix B ‘Method for the determination of iron ‘compounds content expressed as Fe, 0; B.1 Apparatus. The following apparatus is required, Platinum erucible, B.2 Reagents, The reagents used shall be of a recog: nized analytical reagent quality. Distilled weter or Water of equal purity complying with the requice- ‘ments of BS 3978 shall be used. B21 Hydrochloric acid, d= 1.18. B.2.2 Sulphuric acid, 50 % (m/m) solution. 8.2.3 Potassium hydrogen sulphate. B.24 Stannous chioride solution, feeshly prepared by dissolving 60 g of SnCl,2H, 0 in 500 ml of hydro- ‘chtoric acid (@= 1.18) and diluting to 1000 ml with water. B28 Mercurie chloride solution, saturated. B26 Orthophosphorie acid|sulphurie acid mixture, prepared by mixing 310 ml of sulphuric acid (a= 1.84), 250 ml of orthophosphoric aid, HPO, (@= 1.74) and 440 mal of water. B.2.7 Barium diphenyleminesulphonate indicator, prepared by dissolving 04 g of solid reagent in 100 ml ‘of water and filtering, B28 Potassium dichromate, 0.1 solution. * Zirconium ccaibles say be obtained from Imperkl tals Hndusres Lid, Birmingharn, Aleratively, «leet orale erable ty be un ble iter paper iva Whatman No, 54 ta 8.3 Procedure. Weigh, to the nearest miligram, 0.3 g 10044 gof the pigment dried at 105 °C and transfer {to a 500 mi conical flask. Add 25 ml of the hydro- chloric acid and heat the mixture until solution is effected. If the material is difficult to dissolve add 10 ml ofthe 50 % sulphuric acid to assist solution. Filter off any coloured siliceous residue, ignite in the platinum crucible and fuse with the potassium hydrogen sulphate, Extract the melt with water con- taining a litte hydrochloric acid, keeping the total volume as small as possible and add to the main solution, Bring the solution to the boil and, keeping the solution hot, add the stannous chloride solution drop by drop until the solution is colourless. Then add a further two drops. NOTE. Ii important that only x very light excess of stannous chloride solution shouldbe added ony alight Sky white precipitate should be obtained winen the mercuric horide solution is rubsequontly added I's hemvy precipita af erey ov blk colou i obtained, too much stannous thlride has been add and the determination shoud be ‘repeated from the beginning. Cool the solution rapidly to room temperature and add 5 ml of the mercuric chloride solution. Mix thoroughly and wash down the sides ofthe flask with. cold water. Allow the solution to stand for about {min and add 40 ml of the orthophosphoric acid/ sulphuric acid mixture. Dilute the solution to between 100 ml to 200 mi, according to the amount of iron present. ‘Add 0.2m to 0.4 ml of the barium diphenylamine- sulphonate indicator and titrate with the O.1N potassium dichromate solution until the solution begins to darken, Complete the titration by adding the 0.1N potassium dichromate solution diop by

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