BS-1851-1978 ISO-591-1977.pdf

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1、BRITISH STANDARD BS 1851:1978 ISO 591:1977 Specification for Titanium dioxide pigments for paints UDC 667.622.11 120.2:661.882.22 14 Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 This British Standard, having been prepared und

2、er the direction of the Pigments, Paints and Varnishes Standards Committee, was published under the authority of the Executive Board on 30 June 1978 BSI 07-1999 First published March 1952 First revision (in conjunction with BS 239, BS 254, BS 296, BS 338 and BS 637) April 1967 Second revision June 1

3、978 The following BSI references relate to the work on this standard: Committee reference PVC/1 Draft for comment 75/52133 DC ISBN 0 580 10197 5 Cooperating organizations The Pigments, Paints and Varnishes Standards Committee, under whose direction this British Standard was prepared, consists of rep

4、resentatives from the following Government departments and scientific and industrial organizations: British Colour Makers Association* Department of Industry, Chemicals and Textiles Division Department of Industry, Laboratory of the Government Chemist Department of the Environment, Building Research

5、 Establishment Department of the Environment (PSA) Institution of Corrosion Technology London Transport Executive Ministry of Defence* National Federation of Builders and Plumbers Merchants Oil and Colour Chemists Association* Paint Research Association Paintmakers Association of Great Britain Ltd.*

6、 Post Office Royal Institute of British Architects Society of Chemical Industry Titanium Pigment Manufacturers Technical Committee* White Lead Manufacturers Association* Zinc Development Association* Zinc Pigment Development Association* The organizations marked with an asterisk in the above list, t

7、ogether with the following, were directly represented on the committee entrusted with the preparation of this British Standard: Amalgamated Society of Painters and Decorators Chemical Industries Association Paint Manufacturers and Allied Trades Association Amendments issued since publication Amd. No

8、.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 BSI 07-1999i Contents Page Cooperating organizationsInside front cover National forewordii 1Scope and field of application1 2References1 3Description1 4Class

9、ification1 5Required characteristics and their tolerances1 6Sampling1 7Determination of titanium dioxide content1 8Test report3 Figure Nakazono reductor3 Table Required characteristics2 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:0

10、0 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 ii BSI 07-1999 National foreword This British Standard has been prepared under the direction of the Pigments, Paints and Varnishes Standards Committee. It was first published in 1952 and revised in 1967 in conjunction with BS 239, BS 254, BS 296, BS 33

11、8 and BS 637. It is identical with ISO 591:1977 “Titanium dioxide pigments for paints”, which was prepared by Technical Committee 35, Paints and varnishes, of the International Organization for Standardization (ISO), with the active participation and approval of the United Kingdom. Terminology and c

12、onventions. The text of the international standard has been approved as suitable for publication, without deviation, as a British Standard. Some terminology and certain conventions are not identical with those used in British Standards; attention is especially drawn to the following. Wherever the wo

13、rds “International Standard” appear, referring to this standard, they should be interpreted as “British Standard”. The comma has been used throughout as a decimal marker. In British Standards it is current practice to use a full point on the baseline as a decimal marker. Cross references. The follow

14、ing international standards are referred to in the text, and for each there is a corresponding British Standard; these are as listed below: Additional information. The Table in this standard defines certain of the required characteristics by comparison with an agreed sample. This term, which is not

15、defined in the international standard, is applied to a material agreed upon by the interested parties for use as a reference standard. Each agreed sample as mentioned in the Table should be one and the same material; it should comply with all the requirements specified for the pigment under test. Wa

16、ter. Water complying with the requirements of 7.2 is specified in BS 3978:1966 “Water for laboratory use”. NOTETextual error. When adopting the text of the international standard, the printing error given below was noticed. It has been corrected in this British Standard and has been reported to Tech

17、nical Committee 35, Paints and varnishes, of the International Organization for Standardization (ISO) in a proposal to amend the text of the international standard. Note * * below the Table on page 2: “. Parts I and VII .” is deleted and replaced by “. Parts I and XVII .”. International standardCorr

18、esponding British Standard BS 3483:1974 Methods of testing pigments for paints ISO/R 787-I:1968Part A1 Comparison of colour (Technically equivalent) ISO/R 787-II:1968Part B6 Determination of matter volatile at 105 C (Technically equivalent) ISO/R 787-III:1968Part C1 Determination of matter soluble i

19、n water (hot extraction method) (Technically equivalent) ISO/R 787-V:1968Part B7 Determination of oil absorption value (Technically equivalent) ISO/R 787-IX:1970Part C4 Determination of pH value of an aqueous suspension (Technically equivalent) ISO 787-XIV:1973Part C5 Determination of resistivity of

20、 aqueous extract (Technically equivalent) ISO 787-XVII:1973Part A5 Comparison of lightening power of white pigments (Technically equivalent) ISO 787-XVIII:1973Part B4 Determination of residue on sieve (water method) using a mechanical flushing procedure (Technically equivalent) ISO 842:1974BS 4726:1

21、971 Methods for sampling raw materials for paints and varnishes (Technically equivalent) Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 BSI 07-1999iii A British Standard does not purport to include all the necessary provisions

22、of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages 1 to 4, an inside

23、 back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c)

24、BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 BSI 07-19991 1 Scope and field of application This International Standard specifies the requirements and the corresponding methods of test for titanium dioxide pigment

25、s, suitable for use in paints and related products. 2 References ISO 787, General methods of test for pigments. ISO 842, Raw materials for paints and varnishes Sampling. 3 Description The material shall consist essentially of titanium dioxide (TiO2) of the anatase or the rutile crystal structure, as

26、 determined by X-ray examination. The material shall be in the form of a soft dry powder or in such a condition that it may be readily reduced thereto by crushing under a palette knife, without any grinding action. 4 Classification 4.1 Types This International Standard covers two types of titanium d

27、ioxide pigments as follows: Type A: Anatase type Type R: Rutile type 4.2 Grades The pigments are further classified into the following grades: 5 Required characteristics and their tolerances Titanium dioxide pigments shall have the characteristics indicated for their type and grade in the Table. The

28、 requirement for matter volatile at 105 C after preconditioning shall only apply if this characteristic is specified by the interested parties or in a contract. 6 Sampling A representative sample of the pigment to be tested shall be taken as specified in ISO 842. 7 Determination of titanium dioxide

29、content 7.1 Interferences Chromium, vanadium, molybdenum and niobium impurities may affect the results of this determination; these impurities may be present in commercial pigments, but normally in very small quantities only. 7.2 Reagents All reagents shall be of analytical grade. The water used sha

30、ll be distilled water or water of equivalent purity. 7.2.1 Ammonium sulphate 7.2.2 Carbon dioxide or nitrogen. 7.2.3 Sulphuric acid, concentrated ( 1,84 g/ml). 7.2.4 Sulphuric acid, 100 g/l solution. 7.2.5 Sulphuric acid, 40 g/l solution. 7.2.6 Sulphuric acid, 20 g/l solution. 7.2.7 Potassium thiocy

31、anate, 100 g/l solution. 7.2.8 Zinc amalgam, 3 % (m/m) prepared as follows: CAUTIONARY NOTE The following operations shall be carried out in a fume cupboard. Place 50 ml of mercury in a small porcelain dish on a steam bath and cover the surface of the mercury with the sulphuric acid solution (7.2.6)

32、. Add 20 to 30 g of zinc in small granules. Stir from time to time and replenish the dilute acid with water as required. When all the solid zinc has disappeared, allow the amalgam to cool and stand for several hours. Finally, filter through a Gooch crucible with no asbestos pad. Preserve the amalgam

33、 in a small bottle under the sulphuric acid solution (7.2.6). 50 ml of it will serve for many reductions and, when exhausted, may be reactivated by adding further quantities of zinc in the same way. 7.2.9 Ammonium iron(III) sulphate, 0,062 5 N standard volumetric solution, standardized against a sam

34、ple of known titanium dioxide content (TiO2) by the procedure given in 7.4. Grade A1 Type A Grade A2 Grade R1 Type R Grade R2 Grade R3 Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 2 BSI 07-1999 Table Required characteristics

35、7.3 Apparatus Nakazono reductor (see Figure), consisting of a bulb (a) with a capacity of about 350 ml with three stopcocks (b, c, d) attached. Stopcocks (b) and (d) are diametrically opposite and the extension (e) is so shaped as to facilitate the pouring of solutions into the bulb. To the lower st

36、opcock (d) can be attached, by means of thick rubber tubing (f), a small flask (g) of capacity about 50 ml. The third stopcock (c), which is smaller in bore than either of the other two, is attached to the central sphere near the upper stopcock (b) and serves to admit carbon dioxide or nitrogen (7.2

37、.2). 7.4 Procedure Weigh, into a 250 ml beaker to the nearest 0,1 mg, approximately 0,2 g of the sample, previously dried as for the determination of volatile matter at 105 C. Add 20 ml of the sulphuric acid (7.2.3) and 10 g of the ammonium sulphate (7.2.1). Mix carefully and cover with a watch glas

38、s, then heat on a heating plate until copious fumes are evolved. Continue heating at a low heat until the pigment is completely dissolved (generally this is completed after boiling for a few minutes) or until it is clear that the remainder is composed of silica or siliceous material. Cool the soluti

39、on, dilute with 100 ml of water, stir and filter if necessary. Wash the insoluble residue with the cold sulphuric acid solution (7.2.4). Attach the flask (g) to the stopcock (d) and, with the stopcocks (b) and (d) open, pour into the extension (e) sufficient of the sulphuric acid solution (7.2.5) to

40、 fill the flask (g) and leave no air space below the stopcock (d). Close the stopcock (d) and add 20 ml of the zinc amalgam (7.2.8) to the bulb (a) through the extension (e) and the stopcock (b). Heat the solution or filtrate, which should not exceed 300 ml in volume, to 50 C and pour it into the ex

41、tension (e). Attach the stopcock (c) to a source of the carbon dioxide or nitrogen (7.2.2). Pass the inert gas for 3 min and close stopcocks (b) and (c). Characteristic Requirements for Test methodType AType R A1A2R1R2R3 TiO2 content, % min.9892979080Clause 7 or other agreed methoda ColourClosely ma

42、tching that of an agreed sample ISO 787-Ib Lightening powerSimilar to that of an agreed sampleISO 787-XVIIb Matter volatile at 105 C at point of acceptance, % max. 0,50,80,5To be agreedISO 787-II Matter volatile at 105 C after 24 h preconditioning at 23 2 C and (50 5) % RH, % max. 0,50,80,51,52,5ISO

43、 787-II Matter soluble in water, % max.0,60,50,60,50,7ISO 787-IIIc pH of aqueous suspensionSimilar to that of an agreed sampleISO 787-IX Oil absorptionSimilar to that of an agreed sampleISO 787-V Residue on sieve, 45 4m, % max.0,100,100,100,100,10ISO 787-XVIII or other agreed method Resistivity of a

44、queous extractSimilar to that of an agreed sample Similar to that of an agreed sample ISO 787-XIV a Other methods which may be used by agreement are, for example, the modified Nakazono method, the cadmium reductor method, and the Jones reductor method. b A palette knife of plastics material should b

45、e used. This is to be included as an alternative in the revision of ISO 787-I and ISO 787-XVII. c If necessary, a coagulating agent should be used. Licensed Copy: sheffieldun sheffieldun, na, Fri Nov 24 08:20:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 1851:1978 BSI 07-19993 Remove the whole ap

46、paratus from the stand after disconnecting the inert gas supply and shake vigorously for 5 min, holding the apparatus in such a way that the stopcocks are kept shut. The characteristic violet coloration of trivalent titanium is formed. Then, holding the apparatus upright, open the stopcock (d) and a

47、llow the zinc amalgam to flow into the flask (g). Do this cautiously, closing the stopcock (d) as soon as the amalgam has passed. Remove the flask (g) and the rubber tubing (f) and retain the amalgam for another determination. Re-connect the inert gas supply, open the stopcock (c) and then the stopc

48、ock (b). Add 10 ml of the potassium thiocyanate solution (7.2.7) to the bulb (a) and titrate with the ammonium iron(III) sulphate solution (7.2.9) until a faint pink coloration remains for 1 min. Facilitate the titration by attaching a piece of very narrow glass tubing to the tip of the burette with

49、 a piece of rubber tubing. The extension passes through the stopcock (b) into the bulb (a). 7.5 Expression of results The titanium dioxide content (TiO2), expressed as a percentage by mass, is given by the formula 8 Test report The test report shall contain at least the following information: a) a reference to this International Standard or to a corresponding national standard; b) the type and identification of the product tested; c) the results of the tests and whether or not the product tested complies with the relevant speci

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