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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 5796:2000 ICS 83.0
2、40.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Rubber compounding ingredients Natural calcium carbonate Test methods Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared un
3、der the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 2000 BSI 11-2000 ISBN 0 580 36694 4 BS ISO 5796:2000 Amendments issued since publication Amd. No.DateComments National foreword Thi
4、s British Standard reproduces verbatim ISO 5796:2000 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/50, Rubber raw, natural and synthetic, which has the responsibility to: aid enquirers to understand the text; present t
5、o the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obt
6、ained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index, or by using the Find facility of the
7、BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions 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. Summa
8、ry of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 20, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Licensed Copy: sheffieldun sheffieldun,
9、 na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 5796:2000(E) INTERNATIONAL STANDARD ISO 5796 Second edition 2000-09-01 Rubber compounding ingredients Natural calcium carbonate Test methods Ingrdients de mlange du caoutchouc Carbonate de calcium naturel Mthode
10、s dessai Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) iii Contents Page Foreword.iv 1 Scope 1
11、2 Normative references1 3 Sampling.2 4 Methods of test 2 5 Test report10 Annex A (normative) Determination of total copper content Atomic absorption method11 Annex B (normative) Determination of total manganese content Atomic absorption method14 Annex C (normative) Determination of total iron conten
12、t Atomic absorption method.17 Annex D (informative) Classification of natural calcium carbonate and typical physical and chemical properties .20 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) iv Foreword ISO (the Internatio
13、nal Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been
14、established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standar
15、dization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least
16、 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 5796 was prepared
17、 by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This second edition cancels and replaces the first edition (ISO 5796:1990), of which it constitutes a technical revision. Annexes A, B and C form a normat
18、ive part of this International Standard. Annex D is for information only. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 5796:2000(E) 1 Rubber compounding ingredients Natural calcium carbonate Test methods WARNING
19、 Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensur
20、e compliance with any national regulatory conditions. 1 Scope 1.1 This International Standard specifies the methods to be used for the evaluation of natural calcium carbonate (chalk or limestone) ground to a dry powder for use in the rubber industry. NOTE 1 Classification of natural calcium carbonat
21、e according to fineness and chemical purity and typical physical and chemical properties for use in the rubber industry are given in informative annex D. NOTE 2 This International Standard does not cover calcium carbonates prepared by precipitation from solution. 1.2 There are two sets of analytical
22、 methods listed in this International Standard. In the body of the text (4.8.2 to 4.8.4), the traditional spectrophotometric methods are given; these are obsolescent, time-consuming and use a chlorinated solvent. It is recommended that these methods be phased out and replaced by the atomic absorptio
23、n methods listed in annexes A, B and C. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications
24、do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. M
25、embers of ISO and IEC maintain registers of currently valid International Standards. ISO 565:1990, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings. ISO 787-2:1981, General methods of test for pigments and extenders Part 2: Determination of matte
26、r volatile at 105 C. ISO 787-10:1993, General methods of test for pigments and extenders Part 10: Determination of density Pyknometer method. ISO 3262-1:1997 Extenders for paints Specifications and methods of test Part 1: Introduction and general test methods. ISO 4793:1980, Laboratory sintered (fri
27、tted) filters Porosity grading, classification and designation. ISO 15528:2000, Paints, varnishes and raw materials for paints and varnishes Sampling. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) 2 3 Sampling Sampling sha
28、ll be carried out in accordance with ISO 15528. 4 Methods of test 4.1 General During the analysis, all reagents used shall be of recognized analytical reagent quality. Distilled water or water of equal purity shall be used throughout the tests. 4.2 Residue on sieve Determine the sieve residue in acc
29、ordance with ISO 3262-1, using 45 ?m and 125 ?m opening test sieves as defined by ISO 565. 4.3 Calcium carbonate (on dry sample) Determine the calcium carbonate content in accordance with ISO 3262-1. 4.4 Loss on heating at 105 C Determine the loss on heating at 105 C in accordance with ISO 787-2. 4.
30、5 Loss on ignition at 1000 C (on dry sample) Determine the loss on ignition at 1000 C in accordance with ISO 3262-1. 4.6 Matter insoluble in hydrochloric acid 4.6.1 Reagent 4.6.1.1 Hydrochloric acid, 73 g/dm3solution. Dilute 170 cm3of concentrated (35 % by mass) hydrochloric acid (? = 1,18 g/cm3) to
31、 1 dm3with water and mix. 4.6.2 Apparatus 4.6.2.1 Beaker, of capacity 250 cm3, watch glass, suitable for covering the beaker, and glass rod suitable for stirring. 4.6.2.2 Analytical balance, accurate to 0,1 mg. 4.6.2.3 Sintered-glass crucible, porosity grade P 40, in conformity with the requirements
32、 of ISO 4793. 4.6.2.4 Oven, capable of being maintained at a temperature of 105 C ? 2 C. 4.6.2.5 Desiccator. 4.6.3 Procedure 4.6.3.1 Weigh, to the nearest 1 mg, approximately 2 g of sample into the beaker (4.6.2.1). 4.6.3.2 Pour 100 cm3of hydrochloric acid (4.6.1.1) into the beaker and cover with a
33、watch-glass. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) 3 4.6.3.3 Swirl the mixture gently at room temperature, avoiding the formation of foam. Boil the mixture gently for 5 min to 10 min, then leave to cool for 30 min
34、to 60 min, stirring from time to time. 4.6.3.4 Filter off the insoluble matter through the crucible (4.6.2.3) which has previously been washed, dried at 105 C and weighed. Wash with water until the washings are free from chloride. Discard the filtrate and the washings. 4.6.3.5 Dry the crucible conta
35、ining the insoluble residue in the oven (4.6.2.4), maintained at 105 C ? 2 C, until constant mass is achieved, i.e. until further oven-drying, cooling and weighing yields a mass change of less than 1 mg. 4.6.3.6 Cool in the desiccator (4.6.2.5). 4.6.3.7 Weigh to the nearest 1 mg. 4.6.4 Expression of
36、 results The matter insoluble in hydrochloric acid, Mis, is given, as a percentage by mass, by the following equation: M mm m is 21 0 100? ? ? where m0is the mass, in grams, of the test portion; m1is the mass, in grams, of the empty dried crucible; m2is the mass, in grams, of the crucible containing
37、 the insoluble matter. Express the result to the nearest 0,1 % by mass. 4.7 Alkalinity 4.7.1 Reagents 4.7.1.1 Distilled water,boiled to remove carbon dioxide. 4.7.1.2 Phenolphthalein,0,5 % by mass solution in 95 % by volume ethanol. 4.7.1.3 Hydrochloric acid,standard volumetric solution, c(HCI) = 0,
38、01 mol/dm3. 4.7.2 Apparatus 4.7.2.1 Analytical balance,accurate to 0,1 mg. 4.7.2.2 Conical flask,narrow-mouth, of capacity 250 cm3. 4.7.2.3 Filter paper,fine grade. 4.7.2.4 Burette,accurate to 0,1 cm3. 4.7.3 Procedure 4.7.3.1 Weigh, to the nearest 1 mg, about 10 g of sample and place this test porti
39、on in the flask (4.7.2.2). Add 150 cm3of distilled water (4.7.1.1). Leave the mixture for 1 h, shaking it from time to time. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) 4 4.7.3.2 Filter the mixture through the filter pap
40、er (4.7.2.3) and keep all the residue on the filter. Wash three times with a minimum amount of distilled water, adding the washings to the filtrate. 4.7.3.3 Add a few drops of phenolphthalein solution (4.7.1.2) as indicator to the filtrate and titrate with hydrochloric acid (4.7.1.3) until colourles
41、s. Read the volume used for the titration to the nearest 0,1 cm3. 4.7.4 Expression of results The alkalinity, w, expressed in grams of sodium carbonate (Na2CO3) per 100 g of sample, is given by the following equation: w ? ? ? Vc m 0,000 53 100 where V is the volume of HCl, in cubic centimetres, used
42、 for the titration; c is the actual concentration, expressed in moles of HCI per cubic decimetre of hydrochloric acid (4.7.1.3); m is the mass, in grams, of the test portion; 0,00053 is the mass, in grams, of sodium carbonate corresponding to 100 cm3of hydrochloric acid, c(HCI) = 0,010 mol/dm3. 4.8
43、Determination of total copper, total manganese and total iron 4.8.1 Preparation of stock test solution 4.8.1.1 Reagents 4.8.1.1.1 Nitric acid, ?= 1,42 g/cm3. 4.8.1.1.2 Hydrofluoric acid,40 % by mass solution. 4.8.1.1.3 Sulfuric acid,50 % by volume solution. 4.8.1.1.4 Octyl alcohol (octan-1-ol). 4.8.
44、1.1.5 Hydrochloric acid, ?= 1,18 g/cm3(35 % by mass). 4.8.1.2 Apparatus 4.8.1.2.1 Beaker,of capacity 250 cm3. 4.8.1.2.2 Volumetric flask,of capacity 250 cm3. 4.8.1.2.3 Platinum crucible,of capacity 20 cm3. 4.8.1.2.4 Muffle furnace. 4.8.1.2.5 Fume cupboard. 4.8.1.2.6 Quartz triangle. 4.8.1.2.7 Analyt
45、ical balance,accurate to 0,1 mg. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 5796:2000(E) 5 4.8.1.3 Procedure 4.8.1.3.1 Weigh, to the nearest 1 mg, about 5 g of sample into the beaker (4.8.1.2.1). Dissolve this test portion carefully
46、 in 25 cm3of water and 15 cm3of nitric acid (4.8.1.1.1) and heat to boiling. If foam tends to rise during the dissolution of the test portion, break the foam by adding a drop of octyl alcohol (4.8.1.1.4). 4.8.1.3.2 Filter through a medium filter paper, wash the paper with hot water and allow the com
47、bined filtrate plus washings to cool. Then transfer the solution into the volumetric flask (4.8.1.2.2) and retain for 4.8.1.3.7. 4.8.1.3.3 Lift out the filter paper, fold it carefully to enclose any residue and place in the platinum crucible (4.8.1.2.3). Heat gently until dry, then heat more to char
48、 the paper. Then place the crucible in the muffle furnace (4.8.1.2.4) at 1000 C ? 50 C for 30 min to oxidize and to remove all char. 4.8.1.3.4 Cool the crucible and add 2 cm3of hydrofluoric acid (4.8.1.1.2), drop by drop, to the crucible in such a way that all the contents are wetted. Then add 0,5 c
49、m3of sulfuric acid (4.8.1.1.3) drop by drop. Place the crucible on a hotplate in the fume cupboard (4.8.1.2.5) and evaporate to dryness, taking care to avoid overheating and consequent bumping or spitting. Then continue heating until white fumes appear. 4.8.1.3.5 Transfer the crucible, still in the fume cupboard, to a quartz triangle on a stand and heat to a dull red heat until all white fumes have been driven off. 4.8.1.3.6 Allow the crucible to cool. Add 5 cm3of water and 1 cm3of nitric acid (4.8.1.1.1) and warm on a hotp