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1、BRITISH STANDARD BS 5293-10: 2001 ISO 1304:1999 Sampling and testing carbon black for use in the rubber industry Part 10: Method for determination of iodine adsorption number (ISO title: Rubber compounding ingredients Carbon black Determination of iodine adsorption number Titrimetric method) ICS 83.
2、040.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-10:2001 This British Standard, having been prepared under the direction of the Sector Policy and Strategy C
3、ommittee for Materials and Chemicals, was published under the authority of the Standards Policy and Strategy Committee on 6 November 2001 BSI 6 November 2001 ISBN 0 580 38661 9 National foreword This British Standard reproduces verbatim ISO 1304:1999 and implements it as the UK national standard. It
4、 supersedes BS 5293-10:1988 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/50, Natural and synthetic rubbers, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cros
5、s-references The British Standards which implement international or European 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 BSI Standards Electroni
6、c 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. aid enquirers to understand
7、the text; present to 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. Summary of pages This document comprises a fr
8、ont cover, an inside front cover, ISO title page, page ii, pages 1 to 11 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 1
9、6:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI A Reference number ISO 1304:1999(E) INTERNATIONAL STANDARD ISO 1304 Third edition 1999-03-15 Rubber compounding ingredients Carbon black Determination of iodine adsorption number Titrimetric method Ingrdients de mlange du caoutchouc Noir de carbone
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12、etnirP ii Foreword ISO (the International 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
13、 which a technical committee has been 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 a
14、ll matters of electrotechnical standardization. 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 75 % of the member bodies casting a vote. International Standard IS
15、O 1304 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This third edition cancels and replaces the second edition (ISO 1304:1985), which has been technically revised. Annex A of this Interna
16、tional Standard is for information only. 9991:013925 SBBS 529310:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DRADNATS LANOITANRETNI OSI)E(9991:4031 OSI 1 Rubber compounding ingredients Carbon black Determination of iodine adsorption
17、 number Titrimetric method WARNING 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
18、 and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies a titrimetric method for the determination of the iodine adsorption number of carbon blacks for use in the rubber industry. The iodine adsorption number is related to
19、 the surface area of a carbon black, and is generally in agreement with the nitrogen surface area. However, it is significantly depressed in the presence of a high content of volatile or solvent-extractable materials; the iodine adsorption number therefore does not always provide a measure of the sp
20、ecific surface area of a carbon black. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision,
21、and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 385-1:1984, Laboratory glasswa
22、re Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1998, Laboratory glassware One-mark volumetric flasks. ISO 1126:1992, Rubber compounding ingredients Carbon black Determination of loss on heating. ISO TR 6809:1996, Rubber compounding ingredient
23、s Carbon black Standard reference blacks. ISO/TR 9272:1986, Rubber and rubber products Determination of precision for test method standards. 3 Principle A test portion of carbon black is dried, weighed and mixed vigorously with a measured volume of standard iodine solution. The mixture is then centr
24、ifuged. A measured volume of the clear iodine solution is titrated with a standard solution of sodium thiosulfate. From this titration value and the mass of the test portion, the iodine adsorption number of the carbon black is calculated. 9991:013925 SBBS 529310:2001 Licensed Copy: sheffieldun sheff
25、ieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 1304:1999(E) OSI 2 4 Apparatus Ordinary laboratory equipment (beakers, funnels, porcelain spoon, weighing bottles, etc.), plus the following: 4.1 Analytical balance, with 0,1 mg sensitivity. 4.2 Oven, preferably of the gr
26、avity-convection type, capable of temperature regulation to within 1 C at 125 C and temperature uniformity to within 5 C. 4.3 Stoppered one-mark volumetric flasks, preferably class A in accordance with ISO 1042, of capacities a) 2 000 cm3, with a tolerance of 0,60 cm3, b) 1 000 cm3, with a tolerance
27、 of 0,40 cm3. 4.4 One-mark pipettes, high precision, of capacities: a) 20 cm3, with a tolerance of 0,03 cm3, b) 25 cm3, with a tolerance of 0,03 cm3, or repetitive dispenser, 25 cm3 capacity, calibrated to within 0,03 cm3 accuracy. If class A pipettes in accordance with ISO 648 are used, no calibrat
28、ion is necessary. In other cases, pipettes shall be calibrated to the nearest 0,01 cm3 with distilled water, a temperature correction being made if necessary to show the true delivery at any volume used to within 0,01 cm3. The true delivered volume is the read volume plus (or minus) the calibration
29、correction at that volume. For high-precision volume determination (see 7.2.2, 7.3.2, 8.3.3, 8.3.6 and 8.3.8), it is recommended that the 20 cm3 and 25 cm3 pipettes have calibration corrections of the same magnitude and in the same sense. 4.5 Burettes, high precision, side-arm filling, graduated in
30、0,05 cm3 and with automatic zero, of capacities: a) 25 cm3, with a tolerance of 0,05 cm3, b) 50 cm3, with a tolerance of 0,05 cm3, or digital burettes, with 0,01 cm3 increment counter and zero-reset control, calibrated to within 0,05 cm3 accuracy. If class A burettes in accordance with ISO 385-1 are
31、 used, no calibration is necessary. In other cases, burettes shall be calibrated to the nearest 0,01 cm3 with distilled water, a temperature correction being made if necessary to show the true delivery at any volume used to within 0,01 cm3. The true delivered volume is the read volume plus (or minus
32、) the calibration correction at that volume. 4.6 Stoppered bottles, with ground-glass stoppers, of capacities 250 cm3 and 500 cm3. 4.7 Amber-glass stoppered bottles, with ground-glass stoppers, of capacities 1 000 cm3 and 2 000 cm3. 4.8 Centrifuge tubes, of capacity 50 cm3, with screw cap and polyet
33、hylene liner. Cork, rubber or metal stoppers shall not be used. 4.9 Mechanical shaker, capable of 240 strokes/min, with 25 mm stroke length. 4.10 Centrifuge, minimum speed 105 rad/s (1 000 r/min). 4.11 Desiccator. 4.12 Magnetic stirrers and spin bars. 9991:013925 SBBS 529310:2001 Licensed Copy: shef
34、fieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI OSIISO 1304:1999(E) 3 5 Reagents Unless otherwise stated, all chemicals shall be of reagent grade. 5.1 Water, deionized, having a pH-value within the range 6,5 to 7,2 (preferably close to 6,9). NOTE It is recomme
35、nded that freshly reboiled water be used, obtained from water distilled then polished with a mixed bed of ion-exchange materials and a 0,2 m to 4 m membrane filter. Deionized water shall be protected from atmospheric contamination and from dissolution of container and tubing materials. Extreme care
36、shall be exercised in handling the water. Containers and tubing shall be made of polytetrafluoroethylene, solid tin, quartz, 18-8 stainless steel, polyethylene or some other material proven to be sufficiently resistant to chemical attack. 5.2 Iodine (I2). 5.3 Potassium iodide (Kl). 5.4 Potassium iod
37、ate (KIO3). 5.5 Sodium thiosulfate pentahydrate (Na2S2O3 5H2O). 5.6 n-Amyl alcohol (C5H11OH). 5.7 Sulfuric acid (H2SO4), 98 % (m/m), r = 1,84 Mg/m3. 5.8 Soluble starch. 5.9 Salicylic acid (C7H6O3). 6 Preparation of solutions1) 6.1 Iodine solution, 0,023 64 mol/dm3 (0,047 28 N), containing 9,5 parts
38、of potassium iodide to 1 part of iodine. 6.1.1 Weigh, to the nearest 0,01 g, 114,00 g of potassium iodide (5.3) into a 100 cm3 beaker. 6.1.2 Place about three-quarters of the KI in a clean 2 000 cm3 volumetric flask (see 4.3) through a large-diameter funnel. 6.1.3 Add enough water (5.1) to cover the
39、 KI. Swirl to dissolve, and allow to stand until the solution attains ambient temperature. 6.1.4 Place the remainder of the KI in a 250 cm3 beaker with enough water (5.1) to dissolve it. 6.1.5 Weigh exactly2) 12,000 0 g of iodine on the balance (4.1) in a weighing bottle fitted with a ground-glass s
40、topper. Record the mass to the nearest 0,1 mg. Use only a porcelain spoon to transfer the iodine crystals, and close the weighing bottle when making weighings. 6.1.6 Transfer the iodine through a funnel to the potassium iodide solution prepared in 6.1.3. 1) It is easier to weigh approximate masses t
41、o the nearest 0,1 mg and calculate the results rather than attempt to weigh test portion masses exactly. 2) In this case, it is not sufficient to calculate a correction factor, since the test result depends on the concentration of the iodine solution (see 7.3.5). 9991:013925 SBBS 529310:2001 License
42、d Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 1304:1999(E) OSI 4 6.1.7 Wash thoroughly the weighing bottle with portions of the KI solution prepared in 6.1.4 until no colour remains, and transfer the washings through the funnel to the 2 000 c
43、m3 volumetric flask. 6.1.8 Wash the funnel with the rest of the KI solution prepared in 6.1.4. 6.1.9 Add water (5.1) to almost fill the volumetric flask, cap it with the ground-glass stopper, invert it 2 or 3 times to homogenize and let it stand for about one hour. 6.1.10 Open the flask, make up to
44、the mark with water (5.1), insert a spin bar in the flask, place it on the magnetic stirrer (4.12) and stir for 2 h at least at medium speed. NOTE At medium speed, the depth of the vortex should be about 5 mm. 6.1.11 Transfer the solution to an amber-glass bottle (4.7) and let it stand overnight pri
45、or to any use. 6.2 Sodium thiosulfate solution, 0,039 4 mol/dm3 (0,039 4 N). 6.2.1 Weigh, to the nearest 0,005 g, 19,560 g of sodium thiosulfate pentahydrate (5.5) into a suitable container. 6.2.2 With the help of a funnel, transfer the weighed sodium thiosulfate to a 2 000 cm3 volumetric flask (see
46、 4.3). 6.2.3 Add through the funnel about 1 litre of water (5.1). Wash carefully. 6.2.4 Add 10 cm3 of n-amyl alcohol (5.6) to the flask, and shake the solution in the flask vigorously until all crystals are dissolved. 6.2.5 Make up to the mark with water (5.1), insert a spin bar in the flask, place
47、it on the magnetic stirrer and stir for about 2 h at medium speed (see note to 6.1.10). 6.2.6 Transfer the solution to an amber-glass bottle (4.7). 6.3 Potassium iodate/iodide solution, c(KIO3) = 0,006 567 mol/dm3 (0,039 40 N). 6.3.1 Dry an adequate quantity of potassium iodate in the oven (4.2) at
48、125 C for 1 h. Allow to cool to ambient temperature in the desiccator (4.11). 6.3.2 In a 1 000 cm3 volumetric flask (see 4.3), dissolve 45,0 g (weighed to the nearest 0,1 g) of potassium iodide (5.3) in about 200 cm3 of water (5.1). Allow to stand until the solution attains ambient temperature. 6.3.
49、3 Weigh out, to the nearest 0,1 mg, 1,405 4 g of the freshly dried potassium iodate (6.3.1) and transfer to the iodide solution in the volumetric flask. 6.3.4 Make up to the mark with water (5.1), cap the flask and homogenize the solution by inverting the flask 4 to 5 times. 6.3.5 Transfer the solution to an amber-glass bottle (4.7). NOTE The potassium iodate/iodide solution is a primary standard in this test method, and it is essentia