BS-6200-3.37.1-1986.pdf
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1、BRITISH STANDARD BS 6200-3.37.1: 1986 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.37 Determination of zirconium Subsection 3.37.1 Steel: gravimetric method UDC 669.1:543.21:546.831 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:58:30
2、 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.37.1:1986 This British Standard, having been prepared under the direction of the Iron and Steel Standards Committee, was published under the authority of the Board of BSI and comes into effect on September 1986 BSI 09-1999 The following BSI refer
3、ences relate to the work on this standard: Committee reference ISM/18 Draft for comment 85/36441 DC ISBN 0 580 15281 2 Foreword This Subsection of BS 6200 has been prepared under the direction of the Iron and Steel Standards Committee. It supersedes method 1 for the determination of zirconium in BSI
4、 Handbook No. 19, to which it is technically equivalent. BS 6200 is a multipart British Standard covering all aspects of the sampling and analysis of iron, steel and other ferrous metals. A list of contents, together with general information, will be given in Part 1, to be published in due course. A
5、 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. Summary of pages This document comprises a
6、 front cover, an inside front cover, pages i and ii, pages 1 and 2, an inside 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. Amendments issued since pu
7、blication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:58:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.37.1:1986 BSI 09-1999i Contents Page ForewordInside front cover 1Scope1 2Principle1 3Reagents1 4Apparatus1 5Sampling1 6Procedure1 7Calculation
8、and expression of results2 8Test report2 Table 1 Precision data2 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:58:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:58:30 GMT+00:00 200
9、6, Uncontrolled Copy, (c) BSI BS 6200-3.37.1:1986 BSI 09-19991 1 Scope This Subsection of BS 6200 describes a gravimetric method for the determination of zirconium in steel. The method is applicable to zirconium contents exceeding 0.03 % m/m. NOTEThe titles of the publications referred to in this Su
10、bsection of BS 6200 are listed on the inside back cover. 2 Principle Zirconium is precipitated from a sulphuric acid solution of the sample by means of cupferron and then ignited to oxide, any silica being removed by volatilization with hydrofluoric acid. The residue is fused with potassium hydrogen
11、 sulphate, extracted in acid and zirconium is precipitated with mandelic acid. The determination is completed gravimetrically after ignition to the oxide. 3 Reagents During the analysis, use only reagents of recognized analytical reagent grade and only distilled water or water of equivalent purity.
12、3.1 Ammonium nitrate, 20 g/L solution. Dissolve 20 g of ammonium nitrate in water, dilute to 1 L and mix. 3.2 Cupferron, 50 g/L solution. Dissolve 5 g of cupferron in water, dilute to 100 mL and mix. Prepare this solution from fresh reagent immediately before use, since the solid reagent and its sol
13、ution deteriorate on storage. 3.3 Cupferron-acid wash To 900 mL of water add 10 mL of sulphuric acid (3.13) and 5 mL of cupferron solution (3.2). Dilute to 1 L and mix. 3.4 Hydrochloric acid, density () 1.16 g/mL to 1.19 g/mL. 3.5 Hydrochloric acid, 1.16 g/mL to 1.19 g/mL, diluted 1 + 9. 3.6 Hydroch
14、loric acid, 1.16 g/mL to 1.19 g/mL, diluted 1 + 19. 3.7 Hydrochloric acid, 1.16 g/mL to 1.19 g/mL, diluted 1 + 49. 3.8 Hydrofluoric acid, 40 % m/m. 3.9 Mandelic acid, 160 g/L solution. Dissolve 160 g of mandelic acid in water, dilute to 1 L and mix. 3.10 Mandelic acid-hydrochloric acid wash Dissolve
15、 50 g of mandelic acid in hydrochloric acid (3.7), dilute to 1 L with hydrochloric acid (3.7) and mix. 3.11 Potassium carbonate, anhydrous, (K2 CO3). 3.12 Potassium hydrogen sulphate, (KHSO4). 3.13 Sulphuric acid, 1.84 g/mL. 3.14 Sulphuric acid, 1.84 g/mL, diluted 1 + 4. To 400 mL of water add cauti
16、ously 200 mL of sulphuric acid (3.13). Mix, cool, dilute to 1 L and mix. 4 Apparatus Use ordinary laboratory apparatus. 5 Sampling Sampling shall be carried out in accordance with BS 1837. NOTEBS 6200-2 “Methods of sampling and sample preparation”, which will supersede BS 1837, is currently in prepa
17、ration. On its publication, this Subsection will be amended to include a requirement to sample in accordance with BS 6200-2. 6 Procedure 6.1 Test portion Weigh, to the nearest 0.001 g, a test portion of 7.5 g. 6.2 Determination Place the test portion in a 600 mL squat beaker. Add 100 mL of sulphuric
18、 acid (3.14) and heat until solvent action ceases. Evaporate until fuming commences, cool, add 100 mL of water and heat until the soluble salts are dissolved. Dilute to 250 mL and cool to below 15 C. Add a small amount of paper-pulp and, with continuous stirring, add freshly prepared cupferron solut
19、ion (3.2) dropwise until the precipitate begins to turn reddish-brown. Allow to stand for 5 min, filter through a paper-pulp pad and wash with the cupferron-acid wash solution (3.3). Transfer the filter and precipitate to a platinum dish, dry and ignite at 700 C until free from carbonaceous matter.
20、Cool, add 2 mL of sulphuric acid (3.14) and 5 mL of hydrofluoric acid (3.8). Evaporate to dryness and ignite at 700 C. For samples containing niobium, tantalum or tungsten, proceed as follows. Cover the residue with 5 g of potassium carbonate (3.11), fuse at about 950 C for 20 min and then cool. Ext
21、ract with 200 mL of water and boil gently for 15 min. Filter through a paper-pulp pad and wash with hot ammonium nitrate solution (3.1). Transfer the filter and precipitate to the original dish, dry and ignite at about 700 C. Cool, add 2 mL of sulphuric acid (3.14) and 5 mL of hydrofluoric acid (3.8
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