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 669.1:543.21:546.831BS6200-3.37.1:1986 This British Standard, having been prepared u
2、nder the directionof the Iron and Steel Standards Committee, was published under the authority ofthe Board of BSI and comes intoeffect on September1986 BSI 09-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for comment 85/36441 DC ISBN 0 580 15
3、281 2 Foreword This Subsection of BS6200 has been prepared under the direction of the Iron and Steel Standards Committee. It supersedes method 1 for the determination of zirconium in BSI Handbook No. 19, to which it is technically equivalent. BS 6200 is a multipart British Standard covering all aspe
4、cts of the sampling and analysis of iron, steel and other ferrous metals. A list of contents, together with general information, will be given in Part1, to be published in due course. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standard
5、s 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 and ii, pages 1 and 2, an inside back cover and a back cover. This sta
6、ndard 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 publication Amd. No. Date of issue CommentsBS6200-3.37.1:1986 BSI 09-1999 i Contents Page Foreword Inside front cover
7、 1 Scope 1 2 Principle 1 3 Reagents 1 4 Apparatus 1 5 Sampling 1 6 Procedure 1 7 Calculation and expression of results 2 8 Test report 2 Table 1 Precision data 2 Publications referred to Inside back coverii blankBS6200-3.37.1:1986 BSI 09-1999 1 1 Scope This Subsection of BS 6200 describes a gravimet
8、ric method for the determination of zirconium in steel. The method is applicable to zirconium contents exceeding0.03% m/m. NOTEThe titles of the publications referred to in this Subsection of BS6200 are listed on the inside back cover. 2 Principle Zirconium is precipitated from a sulphuric acid solu
9、tion 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 sulphate, extracted in acid and zirconium is precipitated with mandelic acid. The determination is completed gravimetric
10、ally 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. 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,
11、50 g/L solution. Dissolve 5 g of cupferron in water, dilute to100mL and mix. Prepare this solution from fresh reagent immediately before use, since the solid reagent and its solution 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 cupf
12、erron solution (3.2). Dilute to1 L and mix. 3.4 Hydrochloric acid, density ( ) 1.16 g/mL to1.19g/mL. 3.5 Hydrochloric acid, 1.16g/mL to1.19g/mL, diluted1+9. 3.6 Hydrochloric acid, 1.16g/mL to1.19g/mL, diluted1+19. 3.7 Hydrochloric acid, 1.16g/mL to1.19g/mL, diluted1+49. 3.8 Hydrofluoric acid, 40% m/
13、m. 3.9 Mandelic acid, 160 g/L solution. Dissolve 160 g of mandelic acid in water, dilute to1L and mix. 3.10 Mandelic acid-hydrochloric acid wash Dissolve 50 g of mandelic acid in hydrochloric acid(3.7), dilute to1L with hydrochloric acid (3.7) and mix. 3.11 Potassium carbonate, anhydrous, (K 2CO 3 )
14、. 3.12 Potassium hydrogen sulphate, (KHSO 4 ). 3.13 Sulphuric acid, 1.84 g/mL. 3.14 Sulphuric acid, 1.84 g/mL, diluted1+4. To 400 mL of water add cautiously200mL of sulphuric acid (3.13). Mix, cool, dilute to1L and mix. 4 Apparatus Use ordinary laboratory apparatus. 5 Sampling Sampling shall be carr
15、ied out in accordance with BS1837. NOTEBS 6200-2 “Methods of sampling and sample preparation”, which will supersede BS1837, is currently in preparation. On its publication, this Subsection will be amended to include a requirement to sample in accordance with BS6200-2. 6 Procedure 6.1 Test portion We
16、igh, to the nearest0.001g, a test portion of7.5g. 6.2 Determination Place the test portion in a600mL squat beaker. Add 100mL of sulphuric acid (3.14) and heat until solvent action ceases. Evaporate until fuming commences, cool, add100mL of water and heat until the soluble salts are dissolved. Dilute
17、 to250mL and cool to below15 C. Add a small amount of paper-pulp and, with continuous stirring, add freshly prepared cupferron solution (3.2) dropwise until the precipitate begins to turn reddish-brown. Allow to stand for5min, filter through a paper-pulp pad and wash with the cupferron-acid wash sol
18、ution (3.3). Transfer the filter and precipitate to a platinum dish, dry and ignite at700 C until free from carbonaceous matter. Cool, add2mL of sulphuric acid (3.14) and5mL of hydrofluoric acid (3.8). Evaporate to dryness and ignite at700 C. For samples containing niobium, tantalum or tungsten, pro
19、ceed as follows. Cover the residue with5g of potassium carbonate (3.11), fuse at about950 C for20min and then cool. Extract with200mL of water and boil gently for15min. Filter through a paper-pulp pad and wash with hot ammonium nitrate solution (3.1). Transfer the filter and precipitate to the origi
20、nal dish, dry and ignite at about700 C. Cool, add2mL of sulphuric acid(3.14) and5mL of hydrofluoric acid (3.8). Evaporate to dryness and ignite at700 C. Continue as follows, in common with all other test portions.BS6200-3.37.1:1986 2 BSI 09-1999 Fuse the residue with1.5g of potassium hydrogen sulpha
21、te (3.12) and extract the melt with50mL of hydrochloric acid (3.5) contained in a250mL conical beaker. Evaporate to about20mL and filter through a small paper-pulp pad into a250mL conical beaker, washing with hot hydrochloric acid(3.6). Evaporate the filtrate to about15mL, add5mL of hydrochloric aci
22、d (3.4) and50mL of mandelic acid(3.9). Dilute to100mL, heat to85 C and maintain at this temperature for20min. If very little precipitate forms, allow to stand overnight at room temperature. Filter through a paper-pulp pad and wash with the warm mandelic acid-hydrochloric acid wash solution (3.10). T
23、ransfer the filter and precipitate to a weighed platinum dish, ignite at a low temperature until free from carbonaceous matter and finally at about850 C. Cool in a desiccator and weigh as zirconium oxide (ZrO 2 ). If the precipitate is discoloured, repeat the precipitation with mandelic acid, commen
24、cing at the stage where the residue is fused with1.5g of potassium hydrogen sulphate. 7 Calculation and expression of results 7.1 Calculation Calculate the zirconium content, expressed as a percentage by mass, from the equation zirconium content = where m 1is the mass (in g) of zirconium oxide; m is
25、 the mass (in g) of the test portion (6.1). 7.2 Precision A planned trial of this method was carried out by11analysts, each from a different laboratory; three tests were carried out by each analyst on each of three samples. From the results obtained, the95% confidence limits (2s) have been calculate
26、d in accordance with BS5497-1 and are given in Table 1. The difference between two single results found on identical material by one analyst using the same apparatus within a short time interval will exceed the repeatability, r, not more than once in20cases in the normal and correct operation of the
27、 method. The difference between two single and independent results found by two operators working in different laboratories on identical test material will exceed the reproducibility, R, on average, not more than once in20cases in the normal and correct operation of the method. Table 1 Precision dat
28、a 8 Test report The test report shall contain the following information: a) identification of the sample; b) the method of analysis used, by reference to this Subsection of BS6200; c) the results obtained and the form in which they are expressed; d) any particular details noted during the determinat
29、ion; e) any operations not specified in this standard, or any optional operations which may have influenced the results. 74.03m 1 m - Alloy type Zirconium content Repeatability, r Reproducibility, R % m/m 1 % m/m C, 1.5 % m/m Crsteel 0.045 0.008 0.011 13 % m/m Cr stainless steel 0.12 0.008 0.014 1.5
30、 % m/m Cr, 2 % m/m W steel 0.40 0.020 0.024BS6200-3.37.1:1986 BSI 09-1999 Publications referred to BS 1837, Methods for the sampling of iron, steel, permanent magnet alloys and ferro-alloys. BS 5497, Precision of test methods. BS 5497-1, Guide for the determination of repeatability and reproducibili
31、ty for a standard test method. BSI Handbook No. 19, Methods for the sampling and analysis of iron, steel and other ferrous metals 1) . 1) Referred to in the foreword only.BS 6200-3.37.1: 1986 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body
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