BS-6200-3.19.3-1992.pdf
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1、BRITISH STANDARD BS 6200-3.19.3: 1992 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.19: Determination of molybdenum Subsection 3.19.3: Molybdenum oxide and high grade molybdenite ores: gravimetric method Licensed Copy: sheffieldun sheffieldun, na
2、, Wed Dec 06 14:54:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.19.3:1992 This British Standard, having been prepared under the direction of the Iron and Steel Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 June 1992 BSI 09
3、-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for comment 91/44341 DC ISBN 0 580 20796 X Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Iron and Steel Standards Policy Committee
4、 (ISM/-) to Technical Committee ISM/18, upon which the following bodies were represented: BCIRA British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Ferro Alloys and Metals Producers Association Ministry of Defence Amendments issued since publication Amd. No
5、.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:54:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.19.3:1992 BSI 09-1999i Contents Page Committees responsibleInside front cover Forewordii 1Scope1 2Principle1 3Reagents1 4Apparatus1 5Sampling1 6Procedure1 7Calculation a
6、nd expression of results2 8Test report3 Table 1 Precision data2 Publication(s) referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:54:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.19.3:1992 ii BSI 09-1999 Foreword This Subsection of BS 6200 has been prepa
7、red under the direction of the Iron and Steel Standards Policy Committee and supersedes method 3 for the determination of molybdenum in BSI 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, stee
8、l and other ferrous metals. A list of contents, together with general information, is given in Part 1. 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 Standa
9、rd 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 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporat
10、ed. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:54:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.19.3:1992 BSI 09-19991 1 Scope This Subsection of BS 6200 describes a gravimetric method for the determina
11、tion of molybdenum in molybdenum oxide and high grade molybdenite ores. The method is applicable to the range of molybdenum contents normally found in these materials. NOTEThe titles of the publications referred to in this Subsection of BS 6200 are listed on the inside back cover. 2 Principle After
12、dissolution of the test portion in acid, molybdenum is precipitated as its quinolin-8-ol compound in the presence of ethylenediaminetetra-acetic acid disodium salt and ammonium oxalate, filtered, dried and weighed as the anhydrous compound, MoO2(C9H6ON)2. 3 Reagents During the analysis use only reag
13、ents of recognized analytical grade and only grade 3 water as specified in BS 3978. 3.1 Ammonia solution, density = 0.91 g/ml. 3.2 Ammonia solution, = 0.91 g/ml, diluted 1 + 1. 3.3 Ammonium oxalate 3.4 Ethylenediaminetetra-acetic acid disodium salt (EDTA.Na2), 100 g/l solution. Dissolve 10 g of EDTA
14、.Na2 in 80 ml of water, dilute to 100 ml and mix. 3.5 Hydrochloric acid, = 1.16 g/ml to 1.18 g/ml. 3.6 Hydrochloric acid = 1.16 g/ml to 1.18 g/ml, diluted 1 + 1. 3.7 Hydrofluoric acid, 40 % (m/m). 3.8 Nitric acid, = 1.42 g/ml. 3.9 Nitric acid, = 1.42 g/ml, diluted 1 + 3. 3.10 Quinolin-8-ol, 30 g/l s
15、olution. Dissolve 3 g of quinolin-8-ol (also known as 8-hydroxyquinoline or oxine) in 12 ml of acetic acid, = 1.048 g/ml to 1.050 g/ml, add 60 ml of water and warm to approximately 40 C. Add ammonia solution (3.1) dropwise until a slight permanent precipitate is formed. Just redissolve the precipita
16、te with dropwise additions of acetic acid, = 1.048 g/ml to 1.050 g/ml, cool, dilute to 100 ml and mix. 3.11 Sulfuric acid, = 1.84 g/ml, diluted 1 + 1. To 80 ml of water add cautiously, with cooling and stirring, 100 ml of sulfuric acid, = 1.84 g/ml, cool, dilute to 200 ml and mix. 4 Apparatus 4.1 Or
17、dinary laboratory apparatus 4.2 Volumetric glassware, in accordance with class A of BS 1792. 4.3 Polytetrafluoroethylene beakers 4.4 pH meter 4.5 Crucibles, sintered glass, pore size index 4 m to 10 m, in accordance with BS 1752. Use the following procedures for handling and cooling sintered glass c
18、rucibles. a) Before use, wash the crucible several times with hot nitric acid (3.9) and finally with water, using gentle suction. b) After suction washing, wash the outer crucible wall with hot water, dry on filter paper and from that stage do not touch with bare hands. Preferably, handle the crucib
19、le with tweezers or tongs or for a minimum period in a gloved hand. Dry at 125 C. c) After oven drying, place empty crucibles or those containing the quinolin-8-ol precipitate in an efficient desiccator and allow to stand at balance room temperature for 1 h before weighing. Repeat the drying and coo
20、ling until the weight is constant. d) After use, remove the bulk of precipitate with a jet of water, place the crucible in a small beaker containing 5 ml to 10 ml of sulfuric acid (3.11) and fill the crucible with nitric acid (3.8). Heat the beaker until fumes of sulfur trioxide are evolved, cool, r
21、emove the crucible and pass approximately 100 ml of hot water through the sinter under gentle suction. Treat the washed crucible as in b) and c) above. 5 Sampling Carry out sampling in accordance with accepted practice. NOTESuitable procedures will be included in BS 6200-2 which is currently in prep
22、aration. On its publication this Subsection will be amended to include sampling in accordance with BS 6200-2. 6 Procedure 6.1 Test portion Weigh, to the nearest 0.001 g, a test portion of 1.0 g. 6.2 Determination 6.2.1 Preparation of the test solution Place the test portion in a 150 ml polytetrafluo
23、roethylene beaker (4.3). Add 10 ml of sulfuric acid (3.11), 5 ml of nitric acid (3.8) and 5 ml of hydrofluoric acid (3.7). Evaporate until fumes of sulfur trioxide are evolved, and continue fuming for 15 min. Cool, add 5 ml of hydrochloric acid (3.5) and 5 ml of nitric acid (3.8), warm for 10 min, a
24、nd dilute to approximately 50 ml. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:54:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.19.3:1992 2 BSI 09-1999 Add 10 ml of EDTA.Na2 solution (3.4), neutralize with ammonia solution (3.1) then add 5 ml excess. Heat at 50 C to 60 C for 1
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