BS 6783-14-1994 Sampling and analysis of nickel ferronickel and nickel alloys - Method for the determination of total boron content of nickel and nickel alloys by curcumin molecula.pdf
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1、BRITISH STANDARD BS 6783-14: 1994 ISO 11436: 1993 Sampling and analysis of nickel, ferronickel and nickel alloys Part 14: Method for the determination of total boron content of nickel, and nickel alloys by curcumin molecular absorption spectrometry UDC 669.245:543.422:546.27BS6783-14:1994 This Briti
2、sh Standard, having been prepared under the directionof the Non-ferrous Metals Standards Policy Committee, was published underthe authority of the Standards Board and comes intoeffect on 15 June 1994 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference NF
3、M/10 Draft for comment 92/38328 DC ISBN 0 580 23363 4 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Policy Committee (NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented:
4、Association of Bronze and Brass Founders British Non-ferrous Metals Federation British Stainless Steel Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Engineering Equipment and Materials Users Association Institute of British Foundrymen Lond
5、on Metal Exchange Ministry of Defence Nickel Development Institute Non-ferrous Metal Stockists Steel Casting Research and Trade Association Coopted members Amendments issued since publication Amd. No. Date CommentsBS6783-14:1994 BSI 10-1999 i Contents Page Committees responsible Inside front cover N
6、ational foreword ii 1 Scope 1 2 Normative reference 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Sampling and sample preparation 2 7 Procedure 2 8 Expression of results 3 9 Test report 4 Annex A (informative) Examples of aluminium alloy blocks 5 Figure A.1 Example of an aluminium alloy block 1 5 Fig
7、ure A.2 Example of an aluminium alloy block 2 6 Figure A.3 Example of an aluminium alloy block 3 7 Table 1 Boron calibration solutions 3 Table 2 Composition of test samples 4 Table 3 Results of statistical analysis 4 List of references Inside back coverBS6783-14:1994 ii BSI 10-1999 National foreword
8、 This Part of BS 6783 has been prepared under the direction of the Non-ferrous Metals Standards Policy Committee. It is identical with ISO 11436:1993 Nickel and nickel alloys Determination of total boron content Curcumin molecular absorption spectrometric method, published by the International Organ
9、ization for Standardization (ISO). At present this British Standard consists of 15 Parts all concerned with analysis of nickel, ferronickel and nickel alloys. Further International Standards are in preparation on sampling and analysis of nickel, ferronickel and nickel alloys and, when available, the
10、se will be published as further Parts of this British Standard. 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 f
11、rom legal obligations. Cross-reference International Standard Corresponding British Standard ISO 5725:1986 BS 5497 Precision of test methods Part 1:1987 Guide for the determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (Identical) Summary of pages
12、This document comprises a front cover, an inside front cover, pagesi andii, pages1 to8, 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.BS6783-
13、14:1994 BSI 10-1999 1 1 Scope This International Standard specifies a molecular absorption spectrometric method for the determination of the total boron content in the range of 4 g/t to 240 g/t in nickel and nickel alloys. NOTE 1A possible chemical interference from rhenium has been identified. 2 No
14、rmative reference The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this Intern
15、ational Standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 5725:1986, Precision of test methods Determination of repeatability and reprod
16、ucibility for a standard test method by inter-laboratory tests. 3 Principle Dissolution of a test portion in hydrochloric and nitric acids. Decomposition of resistant boron compounds (e.g. boron nitrides) by fuming the sample solution with phosphoric and sulfuric acids at not less than 290 C for 30
17、min. Formation of the boron curcumin complex in a buffered acetic acid and sulfuric acid medium, and measurement of the absorbance of the test solution at a wavelength of 543 nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distil
18、led water or water of equivalent purity. 4.1 Hydrochloric acid, 20= 1,18 g/ml. 4.2 Sulfuric acid, 20= 1,84 g/ml. 4.3 Nitric acid, 20= 1,41 g/ml. 4.4 Phosphoric acid, 20= 1,71 g/ml. 4.5 Sodium hypophosphite, monohydrate (NaH 2 PO 2 .H 2 O). 4.6 Acetic acid, glacial, 20= 1,05 g/ml. The reagent must be
19、 free from aldehydes. Aldehyde test procedure: Transfer 20 ml of the acetic acid to a 50 ml beaker and add 1 ml of 1 g/l potassium permanganate solution. The colour should not disappear within 10 min. If aldehydes are present, an easily visible brown colour will develop in 15 min. 4.7 Acetic acid-su
20、lfuric acid mixture, 1 + 1. Add in small portions, while stirring and cooling under running water, one volume of the sulfuric acid(4.2) to one volume of the acetic acid (4.6). 4.8 Acetate buffer, solution. Dissolve 225 g of ammonium acetate (CH 3 COONH 4 ) in 400 ml of water. Add 300 ml of the aceti
21、c acid(4.6). Filter the solution through a medium filter paper and dilute to 1 000 ml. Store in a polyethylene bottle. 4.9 Sodium fluoride, solution. Dissolve 4 g of sodium fluoride (NaF) in 100 ml of water and mix. 4.10 Boron, standard reference solution (100 mg/l). Weigh, to the nearest 0,000 1 g,
22、 0,285 8 g of boric acid (H 3 BO 3 ) and transfer it to a 500 ml one-mark volumetric flask. Dissolve the acid in water, make up to the mark and mix. Store the solution in a polyethylene flask. 4.11 Boron, standard solution (2 mg/l). Transfer 20,0 ml of the boron stock solution (4.10) to a 1 000 ml o
23、ne-mark volumetric flask. Dilute to volume with water and mix. Store the solution in a polyethylene flask. Prepare freshly before use. 4.12 Curcumin, solution. Dissolve 0,125 g of curcumin (C 26 H 20 O 6 ) in 60 ml of the acetic acid (4.6) in a polyethylene or quartz vessel, by heating in a water ba
24、th and using a magnetic stirrer. Cool and transfer to a 100 ml plastics volumetric flask (5.3). Dilute to volume with the acetic acid (4.6) and mix. This solution must be prepared freshly before use. 5 Apparatus All glassware and plastics flasks used in this method must be rinsed first with the acet
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