《BS-ISO-11174-1996.pdf》由会员分享，可在线阅读，更多相关《BS-ISO-11174-1996.pdf（22页珍藏版）》请在三一文库上搜索。
1、BRITISH STANDARD BS ISO 11174:1996 Implementation of ISO 11174:1996 Workplace air Determination of particulate cadmium and cadmium compounds Flame and electro-thermal atomic absorption spectrometric method ICS 13.040.30 Licensed Copy: London South Bank University, London South Bank University, Tue J
2、an 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 11174:1996 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Board and comes into effect on 15 January 1997 BSI 12-1998 The fo
3、llowing BSI references relate to the work on this standard: Committee reference EH/2/2 Draft for comment 94/503110 DC ISBN 0 580 26876 4 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee EH/2, Air quality, to Subcommittee E
4、H/2/2, Workplace atmospheres, upon which the following bodies were represented: Asbestos Information Centre Limited Asbestosis Research Council BCIRA British Ceramic Research Limited British Gas plc British Occupational Hygiene Society Chemical Industries Association Department of Trade and Industry
5、 (Laboratory of the Government Chemist) Employers Association of Catering Equipment Engineers Limited Engineering Equipment and Materials Users Association Fibre Cement Manufacturers Association Limited Health and Safety Executive Institute of Energy Institute of Occupational Medicine Institution of
6、 Occupational Hygienists London Transport Royal Society of Chemistry Amendments issued since publication Amd. No.DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 11174:1996 BSI 12-1998i Conte
7、nts Committees responsibleInside front cover National forewordii Forewordii 1Scope1 2Normative references1 3Principle1 4Reactions2 5Reagents2 6Apparatus3 7Sampling5 8Procedure for analysis7 9Expression of results10 10Special cases12 11Test report13 Annex A (informative) Typical operating parameters
8、for determination of cadmium by electrothermal atomic absorption spectrometry14 Annex B (informative) BibliographyInside back cover Table A.1 Typical temperature profile for determination of cadmium by electrothermal atomic absorption spectrometry14 Table A.2 Typical autosampler injection volumes fo
9、r the in situ preparation of matrix-modified reference and sample solutions14 Licensed Copy: London South Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 11174-1996 ii BSI 12-1998 National foreword This British Standard reproduces
10、verbatim ISO 11174:1996 and implements it as the UK national standard. This British Standard is published under the direction of the Health and Environment Sector Board whose Technical Committee EH/2 has the responsibility to: aid enquirers to understand the text; present to the responsible internat
11、ional committee any enquiries on interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK. NOTEInternational and European Standards, as well as overseas standards, are available from Customer Servic
12、es, BSI, 389 Chiswick High Road, London W4 4AL. Textual errors. When adopting the text of the international standard, the textual errors listed below were discovered. They have been marked in the text and have been reported to ISO in a proposal to amend the text of the international standard. 1. Cla
13、use 6.1.4. The title should read “Portable flowmeter”. 2. Clause 6.2.9. The title should read “Disposable gloves”. 3. Clause 8.2.2. The phrase with “partially cover with a watch” should read “partially cover with a watch glass”. 4. Clause 9.2.1. The term “spiked filters” should read “dosed filters”
14、for consistency with 9.2.1. of BS 6069-3.8. 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 obligation
15、s. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the ISO title page, page ii, pages 1 to 14, 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
16、 the amendment table on the inside front cover. Licensed Copy: London South Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI Licensed Copy: London South Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Unc
17、ontrolled Copy, (c) BSI BS ISO 11174:1996 ii BSI 12-1998 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 committee
18、s. Each member body interested in a subject for 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 Inter
19、national Electrotechnical Commission (IEC) on all 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 b
20、odies casting a vote. International Standard ISO 11174 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 2, Workplace atmospheres. Annexes A and B of this International Standard are for information only. Licensed Copy: London South Bank University, London South Bank Univer
21、sity, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 11174:1996 BSI 12-19981 WARNING Cadmium and cadmium compounds are toxic and are suspected human carcinogens (see reference 1 in annex B). Avoid any exposure by inhalation. Personal protection (e.g. an effective respirator) m
22、ust be used in all cases where exposure to cadmium or cadmium compounds is possible. 1 Scope This International Standard specifies a method for the determination of the mass concentration of particulate cadmium and cadmium compounds in workplace air, using either flame or electrothermal atomic absor
23、ption spectrometry. The sample digestion procedure specified in 8.2.2 has been validated (see reference 2 in annex B) for a selection of cadmium compounds and pigments and glass enamels containing cadmium. The analytical method has been validated (see reference 2 in annex B) for the determination of
24、 masses of 10 ng to 600 ng of cadmium per sample using electrothermal atomic absorption spectrometry, and 0,15 g to 96 g of cadmium per sample using flame atomic absorption spectrometry. The concentration range for cadmium in air for which this procedure is applicable is determined in part by the sa
25、mpling procedure selected by the user. The method is applicable to personal sampling of the inhalable or respirable fraction of airborne particles, as defined in ISO 7708, and to fixed-location sampling. 2 Normative references The following standards contain provisions which, through reference in th
26、is text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recen
27、t editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3585:1991, Borosilicate glass 3.3 Properties. I
28、SO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6955:1982, Analytical spectroscopic methods Flame emission, atomic absorption and atomic fluorescence Vocabulary. ISO 7708:1995, Air quality Particle size fraction definitions for health-related sampling. ISO 8655-
29、1:1), Piston and/or plunger operated volumetric apparatus (POVA) Part 1: Definitions. ISO 8655-2:1), Piston and/or plunger operated volumetric apparatus (POVA) Part 2: Operating considerations. ISO 8655-3:1), Piston and/or plunger operated volumetric apparatus (POVA) Part 3: Methods of test. ISO 865
30、5-4:1), Piston and/or plunger operated volumetric apparatus (POVA) Part 4: Specifications. ISO 8756:1994, Air quality Handling of temperature, pressure and humidity data. EN 482:1994, Workplace atmospheres General requirements for the performance of procedures for the measurement of chemical agents.
31、 EN 1232:1), Workplace atmospheres Pumps for personal sampling of chemical agents Requirements and test methods. 3 Principle 3.1 Particulate cadmium and cadmium compounds are collected by drawing a measured volume of air through a filter mounted in a sampler designed to collect either the inhalable
32、fraction of airborne particles or the respirable fraction of airborne particles, as appropriate (see note 17). 3.2 A test solution is prepared by treating the filter and collected sample with 5 ml of nitric acid diluted 1 + 1, heating on a hotplate until about 1 ml of concentrated nitric acid soluti
33、on remains, allowing the solution to cool and then diluting to 10 ml with water. 3.3 The test solution is analysed for cadmium by aspirating into the oxidizing air/acetylene flame of an atomic absorption spectrometer equipped with a cadmium hollow cathode lamp or electrodeless discharge lamp. Absorb
34、ance measurements are made at 228,8 nm and results are obtained by the analytical-curve technique (see ISO 6955:1982, subclause 6.1.1). 1) To be published Licensed Copy: London South Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO
35、11174:1996 2 BSI 12-1998 3.4 For accurate determination when the concentration of cadmium in the solution is low, the analysis may be repeated using electrothermal atomic absorption spectrometry. Aliquots of the test solution and a matrix-modifier solution are injected onto a solid, pyrolytic graphi
36、te platform mounted in a pyrolytically coated graphite tube, and after the drying and sample ashing stages the sample is atomized electrothermally. Absorbance measurements are made at 228,8 nm with background correction and results are obtained by the analytical-curve technique (see ISO 6955:1982, s
37、ubclause 6.1.1). 4 Reactions In general, the majority of particulate cadmium compounds which are commonly found in samples of workplace air are converted to water-soluble cadmium ions (Cd2+) by the sample digestion procedure specified in 8.2.2. However, if there is any doubt about the effectiveness
38、of this procedure for digestion of particulate cadmium compounds which could be present in the test atmosphere, investigate this before proceeding with the method (see 10.1). 5 Reagents During the analysis, use only reagents of analytical grade, and only water as specified in 5.1. 5.1 Water, complyi
39、ng with the requirements for ISO 3696 grade 2 water (electrical conductivity less than 0,1 mS/m and resistivity greater than 0,01 Mm at 25 C). 5.2 Nitric acid, (HNO3), concentrated, r 1,42 g/ml, 69 % (m/m) to 71 % (m/m). The concentration of cadmium shall be less than 0,01 g/ml. WARNING Concentrated
40、 nitric acid is corrosive and oxidizing, and nitric acid fumes are irritant. Avoid exposure by contact with the skin or eyes, or by inhalation of fumes. Personal protective equipment (e.g. gloves, face shield or safety spectacles, etc.) must be used when working with the concentrated or diluted nitr
41、ic acid, and concentrated nitric acid must be used in a fume hood. 5.3 Nitric acid, diluted 1 + 1. Carefully add 500 ml of concentrated nitric acid (5.2) to 450 ml of water (5.1) in a 2 litre beaker. Swirl to mix, allow to cool and quantitatively transfer to a 1 000 ml one-mark volumetric flask (6.2
42、.1.5). Dilute to the mark with water, stopper and mix thoroughly. 5.4 Nitric acid, diluted 1 + 9. Pour approximately 800 ml of water (5.1) into a 1 000 ml one-mark volumetric flask (6.2.1.5). Carefully add 100 ml of concentrated nitric acid (5.2) to the flask and swirl to mix. Allow to cool, dilute
43、to the mark with water, stopper and mix thoroughly. 5.5 Cadmium stock standard solution, corresponding to 1 000 mg of Cd per litre. 5.5.1 Use a commercially available cadmium standard solution at a concentration of 1 000 mg/l. Observe the manufacturers expiry date or recommended shelf-life. Alternat
44、ively, prepare a cadmium standard solution according to the procedure specified in 5.5.2. 5.5.2 Accurately weigh 1,000 g 0,001 g of cadmium metal, 99,9 % (m/m) of Cd, into a 50 ml beaker (6.2.1.1), add 20 ml of the nitric acid diluted 1 + 1 (5.3), cover with a watch glass (6.2.1.2) and heat to appro
45、ximately 150 C on the hotplate (6.2.4) in a fume hood until the metal is completely dissolved. Remove the beaker from the hotplate, allow to cool, quantitatively transfer the solution to a 1 000 ml one-mark volumetric flask (6.2.1.5), dilute to the mark with water (5.1), stopper and mix thoroughly.
46、This solution may be stored in a polypropylene bottle (6.2.2) for up to one year. 5.6 Cadmium working standard solution A, corresponding to 100 mg of Cd per litre. Using a pipette (6.2.1.3), accurately add 10,0 ml of stock cadmium solution (5.5) to a 100 ml one-mark volumetric flask (6.2.1.5). Add 1
47、 ml of concentrated nitric acid (5.2), dilute to the mark with water (5.1), stopper and mix thoroughly. This solution may be stored in a polypropylene bottle (6.2.2) for up to one month. 5.7 Cadmium working standard solution B, corresponding to 1 mg of Cd per litre. Using a pipette (6.2.1.3), accura
48、tely add 100 l of cadmium stock solution (5.5) to a 100 ml one-mark volumetric flask (6.2.1.5). Add 1 ml of nitric acid (5.2), dilute to the mark with water (5.1), stopper and mix thoroughly. This solution may be stored in a polypropylene bottle (6.2.2) for up to one month. Licensed Copy: London Sou
49、th Bank University, London South Bank University, Tue Jan 30 01:19:31 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 11174:1996 BSI 12-19983 5.8 Matrix-modifier solution, corresponding to 1 g of Mg(NO3)26H2O per litre and 20 g of NH4H2PO4 per litre. Weigh 0,100 g of magnesium nitrate hexahydrate Mg(NO3)26H2O and 2,00 g of ammonium dihydrogen phosphate (NH4H2PO4) into a 250 ml beaker (6.2.1.1). Add 50 ml of water (5.1) and swirl to dissolve. Add 10 ml of concentrated nitric acid (5.2), swirl to mix, and