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1、DRAFT FOR DEVELOPMENT DD ENV 14138:2001 Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emissions spectrometry (ICP-ES), after separation by co-precipitation ICS 77.120.60 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LA
2、W Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD ENV 14138:2001 This Draft for Development, having been prepared under the direction of the Engineering Sector Policy and Strategy Committee, was published un
3、der the authority of the Standards Policy and Strategy Committee on 21 December 2001 BSI 21 December 2001 ISBN 0 580 38084 X National foreword This Draft for Development is the English language version of ENV 14138:2001. This publication is not to be regarded as a British Standard. It is being issue
4、d in the Draft for Development series of publications and is of a provisional nature because, although the analytical procedures in the method are generally recognized, the evaluation of the method via Round-Robin analyses, together with the resultant statistical validation, as required by CEN, has
5、not yet been carried out. It should be applied on this provisional basis, so that information and experience of its practical application may be obtained. Comments arising from the use if this Draft for Development are requested so that UK experience can be reported to the European organization resp
6、onsible for its conversion into a European Standard. A review of this publication will be initiated 2 years after its publication by the European organization so that a decision can be taken on its status at the end of its three-year life. The commencement of the review period will be notified by an
7、 announcement in Update Standards. According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the prestandard or to withdraw it. Comments should be sent in writing to t
8、he Secretary of BSI Technical Committee NFE/22, Lead and lead alloys, at 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on
9、 request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility
10、 of the BSI Standards Electronic Catalogue. Summary of pages This document comprises a front cover, an inside front cover, the ENV title page, pages 2 to 14, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendmen
11、ts issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN PRESTANDARD PRNORME EUROPENNE EUROPISCHE VORNORM ENV 14138 December 2001 ICS 77.120.60 English version
12、Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation by co-precipitation Plomb et alliages de plomb - Analyse par spectromtrie dabsorption atomique dans la flamme (FAAS) ou par spectromtrie dmiss
13、ion plasma inductif coupl (ICP- ES), aprs sparation par co-prcipitation Blei und Bleilegierungen - Analyse durch Flammen- Atomabsorptionsspektrometrie (FAAS) oder Emission- Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES), nach Abtrennung durch Mitfllung This European Prestandard (ENV) was app
14、roved by CEN on 18 November 2001 as a prospective standard for provisional application. The period of validity of this ENV is limited initially to three years. After two years the members of CEN will be requested to submit their comments, particularly on the question whether the ENV can be converted
15、 into a European Standard. CEN members are required to announce the existence of this ENV in the same way as for an EN and to make the ENV available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the
16、 final decision about the possible conversion of the ENV into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland
17、 and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. ENV 1
18、4138:2001 E Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 2 Contents page Foreword4 1Scope 5 2Normative references 5 3Principle5 3.1Preparation of the test solution5 3.2Instrumental techniq
19、ues .6 3.2.1Flame atomic absorption spectrometry (FAAS).6 3.2.2Inductively coupled plasma emission spectrometry (ICP-ES)6 4Apparatus .6 4.1General6 4.2Volumetric glassware6 4.3Filtration system 6 4.4Instruments.6 4.4.1Flame atomic absorption spectrometer 6 4.4.2Inductively coupled plasma emission sp
20、ectrometer .7 5Reagents.7 5.1General7 5.2Nitric acid (HNO3) 7 5.2.1Concentrated nitric acid7 5.2.2Nitric acid 1:1 (V/V) 7 5.2.3Nitric acid 1:2 (V/V) 7 5.3Hydrochloric acid (HCl).7 5.3.1Concentrated hydrochloric acid.7 5.3.2Hydrochloric acid 1:1 (V/V).7 5.4Ammonia solution7 5.5Pure lead.7 5.6Manganes
21、e nitrate solution 8 5.7Potassium permanganate solution8 5.8Standard solutions 8 5.8.1Standard solutions (1g/l).8 5.8.2Standard solutions (100 mg/l).8 5.8.3Standard solutions (10 mg/l).9 5.8.4Multi-element solutions (either 10 mg/l or 100 mg/l)9 6Sampling and sample preparation.9 7Procedure .9 7.1Pr
22、eparation of the test solution9 7.1.1Dissolution9 7.1.2Co-precipitation with manganese dioxide.9 7.1.3Test solution.9 7.2Preparation of the synthetic test solution.9 7.3Preparation of the blank test solution .10 7.4Preparation of calibration solutions 10 8Determination of elements by FAAS10 8.1Gener
23、al10 8.2Calibration and measurement of the test solution.11 8.3Expression of results 11 8.3.1Analyte recovery rate 11 8.3.2Analyte content in the sample11 9Determination of elements by ICP-ES .12 9.1General12 9.2Calibration and measurement of the test solution.12 Licensed Copy: London South Bank Uni
24、versity, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 3 9.3Expression of results 13 9.3.1Analyte recovery rate 13 9.3.2Analyte content in the sample13 10Test report13 Bibliography14 Licensed Copy: London South Bank University, London
25、 South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 4 Foreword This European Prestandard has been prepared by Technical Committee CEN /TC 306, “Lead and lead alloys“, the secretariat of which is held by AFNOR. According to the CEN/CENELEC Interna
26、l Regulations, the national standards organizations of the following countries are bound to announce this European Prestandard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland
27、and the United Kingdom. CAUTION FOR SAFETY AND TRAINING The methods in this Prestandard are recommended for the certification of reference materials and as umpire methods in cases of a dispute. The importance of either application, and the paramount issue of safety, requires that they should only be
28、 carried out by fully-trained analysts who are experienced in all relevant techniques and the precautions necessary in the inherently hazardous environs of a laboratory, especially those required when using particularly hazardous apparatus and reagents used in some of these methods. Where a particul
29、ar hazard exists, this is given as a DANGER adjacent to the point in the text where the apparatus or reagent is referenced. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 5 1 Scope This Euro
30、pean Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-ES) for the determination of elements at low content in lead for the ranges given in Table 1. Higher contents than those listed in Table 1 should be determin
31、ed according to ENV 13800. Table 1 Ranges of application for the determination of elements Ranges of applications (% m/m) Element FAASICP-ES As0,0002-0,0050,00005-0,005 Sb0,0002-0,00250,0002-0,0025 Se0,0002-0,0050,0002-0,005 Sn0,0005-0,0050,0002-0,005 Te0,00002-0,00250,00002-0,0025 These methods are
32、 intended as the definitive methods in case of dispute for the determination of elements at low content in lead. They are also recommended for the analysis of Certified Reference Materials (CRM) and Reference Materials (RM) which are used in analysis according to ENV 12908. 2 Normative references Th
33、is European Prestandard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these pu
34、blications apply to this European Prestandard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN 12402, Lead and lead alloys - Methods of sampling for analysis. ENV 12908, Lead and lead al
35、loys - Analysis by Optical Emission Spectrometry (OES) with spark excitation. ENV 13800, Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrix. ISO 648, Laboratory glassware One
36、-mark pipettes. EN ISO 1042, Laboratory glassware One-mark volumetric flasks (ISO 1042:1998). EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987). 3 Principle 3.1 Preparation of the test solution Dissolution of a test portion in nitric acid. Separation o
37、f analyte by co-precipitation with manganese dioxide. Dissolution of the precipitate, made up to a defined volume. Determination of the analyte concentration using one of the two techniques described in 3.2. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:
38、06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 6 3.2 Instrumental techniques 3.2.1 Flame atomic absorption spectrometry (FAAS) The analyte concentration in the test solution is obtained by : ? nebulization of the test solution into the flame of an atomic absorption spectrometer ; ?
39、 measurement of the absorption of the resonance line energy of the spectrum from the element at the relevant wavelength (absorbance) ; ? comparison with that of calibration solutions of the same element. 3.2.2 Inductively coupled plasma emission spectrometry (ICP-ES) The analyte concentration in the
40、 test solution is obtained by : ? nebulization of the test solution into the plasma of an inductively coupled plasma optical emission spectrometer ; ? measurement of the intensity of the emission signal from the spectrum of the element to be determined at the relevant wavelength ; ? comparison with
41、that of calibration solutions of the same element. 4 Apparatus 4.1 General Use ordinary apparatus as available in a chemical laboratory. All glassware to be used shall be cleaned with diluted hydrochloric acid (5.3.2) and thoroughly rinsed with water. 4.2 Volumetric glassware 4.2.1One-mark volumetri
42、c flasks of capacities 25 ml, 100 ml, 500 ml and 1 000 ml in accordance with EN ISO 1042 class A. 4.2.2One-mark pipettes of capacities 5 ml, 10 ml, 15 ml, 20 ml, 25 ml and 50 ml in accordance with ISO 648 class A. 4.3 Filtration system Vacuum filtration system with a filter membrane of PTFE, or othe
43、r material inert to nitric acid, of about 5 m porosity (filtering diameter 20 mm to 50 mm). 4.4 Instruments 4.4.1 Flame atomic absorption spectrometer Flame atomic absorption spectrometer (FAAS) equipped with laminar flow burners suitable for acetylene-air, hydrogen-air or acetylene-nitrous oxide fl
44、ames, and with radiation sources such as hollow cathode lamps (HCL) or electrode-less discharge lamps (EDL) as appropriate to the element to be determined. The instrument shall be used in accordance with the manufacturers instructions and the performance checked (see also ISO/DIS 13204-2 and ISO/DIS
45、 13204-3). DANGERTo avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be exhausted externally. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ENV 14138:2001 (E) 7 4.4.2 Indu
46、ctively coupled plasma emission spectrometer Inductively coupled plasma emission spectrometer (ICP-ES), either a simultaneous instrument with the relevant wavelengths installed or a sequential instrument where a monochromator system allows the selection of wavelengths (see also ISO/DIS 12235-1). The
47、 instrument shall be used in accordance with the manufacturers instructions and the performances checked (see also ISO/DIS 12235-2). DANGERTo avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be exhausted externally. 5 Reagents 5.1 General For all stages of analys
48、is, unless otherwise stated, use only reagents of recognised analytical grade, preferably with an actual analysis, suitable for trace analysis and only water of at least grade 2, as specified in EN ISO 3696. Prepare all solutions using the same container of each reagent. 5.2 Nitric acid (HNO3) 5.2.1
49、 Concentrated nitric acid Nitric acid of high purity, which ?20 = 1,41 g/ml. 5.2.2 Nitric acid 1:1 (V/V) Add to one volume of water, in a suitable container, the same volume of concentrated nitric acid (5.2.1) and mix thoroughly. 5.2.3 Nitric acid 1:2 (V/V) Add 200 ml concentrated nitric acid (5.2.1) to 400 ml water in a 1 000 ml beaker and mix thoroughly. 5.3 Hydrochloric acid (HCl) 5.3.1 Concentrated hydrochloric acid Hydrochloric acid of high purity, which ?20 = 1,18 g/ml. 5.3.2 Hydrochloric acid 1:1 (V/V) Add 400 ml of concentrated hydrochloric acid (