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1、DRAFT FOR DEVELOPMENT DD ENV 14029:2001 Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation of the lead matrix ICS 77.150.60 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW
2、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 14029:2001 This Draft for Development, having been prepared under the direction of the Engineering Sector Committee, was published under the authority of t
3、he Standards Committee and comes into effect on 15 September 2001 BSI 07-2001 ISBN 0 580 37219 7 National foreword This Draft for Development is the English language version of ENV 14029:2001. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Developme
4、nt series of publications and is of a provisional nature because, although the analytical procedures in the method are generally recognised, the evaluation of the method via Round-Robin analyses, together with the resultant statistical validation, as required by CEN, has not yet been carried out. It
5、 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 responsible for its conversion i
6、nto 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 announcement in Update Stan
7、dards. 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 the Secretary of BSI Technica
8、l 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 request to its secretary. C
9、ross-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 of the BSI Standards Electr
10、onic 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. Amendments issued since publication
11、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 14029 July 2001 ICS 77.040.30; 77.120.60 English version Lead and lead alloys
12、- Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation of the lead matrix Plomb et alliages de plomb - Analyse par spectromtrie dabsorption atomique dans la flamme (FAAS) ou spectromtrie dmission atomique plasma induct
13、if coupl (ICP-ES), aprs sparation de la matrice plomb Blei und Bleilegierungen - Analyse durch Flammen- Atomabsorptionsspektrometrie (FAAS) oder Emissions - Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES), nach Abtrennung der Bleimatrix This European Prestandard (ENV) was approved by CEN on 9
14、 June 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 into a European Stand
15、ard. 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 final decision about
16、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 and United Kingdom. E
17、UROPEAN 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 14029:2001 E Licensed C
18、opy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 2 Contents page Foreword3 1Scope.4 2Normative references 5 3Principle5 3.1Preparation of the test solution5 3.2Instrumental techniques5 4Apparatus .6 4.1
19、General6 4.2Volumetric glassware6 4.3Filtration system 6 4.4Instruments.6 5Reagents.6 5.1General6 5.2Nitric acid (HNO3) 7 5.3Hydrochloric acid (HCl).7 5.4Pure lead.7 5.5Standard solutions.7 6Sampling and sample preparation.9 7Procedure .9 7.1Preparation of the test solution9 7.2Preparation of the sy
20、nthetic test solution.9 7.3Preparation of the blank test solution .9 7.4Preparation of calibration solutions 10 8Determination of elements by FAAS10 8.1General10 8.2Calibration and measurement of the test solution.11 8.3Expression of results.12 9Determination of elements by ICP-ES13 9.1General13 9.2
21、Calibration and measurement of the test solution.14 9.3Expression of results.14 10Test report 14 ENV 14029:2001 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 3 Foreword This European Presta
22、ndard has been prepared by Technical Committee CEN/TC 306, “Lead and lead alloys“, the secretariat of which is held by AFNOR. CAUTION FOR SAFETY AND TRAINING The methods in this standard are recommended for the certification of reference materials and as umpire methods in cases of a dispute. The imp
23、ortance of either application, and the paramount issue of safety, requires that they should only be 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
24、using particularly hazardous apparatus and reagents used in some of these methods. Where a particular hazard exists, this is given as a DANGER adjacent to the point in the text where the apparatus or reagent is referenced. According to the CEN/CENELEC Internal Regulations, the national standards org
25、anizations 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 and the United Kingdom. ENV 14029:2001 Li
26、censed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 4 1 Scope This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission s
27、pectrometry (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 determined according to ENV 13800. Table 1 Ranges of application for the determination of elements Ranges of applications (% m/m)Eleme
28、nt FAASICP-ES Ag0,00001-0,0010,00001-0,001 Al0,0001-0,0050,00005-0,005 As0,0002-0,0050,00005-0,005 Bi0,00005-0,00250,00005-0,0025 Ca0,00005-0,0010,00001-0,001 Cd0,00005-0,0010,00001-0,001 Co0,00005-0,0010,00005-0,001 Cr0,00005-0,0010,00005-0,001 Cu0,00001-0,0010,00001-0,001 Fe0,00005-0,0010,00005-0,
29、001 Mg0,00005-0,0010,00005-0,001 Mn0,00005-0,0010,00005-0,001 Na0,00005-0,0010,00001-0,001 Ni0,00005-0,0010,00001-0,001 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 TI0,00002-0,00250,00002-0,0025 Zn0,00001-0,0010,00001-0,001 These
30、methods are 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. ENV 14029:2001
31、 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 5 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normativ
32、e 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 publications apply to this European Standard only when incorporated in it by amendment or revision. For undated referenc
33、es 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 alloys - Analysis by Optical Emission Spectrometry (OES) with spark excitation. ENV 13800, Lead and lead alloys Analysis by
34、 flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrix. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1998, Laboratory glassware One-mark volumetric flasks. ISO 3696, Water for analytical labor
35、atory use - Specification and test methods. 3 Principle 3.1 Preparation of the test solution Dissolution of a test portion in nitric acid. Separation of lead by crystallisation as lead nitrate. Reduction of the test solution to a defined volume, and determination of the analyte concentration using o
36、ne of the two techniques described in 3.2. 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; ? measurement of the absorp
37、tion of the resonance line energy of the spectrum from the element at the relevant wavelength (absorbance); ? comparison with that of matrix-matched calibration solutions of the same element. 3.2.2 Inductively coupled plasma emission spectrometry (ICP-ES) The analyte concentration in the test soluti
38、on 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 that of matrix-
39、matched calibration solutions of the same element. ENV 14029:2001 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 6 4 Apparatus 4.1 General Use ordinary apparatus as available in a chemical l
40、aboratory. All glassware to be used shall be cleaned with diluted nitric acid (5.2.2) and thoroughly rinsed with water. 4.2 Volumetric glassware 4.2.1One-mark volumetric flasks of capacities 20 ml, 200 ml, 500 ml, and 1 000 ml in accordance with ISO 1042:1998 class A. 4.2.2One-mark pipettes of capac
41、ities 2 ml, 5 ml, 10 ml, and 50 ml in accordance with ISO 648:1977 class A. 4.3 Filtration system Vacuum filtration system with a filter membrane of PTFE, or other 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
42、spectrometer Flame atomic absorption spectrometer (FAAS) equipped with laminar flow burners suitable for acetylene-air, hydrogen-air or acetylene-nitrous oxide flames, and with radiation sources such as hollow cathode lamps (HCL) or electrode-less discharge lamps (EDL) as appropriate to the element
43、to be determined. The instrument shall be used in accordance with the manufacturers instructions and the performance checked (see also the ISO documents in preparation, numbers 00023056 and 00023057). DANGERTo avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be e
44、xhausted externally. 4.4.2 Inductively 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
45、(see also the ISO document in preparation number 00021288). The instrument shall be used in accordance with the manufacturers instructions and the performances checked (see also the ISO document in preparation, number 00023058). DANGERTo avoid any risk to personnel due to emission of acid and lead f
46、umes, the off-gas shall be exhausted externally. 5 Reagents 5.1 General For all stages of analysis, unless otherwise stated, use only reagents suitable for trace analysis of recognised analytical grade, preferably with an actual analysis, and only water of at least grade 2, as specified in ISO 3696.
47、 Prepare all solutions using the same container of each reagent. ENV 14029:2001 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:49:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI VNE 41:9202100 (E) 7 5.2 Nitric acid (HNO3) 5.2.1 Concentrated nitric acid Nitric
48、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 nitric acid (5.2.1) and mix thoroughly. This diluted acid is also used to clean the laboratory ware. 5.2.3 Nitric acid 1:2 (v/v) Add 200 ml nitric acid (5.
49、2.1) to 400 ml water in a 1 000 ml beaker and mix thoroughly. 5.3 Hydrochloric acid (HCl) Hydrochloric acid of high purity, which ?20 = 1,18 g/ml. 5.4 Pure lead For the determination of the recovery rate of the analyte (see 7.2), very pure lead (99,9999 % m/m) should be used. However, lead of lower purity may be used provided that the analyte is not present in an amount that could be significant to the determination required. 5.5 Standard solutions 5.5.1 Standard solutions (1 g/l) 5.5.1.1 General Either use commercially available certified standard solution