1、DRAFT FOR DEVELOPMENT 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 a ICs 77.150.60 a DD ENV 14029:2001 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGH
2、T LAW DD ENV 14029:2001 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 Development series of publications and is of a provisional nature because, althoug
3、h 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 should be applied on this provisional basis, so that information and exp
4、erience 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 into a European Standard. A review of this publication will be initiated 2
5、 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 Standards. According to the replies received by the end of the review period,
6、 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 Technical Committee NFE22, Lead and lead alloys, at 389 Chiswick High Road, Londo
7、n 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. Cross-references The British Standards which implement international or Eur
8、opean 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 Electronic Catalogue. This Draft for Development, having been prepared under the
9、 direction of the Engineering Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 September 2001 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 co
10、ver. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. IDate I Comments O BSI 07-2001 ISBN O 580 37219 7 ENV 14029 EUROPEAN PRESTANDARD PRNORME EUROPENNE EUROPISCHE VORNORM July 2001 ICs 77.040.30; 77.120.60 En
11、glish version 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 Plomb et alliages de plomb - Analyse par spectromtrie dabsorption atomique dans la flamme (FAAS) ou spectromt
12、rie dmission atomique plasma inductif 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 Prestan
13、dard (ENV) was approved by CEN on 9 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
14、 be converted 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 E
15、NV) until the 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
16、, Switzerland and United Kingdom. EUROPEAN COMMEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 0 2001 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members.
17、 Ref. No. ENV 14029:2001 E ENV 14029:2001 Contents Page Foreword 3 1 2 3 3.1 3.2 4 4.1 4.2 4.3 4.4 5 5.1 5.2 5.3 5.4 5.5 6 7 7.1 7.2 7.3 7.4 8 8.1 8.2 8.3 9 9.1 9.2 9.3 10 Scope . 4 Normative references 5 Principle 5 Preparation of the test solution 5 Instrumental techniques 5 Apparatus . 6 General
18、6 Volumetric glassware 6 Filtration system . 6 Instruments . 6 Reagents . 6 General 6 Nitric acid (“03) 7 Hydrochloric acid (HCI) . 7 Pure lead . 7 Standard solutions . 7 Sampling and sample preparation . 9 Procedure . 9 Preparation of the test solution 9 Preparation of the synthetic test solution .
19、 9 Preparation of the blank test solution . 9 Preparation of calibration solutions 10 General 10 Calibration and measurement of the test solution . 11 Expression of results . 12 Determination of elements by ICP-ES 13 General 13 Calibration and measurement of the test solution . 14 Expression of resu
20、lts . 14 Test report 14 Determination of elements by FAAS 10 . O 2 . ENV 14029:2001 Foreword This European Prestandard has been prepared by Technical Committee CENTTC 306, “Lead and lead alloys“, the secretariat of which is held by AFNOR. CAUTION FOR SAFETY AND TRAINING The methods in this standard
21、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 carried out by fully-trained analysts who are experienced in all relevant techniques an
22、d 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 particular hazard exists, this is given as a DANGER adjacent to the point in the text where the
23、apparatus or reagent is referenced. According to the CENKENELEC Internal 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,
24、 Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. 3 ENV 14029:2001 1 Scope This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-ES) for the determination of
25、 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 Element Ag AI As Bi Ca Cd Co Cr Cu Fe Mg Mn Na Ni Sb Se Sn Te TI Zn Ranges of
26、applications (% dm) FAAS 0,00001 0,0001 0,0002 0,00005 0,00005 0,00005 0,00005 0,00005 0,00001 0,00005 0,00005 0,00005 0,00005 0,00005 0,0002 0,0002 0,0005 0,00002 0,00002 0,00001 - 0,001 - 0,005 - 0,005 - 0,0025 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,001 - 0,002
27、5 - 0,005 - 0,005 - 0,0025 - 0,0025 - 0,001 ICP-ES 0,00001 - 0,001 0,00005 - 0,005 0,00005 - 0,005 0,00005 - 0,0025 0,00001 - 0,001 0,00001 - 0,001 0,00005 - 0,001 0,00005 - 0,001 0,00001 - 0,001 0,00005 - 0,001 0,00005 - 0,001 0,00005 - 0,001 0,00001 - 0,001 0,00001 - 0,001 0,0002 - 0,0025 0,0002 -
28、 0,005 0,0002 - 0,005 0,00002 - 0,0025 0,00002 - 0,0025 0,00001 - 0,001 These 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 Ma
29、terials (RM) which are used in analysis according to ENV 12908. 4 ENV 14029:2001 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publicatio
30、ns 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 references the latest edition of the publication referred to applies (including amendme
31、nts). 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 flame atomic absorption spectrometry (FAAS) or inductively coupled plasma em
32、ission spectrometry (ICP-ES), without separation of the lead matrix. IS0 648:1977, Laboratory glassware - One-mark pipettes. IS0 1042:1998, Laboratory glassware - One-mark volumetric flasks. IS0 3696, Water for analytical laboratory use - Specification and test methods. 3 Principle 3.1 Preparation o
33、f 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 one of the two techniques described in 3.2. 3.2 Instrumental techniques 3.
34、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 absorption of the resonance line energy of the spectrum from the element at the
35、 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 solution is obtained by: nebulization of the test solution into the plasma of a
36、n 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-matched calibration solutions of the same element. 5 ENV 14029:2001 4 Apparatus
37、 4.1 General Use ordinary apparatus as available in a chemical laboratory. All glassware to be used shall be cleaned with diluted nitric acid (5.2.2) and thoroughly rinsed with water. 4.2 Volumetric glassware 4.2.1 One-mark volumetric flasks of capacities 20 ml, 200 ml, 500 ml, and 1 O00 ml in accor
38、dance with IS0 1042:1998 class A. 4.2.2 One-mark pipettes of capacities 2 ml, 5 ml, 10 ml, and 50 ml in accordance with IS0 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 pm porosity (filtering diame
39、ter 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 flames, and with radiation sources such as hollow cathode lamps (HCL) or
40、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 the IS0 documents in preparation, numbers 00023056 and 00023057). DANGER exhausted externally. To
41、avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be 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 instrume
42、nt where a monochromator system allows the selection of wavelengths (see also the IS0 document in preparation number 00021288). The instrument shall be used in accordance with the manufacturers instructions and the performances checked (see also the IS0 document in preparation, number 00023058). DAN
43、GER exhausted externally. To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be 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 an
44、alysis, and only water of at least grade 2, as specified in IS0 3696. Prepare all solutions using the same container of each reagent. ENV 14029:2001 5.2 Nitric acid (“0,) O 5.2.1 Concentrated nitric acid Nitric acid of high purity, which p20 = 1,41 g/ml. 5.2.2 Nitric acid 1:l (vh) Add to one volume
45、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 (vh) Add 200 ml nitric acid (5.2.1) to 400 ml water in a 1 O00 ml beaker and mix thoroughly. 5.3 Hydrochloric acid (HCI)
46、Hydrochloric acid of high purity, which p20 = 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 sig
47、nificant to the determination required. 5.5 Standard solutions 5.5.1 Standard solutions (1 gl) 5.5.1.1 General Either use commercially available certified standard solutions or prepare standard solutions as described in 5.5.1.2 to 5.5.1.10. 5.5.1.2 nickel, thallium and zinc Solutions for silver, bis
48、muth, cadmium, cobalt, chromium, iron, manganese, magnesium, copper, Weigh (1,O * 0,001) g of the relevant metal (99,99 Yo m/m minimum purity) and transfer into a 250 ml beaker. Add 75 ml of nitric acid (5.2.3), cover with a watch glass and heat gently until dissolution is complete. Allow to cool, t
49、hen transfer into a 1 O00 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. Store the silver solution in the dark. 5.5.1.3 Solution for aluminium The aluminium used for this solution shall be in a form of clean wire, foil, or pieces cut or milled from an ingot. Do not use aluminium powder because of possible oxidation of the very large specific surface involved. Weigh (1,000 * 0,001) g of aluminium (99,99 Yo rn/m minimum purity) and transfer into a 250 ml beaker, add 10 ml of hydrochloric acid (5.3), cover with a watch glass, and heat
