1、BRITISH STANDARD BS EN ISO 3815-2:2005 Zinc and zinc alloys Part 2: Analysis by inductively coupled plasma optical emission spectrometry The European Standard EN ISO 3815-2:2005 has the status of a British Standard ICS 77.120.60; 77.040.30 BS EN ISO 3815-2:2005 This British Standard was published un
2、der the authority of the Standards Policy and Strategy Committee on 31 October 2005 BSI 31 October 2005 ISBN 0 580 46795 3 National foreword This British Standard is the official English language version of EN ISO 3815-2:2005. It is identical with ISO 3815-2:2005. BS EN ISO 3815-2 together with BS E
3、N ISO 3815-1 supersedes BS EN 12019:1998, which is withdrawn The UK participation in its preparation was entrusted to Technical Committee NFE/8, Zinc, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on t
4、he interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards
5、 which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This pub
6、lication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front co
7、ver, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 6, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No.
8、 Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO38152 July2005 ICS77.120.60;77.040.30 SupersedesEN12019:1997 EnglishVersion ZincandzincalloysPart2:Analysisbyinductivelycoupled plasmaopticalemissionspectrometry(ISO38152:2005) ZincetalliagesdezincPartie2:Analysepar spectromtriedmissi
9、onoptiqueavecsourceplasma couplageinductif(ISO38152:2005) ZinkundZinklegierungenTeil2:Optische Emissionsspektrometriemitinduktivgekoppelter Plasmaanregung(ISO38152:2005) ThisEuropeanStandardwasapprovedbyCENon12May2005. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatethec
10、onditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,Germa
11、n).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,
12、Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels
13、2005CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO38152:2005:E Foreword This document (EN ISO 3815-2:2005) has been prepared by Technical Committee ISO/TC 18 “Zinc and zinc alloys“ in collaboration with Technical Committee CEN/TC 209 “Zinc and
14、zinc alloys“, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2006, and conflicting national standards shall be withdrawn at the latest by Januar
15、y 2006. This document supersedes EN 12019:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gree
16、ce, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 3815-2:2005 has been approved by CEN as EN ISO 3815-2:2005 without any modification
17、s. EN ISO 3815-2:2005 Reference number ISO 3815-2:2005(E)INTERNATIONAL STANDARD ISO 3815-2 First edition 2005-07-15 Zinc and zinc alloys Part 2: Analysis by inductively coupled plasma optical emission spectrometry Zinc et alliages de zinc Partie 2: Analyse par spectromtrie dmission optique avec sour
18、ce plasma couplage inductif EN ISO 3815-2:2005ii iii 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 committees. E
19、ach 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 Internati
20、onal Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standa
21、rds 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 bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject
22、 of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 3815-2 was prepared by Technical Committee ISO/TC 18, Zinc and zinc alloys, Subcommittee SC 1, Methods of sampling and analysis of zinc and zinc alloys. This first edition of ISO 3815-2 cancels an
23、d replaces ISO 3815:1976, which has been technically revised. ISO 3815 consists of the following parts, under the general title Zinc and zinc alloys: Part 1: Analysis of solid samples by optical emission spectrometry Part 2: Analysis by inductively coupled plasma optical emission spectrometry EN ISO
24、 3815-2:2005blank1 Zinc and zinc alloys Part 2: Analysis by inductively coupled plasma optical emission spectrometry 1 Scope This part of ISO 3815 specifies analytical methods for determining the chemical composition of zinc and zinc alloys in accordance with ISO 301 and ISO 752 by inductively coupl
25、ed plasma optical emission spectrometry. This part of ISO 3815 includes provisions for preparation of test solutions and calibration solutions for zinc and zinc alloys. The ranges specified for each method can be extended and/or adapted for determinations of low concentrations. This part of ISO 3815
26、 can be applied to other elements (e.g. Ni, Cr and Ti). However, such results will need to be carefully checked by taking into account the interferences, the sensitivity, the resolution and the linearity criteria for each instrument and each wavelength. 2 Normative references The following reference
27、d documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 301, Zinc alloy ingots intended for casting ISO 752, Zinc ingots ISO
28、 1169, Zinc alloys Determination of aluminium content Volumetric method ISO 20081: 1) , Zinc and zinc alloys Method of sampling Specifications EN 988, Zinc and zinc alloys Specifications for rolled flat products for building EN 12844, Zinc and zinc alloys Castings Specifications 1) To be published.
29、EN ISO 3815-2:2005EN ISO 3815-2:2005 2 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 301, ISO 752, ISO 20081 and the following apply. 3.1 inductively coupled plasma optical emission spectrometry measurement of the intensity of electromagnetic radia
30、tion emitted by the components of a sample when excited by a plasma NOTE A plasma is a high-temperature emission source generated by an RF field consisting of a mixture of argon atoms, argon ions and electrons. Sample atoms entering the plasma emit light radiation, whose characteristic wavelengths a
31、nd intensities are used to identify the elements and determine concentrations, respectively. Samples are usually presented to the plasma in solution form. 4 Principle A sample of the metal or alloy is dissolved in a mixture of nitric and tartaric acid, and after adequate dilution and atomization of
32、the solution in an inductively coupled plasma, the content of the particular elements is determined by optical emission spectrometry. 5 Reagents During the test, use only reagents of known or analytical grade and distilled or demineralized water. 5.1 Hydrochloric acid, = 1,19 g/ml. 5.2 Nitric acid,
33、= 1,4 g/ml. 5.3 Tartaric acid, solid. 5.4 Tartaric acid solution, 25 g/l. 5.5 Zinc, purity 99,999 % (mass fraction), free of lead, cadmium, iron, tin, copper, magnesium, nickel, chromium and titanium. 5.6 Aluminium nitrate nonahydrate, heavy metal impurities: lead max. 0,002 %, iron max. 0,001 %. 5.
34、7 Acid mixture Dissolve 1 g of tartaric acid (5.3) in about 500 ml of water in a 1 000 ml volumetric flask, add 200 ml of nitric acid (5.2), dilute to the mark with water and mix. 5.8 Zinc solution Prepare a solution of 100 g/l by carefully dissolving 100 g of zinc (5.5), weighed to the nearest 0,1
35、g, with a minimum of nitric acid (5.2), added in small increments. Transfer to a 1 l volumetric flask, add 40 ml of tartaric acid solution (5.4) and, after cooling to room temperature, dilute to the mark with water and mix. It is recommended to verify the purity of the zinc used (absence of analyte
36、elements). If any analyte element is present, determine its concentration by the standard addition method and take this concentration into account in the calibration standards (see 8.2). EN ISO 3815-2:2005 3 5.9 Mono-element standard solutions Prepare solutions of 1 g/l of lead, cadmium, iron, coppe
37、r, aluminium and magnesium, by dissolving 1 g of each of these metals, weighed to the nearest 0,001 g, in the acid mixture (5.7) and making up to volume with the acid mixture (5.7). Prepare a solution of 1 g/l of tin, by carefully adding 100 ml of hydrochloric acid (5.1) to 1 g of pure tin. When dis
38、solution is complete, cool and transfer quantitatively to a 1 000 ml volumetric flask. Dilute to the mark with water and mix. By dilution, prepare standard solutions of 100 mg/l and 10 mg/l, if necessary (see 8.2). 5.10 Aluminium standard solution, to be used for alloys with aluminium content 3 % (m
39、ass fraction). Prepare a solution of 50 g/l by dissolving 695,2 g of aluminium nitrate nonahydrate (5.6), weighed to the nearest 0,1 g, in water. Transfer to a 1 l volumetric flask, add 40 ml of tartaric acid solution (5.4), dilute to the mark with water and mix. By taking an appropriate aliquot, de
40、termine the exact aluminium content in accordance with ISO 1169. 5.11 Internal standard solution Weigh 6,25 g of Y 2 O 3(yttrium oxide p.a.), to the nearest 0,01 g, and transfer into a 5 l volumetric flask. Add about 2,5 l of water, 250 ml of nitric acid (5.2) and warm gently until dissolution. Cool
41、 to room temperature, dilute to the mark with water, and mix. 6 Sampling Sampling shall be in accordance with ISO 20081. 7 Preparation of test solutions 7.1 Test portion Weigh 10 g of the test sample to the nearest 0,001 g. 7.2 Preparation of the test solution Introduce the test portion into a 500 m
42、l beaker fitted with a watch-glass cover and dissolve by carefully adding 10 ml of tartaric acid solution (5.4) and 50 ml of nitric acid (5.2). Alternatively, dissolve the test portion in 50 ml of hydrochloric acid-nitric acid mixture (45+1). In this case, zinc solution (5.8) and standard solutions
43、(5.9), (5.10) are also prepared such that the resulting calibration solutions (8.2) have an acid composition identical to the sample solution. After dissolution, transfer quantitatively to a 250 ml volumetric flask, add 10 ml of internal standard solution (5.11) and, after cooling to room temperatur
44、e, make up to the mark with water and mix. 4 8 Test procedure 8.1 General Carry out the test by optical emission spectrometry with plasma source, using test solutions prepared in accordance with Clause 7. For the analysis of the impurities and alloying elements in zinc and zinc alloys, as defined in
45、 ISO 301 and ISO 752, by optical emission spectrometry, different analytical lines can be used. A list of the wavelengths of appropriate analytical lines is given in Annex A. Which of the different analytical lines are used depends on the analytical programme and the type of spectrometer. 8.2 Calibr
46、ation The apparatus used shall be capable and suitable for the detection and determination of all elements specified in the relevant product standards (ISO 301 and ISO 752). Calibrate the apparatus within a reasonable time, in accordance with the procedures described in the instruction manual. Prepa
47、re the calibration solutions taking into account the product specification on chemical composition, in accordance with Table 1 below. Table 1 Composition of spectrometer calibration solution Calibration standard No. 1 2 3 4 5 6 7 Alloying element 1 0,8 m m (3m+M)/4 (m+M)/2 (m+3M)/4 M 1,2 M Alloying
48、element 2 1,2 M M (m+3M)/4 (m+M)/2 (3m+M)/4 m 0,8 m Alloying element 3 (3m+M)/4 m 0,8 m ( m+M)/2 1,2 M M (m+3M)/4 Alloying element 4 (m+3M)/4 M 1,2 M ( m+M)/2 0,8 m m (3m+M)/4 Impurity element 1 blank 0,2 L 0,5 L 0,8 L L 1,2 L 1,5 L Impurity element 2 0,2 L 0,5 L 0,8 L L 1,2 L 1,5 L blank Impurity element 3 0,5 L 0,8 L L 1,2 L 1,5 L blank 0,2 L Impurity element 4 0,8 L L 1,2 L 1,5 L blank 0,2 L 0,5 L Impurity element 5 L 1,2 L 1,5 L blank 0,2 L 0,5 L 0,8 L Impurity element 6 1,2 L 1,5 L blank 0,2
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