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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1810:1998 The Europ
2、ean Standard EN 1810:1998 has the status of a British Standard ICS 39.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Body-piercing post assemblies Reference test method for determination of nickel content by flame atomic absorption spectrometry Licensed Copy: sheffieldun
3、sheffieldun, na, Mon Oct 30 05:10:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 November 1998 BSI 1998
4、 ISBN 0 580 29982 1 BS EN 1810:1998 Amendments issued since publication Amd. No.DateText affected National foreword This British Standard is the English language version of EN 1810:1998. The UK participation in its preparation was entrusted to Technical Committee STI/53, Jewellery, which has the res
5、ponsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organ
6、izations represented on this committee can be obtained on 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 Standard
7、s Correspondence Index, or by using the Find facility of the BSI Standards Electronic Catalogue. 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 doe
8、s not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 7 and a back cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 05:10:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN Euro
9、pean Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1810:1998 E EUROP
10、EAN STANDARDEN 1810 NORME EUROPE ENNE EUROPA ISCHE NORM May 1998 ICS 39.060 Descriptors: precious metals, alloys, aluminium alloys, silver alloys, gold alloys, titanium alloys, copper alloys, steels, tests, determination, determination of content, nickel, atomic absorption spectrometrophotometry Eng
11、lish version Body-piercing post assemblies Reference test method for determination of nickel content by flame atomic absorption spectrometry Ensembles de perage de parties du corps Me thode dessai de re fe rence pour la de termination de la teneur en nickel par spectrome trie dabsorption atomique de
12、 flamme Stecker, die durch Teile des Ko rpers gestochen werden Referenzpru fverfahren zur Bestimmung des Nickelgehalts durch Atomabsorptionsspektrometrie This European Standard was approved by CEN on 10 April 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipu
13、late the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard ex
14、ists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards b
15、odies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 05:10:30 GMT+00:00 2006, Uncontrolled Copy,
16、(c) BSI Page 2 EN 1810:1998 BSI 1998 Foreword This European Standard has been prepared by Technical Committee CEN/TC 283, Precious metals Applications in jewellery and associated products, the Secretariat of which is held by UNI. This European Standard shall be given the status of a national standar
17、d, either by publication of an identical text or by endorsement, at the latest by November 1998, and conflicting national standards shall be withdrawn at the latest by November 1998. Annex A is informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of th
18、e following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffiel
19、dun, na, Mon Oct 30 05:10:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 1810:1998 BSI 1998 Introduction This method is used to determine whether the nickel content in post assemblies which are inserted into pierced ears and other pierced parts of the human body during epithelization of the
20、 wound caused by piercing, whether subsequently removed or not, is equal to or less than 0,05 % (m/m). 1 Scope This European Standard specifies a method for the determination of nickel in aluminium, titanium, copper, silver, gold and their alloys and in steels by flame atomic absorption spectrophoto
21、metry. The method is primarily suitable when the nickel content of a sample lies between 0,03 % and 0,07 % (m/m). 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate plac
22、es 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 standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to
23、applies. prEN 1811, Precious metals Reference test method for release of nickel from products intended to come into direct and prolonged contact with the skin. 3 Principle A test portion is dissolved in an acid medium. The resulting solution is atomized into an air-acetylene flame of the atomic abso
24、rption spectrophotometer, and the absorption of the resonance energy of nickel (232,0 nm) is compared with that of calibration solutions. 4 Reagents All reagents shall be of recognized pro-analysis, p.a., grade or better, and shall be free of nickel. NOTEOnly those reagents appropriate to the matric
25、es under examination are required. WARNING. Concentrated acids are hazardous. Wear safety glasses or goggles and carry out dissolution of metals in a well-ventilated fume cupboard. 4.1 Deionized water, specific conductivity maximum 1 mS/cm. 4.2 Hydrochloric acid, 38 % (m/m), r = 1,19 g/ml. 4.3 Dilut
26、e hydrochloric acid, 20 % (m/m), r = 1,10 g/ml. Carefully add 125 ml of hydrochloric acid (see 4.2) to approximately 110 ml of deionized water in a 500 ml beaker. Stir and cool to room temperature. Transfer the solution into a 250 ml volumetric flask and make up to volume with deionized water. 4.4 H
27、ydrogen peroxide solution, 30 % (m/m). 4.5 Hydrofluoric acid, 40 % (m/m), r = 1,13 g/ml. 4.6 Nitric acid, 65 % (m/m), r = 1,40 g/ml. 4.7 Dilute nitric acid, 33 % (m/m), r = 1,20 g/ml. Carefully add 44 ml of nitric acid (see 4.6) to approximately 40 ml of deionized water in a 250 ml beaker. Stir and
28、cool to room temperature. Transfer the solution into a 100 ml volumetric flask and make up to volume with deionized water. 4.8 Perchloric acid, 60 % (m/m), r 5 1,54 g/ml. 4.9 Aqua regia Cautiously mix 120 ml of hydrochloric acid (see 4.2) and 40 ml of nitric acid (see 4.6). This mixture shall be pre
29、pared immediately before use. 4.10 Solution of hydrochloric acid and nitric acid Cautiously add 50 ml of hydrochloric acid (see 4.2) to 40 ml of deionized water, with stirring. Add 20 ml of nitric acid (see 4.6) and mix well. Prepare this solution immediately before use. 4.11 Solution of nitric acid
30、 and perchloric acid Cautiously mix 5 ml of nitric acid (see 4.6) and 40 ml of perchloric acid (see 4.8). Transfer the solution into a 50 ml volumetric flask and make up to volume with deionized water. 4.12 Nickel stock solution, (1,000 00,000 2) g/l. Prepare nickel stock solution, for example, by u
31、sing a certified standard solution ampoule. 4.13 Aluminium matrix, 10 g/l stock solution. Weigh, to the nearest 0,001 g, 2,000 g of aluminium (containing less than 0,000 5 % nickel) and transfer to a 125 ml conical flask. Add, in small portions, 60 ml of dilute hydrochloric acid (see 4.3) and warm g
32、ently until complete dissolution. Add a few drops of hydrogen peroxide (see 4.4) and heat for about 2 min to remove excess hydrogen peroxide. Cool to room temperature, transfer the solution into a 200 ml volumetric flask and make up to volume with deionized water. 4.14 Titanium matrix, 10 g/l stock
33、solution. Weigh, to the nearest 0,001 g, 2,000 g of titanium (containing less than 0,000 5 % nickel) and transfer to a 125 ml conical flask. Add, in small portions, 60 ml of hydrofluoric acid (see 4.5) and warm gently until complete dissolution. Cool to room temperature, transfer the solution into a
34、 200 ml volumetric flask and make up to volume with deionized water. Use laboratory apparatus appropriate for hydrofluoric acid, e.g. polytetrafluoroethylene (PTFE). Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 05:10:30 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 1810:1998 BSI 199
35、8 4.15 Copper matrix, 10 g/l stock solution. Weigh to the nearest 0,001 g, 2,000 g of copper (containing less than 0,000 5 % nickel) and transfer to a 125 ml conical flask. Add, in small portions, 40 ml of dilute hydrochloric acid (see 4.3) and 10 ml of hydrogen peroxide (see 4.4). Cool until the vi
36、olent reaction has ceased. When completely dissolved, heat the solution to boiling and continue boiling for approximately 1 min to remove excess hydrogen peroxide, then cool to room temperature. Transfer the solution into a 200 ml volumetric flask and make up to volume with deionized water. 4.16 Sil
37、ver matrix, 10 g/l stock solution. Weigh, to the nearest 0,001 g, 2,000 g of silver (containing less than 0,000 5 % nickel) and transfer to a 125 ml conical flask. Add 60 ml of dilute nitric acid (see 4.7) and warm gently until complete dissolution. Heat, without boiling, until evolution of nitrogen
38、 oxide fumes ceases. Cool to room temperature, transfer the solution into a 200 ml volumetric flask and make up to volume with deionized water. 4.17 Gold matrix, 10 g/l stock solution. Weigh, to the nearest 0,001 g, 2,000 g of gold (containing less than 0,000 5 % nickel) and transfer to a 125 ml con
39、ical flask. Add 80 ml aqua regia (see 4.9) and warm. Add aqua regia, as required, until complete dissolution. Note the amount of aqua regia used. Cool to room temperature, transfer the solution into a 200 ml volumetric flask and make up to volume with deionized water. 4.18 Iron matrix, 10 g/l stock
40、solution. Weigh, to the nearest 0,001 g, 2,000 g of iron (containing less than 0,000 5 % nickel) and transfer to a 125 ml conical flask. Add 50 ml of the hydrochloric acid-nitric acid solution (see 4.10) and warm until complete dissolution. Cool to room temperature and filter if necessary. Transfer
41、the solution into a 200 ml volumetric flask and make up to volume with deionized water. 5 Apparatus Normal laboratory equipment, and: 5.1 Balance, capable of weighing in grams to four decimal places. 5.2 An atomic absorption spectrophotometer, a nickel hollow-cathode lamp and supplies of air and ace
42、tylene (free from water, oil and nickel) sufficiently pure to give a steady clear flame. The apparatus shall, after optimization according to 6.5, meet the performance criteria given in 5.2.1 to 5.2.3. Additionally, it is recommended that the apparatus conforms to the performance criteria given in 5
43、.2.4. 5.2.1 Minimum precision The standard deviation of 10 measurements of the absorbance of the most concentrated calibration solution (see 6.4) shall not exceed 1,0 % of the mean absorbance of the most concentrated calibration solution. The standard deviation of 10 measurements of the absorbance o
44、f the least concentrated calibration solution (excluding the zero calibration solution) (see 6.4) shall not exceed 0,5 % of the mean absorbance of the most concentrated calibration solution. 5.2.2 Characteristic concentration The characteristic concentration for nickel in a matrix similar to the fin
45、al test solution shall be no greater than 0,10 mg/l of nickel at 232,0 nm. 5.2.3 Limit of detection The limit of detection shall be considered as twice the standard deviation of 10 measurements of the absorbance of a solution containing nickel at a concentration level selected to give an absorbance
46、just above that of the zero calibration solution. The limit of detection of nickel in a matrix similar to the final test solution shall be better than 0,15 mg/l at 232,0 nm. 5.2.4 Graph linearity The slope of the calibration graph covering the top 20 % of the concentration range (expressed as a chan
47、ge in absorbance) should be not less than 0,7 times the value of the slope for the bottom 20 % of the concentration range. In this standard, the calibration graph is drawn at the lower part of the optimum working range, normally defined as 20 to 125 times the characteristic concentration. NOTEThe pe
48、rformance criteria given in 5.2.1 to 5.2.4 are based on provisions given in ISO/CD 13204. 6 Procedure 6.1 Detection of surface layers Samples shall be subjected to the nickel release test according to prEN 1811 to detect nickel contamination on the surface, and abraded with an abrasive material to c
49、heck visually for the presence of coatings. When checking for the presence of nickel on the surface, samples shall not be degreased prior to analysis. NOTEIf coatings are suspected, X-ray analysis may assist recognition. 6.2 Composition of sample Identify the approximate composition of the sample by any appropriate means, for example, by X-ray fluorescence spectrometry (XRF) or other semi-quantitative method. This is necessary in order to classify the sample as an aluminium, titanium, copper, silver, gold or steel alloy. Licensed Copy: sheffield
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