1、February 2016 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 77.040.30!%LA“2410430www.din.de
2、DIN EN 10361Alloyed steels Determination of nickel content Inductively coupled plasma optical emission spectrometric method;English version EN 10361:2015,English translation of DIN EN 10361:2016-02Legierte Sthle Bestimmung des Nickelanteils Verfahren mittels optischer Emissionsspektrometrie mit indu
3、ktiv gekoppeltem Plasma;Englische Fassung EN 10361:2015,Englische bersetzung von DIN EN 10361:2016-02Aciers allis Dtermination du nickel Mthode par spectromtrie dmission optique avec source plasma induit;Version anglaise EN 10361:2015,Traduction anglaise de DIN EN 10361:2016-02www.beuth.deDocument c
4、omprises 1 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.901.16 2 A comma is used as the decimal marker. National foreword This document (EN 10361:2015) has been prepared by Technical Committee ECISS/TC 102 “Methods of chemic
5、al analysis of iron and steel“ (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was DIN-Normenausschuss Eisen und Stahl (DIN Standards Committee Iron and Steel), Working Committee NA 021-00-30 AA Analyseverfahren. There is no national standard on the subject. DIN E
6、N 10361:2016-02 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10361 December 2015 ICS 77.040.30 English Version Alloyed steels - Determination of nickel content - Inductively coupled plasma optical emission spectrometric method Aciers allis - Dtermination du nickel - Mthode par spectromtrie d
7、mission optique avec source plasma induit Legierte Sthle - Bestimmung des Nickelanteils - Verfahren mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma This European Standard was approved by CEN on 20 June 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regul
8、ations which stipulate 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 CEN-CENELEC Management Centre or to any CEN membe
9、r. This European Standard exists 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 CEN-CENELEC Management Centre has the same status as the official versions. CE
10、N members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
11、Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in a
12、ny form and by any means reserved worldwide for CEN national Members. Ref. No. EN 10361:2015 EEN 10361:2015 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Normative references 4 3 Principle . 4 4 Reagents . 4 5 Apparatus . 5 6 Sampling . 6 7 Procedure. 6 8 Determination 8 9 Expression of the
13、results 9 10 Test report . 9 Annex A (informative) Plasma optical emission spectrometer - Suggested performance criteria to be checked . 13 Annex B (informative) Composition of the samples used for the validation precision test. 15 Annex C (informative) Graphical representation of the precision data
14、 16 Bibliography . 17 DIN EN 10361:2016-02 EN 10361:2015 (E) 3 European foreword This document (EN 10361:2015) has been prepared by Technical Committee ECISS/TC 102 “Methods of chemical analysis of iron and steel”, the secretariat of which is held by SIS. This European Standard shall be given the st
15、atus of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2016 and conflicting national standards shall be withdrawn at the latest by June 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject
16、of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgar
17、ia, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turk
18、ey and the United Kingdom. DIN EN 10361:2016-02 EN 10361:2015 (E) 4 1 Scope This European Standard specifies an inductively coupled plasma optical emission spectrometric method for the determination of nickel content (mass fraction) between 5,0 % and 25,0 % in alloyed steels. The method does not app
19、ly to alloyed steels having niobium and/or tungsten contents higher than 0,1 %. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undate
20、d references, the latest edition of the referenced document (including any amendments) applies. EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648) EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042) 3 Principle Dissolution of a test portion with hydrochloric an
21、d nitric acids. Filtration and ignition of the acid insoluble residue. Removal of silica with hydrofluoric acid. Fusion of the residue with potassium hydrogen sulphate (or with potassium disulphate), dissolution of the melt with acid and addition of this solution to the reserved filtrate. After suit
22、able dilution and, if necessary, addition of an internal reference element, nebulization of the solution into an inductively coupled plasma emission spectrometer and measurement of the intensity of the emitted light (including, where appropriate, that of the internal reference element). The method u
23、ses a calibration based on a very close matrix matching of the calibration solutions to the sample and bracketing of the mass fractions between 0,95 to 1,05 of the approximate content of nickel in the sample to be analysed. The content of all elements in the sample has, therefore, to be approximatel
24、y known. If the contents are not known the sample shall be analysed by some semi quantitative method. The advantage with this procedure is that all possible interferences from the matrix will be compensated, which will result in high accuracy. This is most important for spectral interferences, which
25、 can be severe in very highly alloyed matrixes. All possible interferences shall be kept at a minimum level. Therefore, it is essential that the spectrometer used meets the performance criteria specified in the method for the selected analytical lines. The optical lines reported in the Table 1 have
26、been investigated and the strongest possible interferences are given. If other optical lines are used, they shall be carefully checked. The analytical line for the internal reference element should be selected carefully. The use of scandium at 363,1 nm or yttrium at 371,0 nm is recommended. These li
27、nes are interference-free for the elements and contents generally found in alloyed steels. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. The same reagents should be used for the preparation of calibration solu
28、tions and of sample solutions. 4.1 Hydrochloric acid, HCl (20= 1,19 g/ml). 4.2 Nitric acid, HNO3(20= 1,33 g/ml). DIN EN 10361:2016-02 EN 10361:2015 (E) 5 4.3 Hydrofluoric acid, HF (20= 1,13 g/ml). WARNING Hydrofluoric acid is extremely irritating and corrosive to skin and mucous membranes producing
29、severe skin burns which are slow to heal. In the case of contact with skin, wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate, and seek immediate medical treatment. 4.4 Sulphuric acid, H2SO4(20= 1,84 g/ml). 4.5 Sulphuric acid, solution 1 + 1. While cooling,
30、 add 25 ml of sulphuric acid (4.4) to 25 ml of water. 4.6 Potassium hydrogen sulphate KHSO4 or potassium disulphate K2S2O7. 4.7 Nickel standard solution, 10 g/l. Weigh, to the nearest 0,001 g, 5 g of high purity nickel min 99,9 % (mass fraction), place it in a beaker and dissolve in 50 ml of water a
31、nd 100 ml of nitric acid (4.2). Cover with a watch glass and heat gently until the nickel is completely dissolved. Cool and transfer quantitatively into a 500 ml one-mark volumetric flask. Dilute to mark with water and mix. 1 ml of this solution contains 10 mg of nickel. 4.8 Nickel standard solution
32、, 5 g/l. Weigh, to the nearest 0,001 g, 2,5 g of high purity nickel min 99,9 % (mass fraction), place it in a beaker and dissolve in 25 ml of water and 50 ml of nitric acid (4.2). Cover with a watch glass and heat gently until the nickel is completely dissolved. Cool and transfer quantitatively into
33、 a 500 ml one-mark volumetric flask. Dilute to mark with water and mix. 1 ml of this solution contains 5 mg of nickel. 4.9 Standard solutions of matrix elements. Prepare standard solutions for each element whose mass fraction is higher than 1 % in the test sample. Use pure metals or chemical substan
34、ces with nickel mass fractions less than 100 g/g. 4.10 Internal reference element solution, 1 g/l. Choose a suitable element to be added as internal reference and prepare a 1 g/l solution. NOTE Elements such as In, Sc and Y were used during the precision test of this method. 5 Apparatus All volumetr
35、ic glassware shall be class A and calibrated in accordance with EN ISO 648 or EN ISO 1042, as appropriate. 5.1 Medium texture filter paper. 5.2 Platinum crucibles. 5.3 Optical emission spectrometer, equipped with inductively coupled plasma. This shall be equipped with a nebulization system. The inst
36、rument used will be satisfactory if, after optimizing in accordance with the manufacturers instructions, it meets the performance criteria given in Annex A. DIN EN 10361:2016-02 EN 10361:2015 (E) 6 The spectrometer can be either a simultaneous or a sequential one. If a sequential spectrometer can be
37、 equipped with an extra arrangement for simultaneous measurement of the internal reference element line, it can be used with the internal reference method. If the sequential spectrometer is not equipped with this arrangement, an internal reference cannot be used and an alternative measurement techni
38、que without internal reference element shall be used. 6 Sampling Sampling shall be carried out in accordance with EN ISO 14284 or with an appropriate national standard for steels. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,001 g, 1 g of the test sample. 7.2 Preparation of the test solution
39、, TNiTransfer the test portion (7.1) into a 250 ml beaker. Add 15 ml of hydrochloric acid (4.1), cover with a watch glass, heat gently until the attack reaction ceases, and then add dropwise, 10 ml of nitric acid (4.2). Depending on the composition of each sample, larger amounts of hydrochloric acid
40、 may be necessary. Addition of hydrogen peroxide (H2O2) may advantageously help dissolution. The same quantities of the dissolution reagents shall be added to the corresponding calibration solutions. Boil until nitrous fumes have been expelled. After cooling, add about 20 ml of water, filter the sol
41、ution through a medium texture filter paper (5.1) and collect the filtrate into a 200 ml one-mark volumetric flask. Wash the filter paper and its content with warm water slightly acidified with nitric acid (4.2) several times and collect the washings in the 200 ml one-mark volumetric flask. Transfer
42、 the filter into a platinum crucible (5.2), dry and ignite first at a relatively low temperature (until all carbonaceous matter is removed) and then at about 800 C for at least 15 min. Allow the crucible to cool. Add into the crucible 0,5 ml to 1,0 ml of sulphuric acid solution (4.5) and 2 ml of hyd
43、rofluoric acid (4.3). Evaporate to dryness and cool. Add into the crucible 1,00 g of potassium hydrogen sulphate or potassium disulphate (4.6) and fuse carefully by means of a Meker burner, until a clear melt is obtained. NOTE 1 For residues containing substantial amounts of chromium carbides, prolo
44、nged heating may be necessary for complete fusion. The potassium hydrogen sulphate can be regenerated by allowing the melt to cool, adding some drops of sulphuric acid (4.4) and repeating the fusion until the residue is fused. NOTE 2 Depending on the composition of each sample, larger amounts of pot
45、assium hydrogen sulphate or potassium disulphate (4.6) can be used, provided the same amount is added to the corresponding calibration solutions. Allow the crucible to cool and add about 10 ml of water and 2 ml of hydrochloric acid (4.1) to the solidified melt. Heat gently, in order to dissolve the
46、fusion products. Allow the crucible to cool and transfer the solution quantitatively to the filtrate in the 200 ml one-mark volumetric flask. NOTE 3 The volume of hydrochloric acid (4.1) can be increased, provided the same volume is added to the appropriate calibration solutions. DIN EN 10361:2016-0
47、2 EN 10361:2015 (E) 7 Dilute to the mark with water and mix. Transfer 20 ml of this sample solution into a 100 ml one-mark volumetric flask and add 10 ml of hydrochloric acid (4.1). NOTE 4 Depending on the instrument performances, the final concentration of the test solution may be lower (or higher)
48、, provided the corresponding calibration solutions have the same final concentration. If an internal reference element is used add, with a calibrated pipette, 10 ml of the internal reference element solution (4.10). NOTE 5 Depending on the instrument performances, the volume and/or the concentration
49、 of the internal reference element solution may be different. Dilute to the mark with water and mix. 7.3 Predetermination of the test solution Prepare two calibration solutions labelled K25and K0, matrix matched to the test sample solution as follows: Add 25 ml of the nickel standard solution (4.7) in a 400 ml beaker, labelled K25. In each 400 ml beaker, K25and K0, add the volumes of the standard solutions (4.9) necessary to match the sample matrix to be tested
