DIN EN ISO 11876-2010 Hardmetals - Determination of calcium copper iron potassium magnesium manganese sodium nickel and zinc in cobalt metal powders - Flame atomic absorption spect.pdf

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1、December 2010 Translation by DIN-Sprachendienst.English price group 7No 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).IC

2、S 77.160!$ld#“1736500www.din.deDDIN EN ISO 11876Hardmetals Determination of calcium, copper, iron, potassium, magnesium,manganese, sodium, nickel and zinc in cobalt metal powders Flame atomic absorption spectrometric method (ISO 11876:2010)English translation of DIN EN ISO 11876:2010-12Hartmetalle B

3、estimmung des Calcium-, Kupfer-, Eisen-, Kalium-, Magnesium-, Mangan-, Natrium-,Nickel- und Zinkgehaltes in Kobalt-Metallpulvern Verfahren mit Flammen-Atomabsorptionsspektrometrie (ISO 11876:2010)Englische bersetzung von DIN EN ISO 11876:2010-12Mtaux-durs Dosage du calcium, du cuivre, du fer, du pot

4、assium, du magnsium, du manganse, dusodium, du nickel et du zinc dans les poudres mtalliques de cobalt Mthode par spectromtrie dabsorption atomique dans la flamme (ISO 11876:2010)Traduction anglaise de DIN EN ISO 11876:2010-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language

5、original shall be considered authoritative.9 12.10 DIN EN ISO 11876:2010-12 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy” (Secretariat: SIS, Sweden) in collaboration with Technical Committee CEN/SS M11

6、 “Powder metallurgy” (Secretariat: CCMC). The responsible German body involved in its preparation was the Normenausschuss Werkstofftechnologie (Technology of Materials Standards Committee), Working Committee NA 145-01-04 AA Probenahme und Prfverfahren fr Hartmetalle. The DIN Standard corresponding t

7、o the International Standard referred to in this document is as follows: ISO 3534-1:2006 DIN ISO 3534-1:2009-10 National Annex NA (informative) Bibliography DIN ISO 3534-1:2009-10, Statistics Vocabulary and symbols Part 1: General statistical terms and terms used in probability DIN ISO 5725-1, Accur

8、acy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement me

9、thod DIN ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method DIN ISO 5725-4, Accuracy (trueness and precision) of measurement methods and results Part 4: Basic methods for the determination o

10、f the trueness of a standard measurement method DIN ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method DIN ISO 5725-6, Accuracy (trueness and precision) of measurement me

11、thods and results Part 6: Use in practice of accuracy values EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11876 August 2010 ICS 77.160 English Version Hardmetals - Determination of calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel and zinc in cobalt metal powders - F

12、lame atomic absorption spectrometric method (ISO 11876:2010) Mtaux-durs - Dosage du calcium, du cuivre, du fer, du potassium, du magnsium, du manganse, du sodium, du nickel et du zinc dans les poudres mtalliques de cobalt - Mthode par spectromtrie dabsorption atomique dans la flamme (ISO 11876:2010)

13、 Hartmetalle - Bestimmung des Calcium-, Kupfer-, Eisen-, Kalium-, Magnesium-, Mangan-, Natrium-, Nickel- und Zinkgehaltes in Kobalt-Metallpulvern - Verfahren mit Flammen-Atomabsorptionsspektrometrie (ISO 11876:2010)This European Standard was approved by CEN on 14 August 2010. CEN members are bound t

14、o comply with the CEN/CENELEC Internal Regulations 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 M

15、anagement Centre or to any CEN member. 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 Management Centre has the same status

16、as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, R

17、omania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserv

18、ed worldwide for CEN national Members. Ref. No. EN ISO 11876:2010: EContents DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 2 Page Foreword3 1 Scope 4 2 Normative references 4 3 Reagents.4 4 Procedure .4 4.1 Test portion 4 4.2 Dissolution of the test portion4 4.3 Dilution volume5 4.4 Preparation of

19、calibration and blank solutions 5 4.5 Adjustment of the atomic absorption spectrometer5 4.6 Atomic absorbance measurement.5 5 Expression of results 6 5.1 Calculation6 5.2 Permissible tolerances6 5.3 Final result6 6 Test report 6 Bibliography 7 Foreword This document (EN ISO 11876:2010) has been prep

20、ared by Technical Committee ISO/TC 119 Powder metallurgy 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 February 2011, and conflicting national standards shall be withdrawn at the latest by Febru

21、ary 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject 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 or

22、ganizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,

23、Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 11876:2010 has been approved by CEN as a EN ISO 11876:2010 without any modification. ”.“DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 3 1 Scope This International Standard sp

24、ecifies a flame atomic absorption spectrometric method to be used for the determination of the mass fractions of copper, potassium, magnesium, manganese, sodium and zinc in cobalt metal powders in the range of 0,001 % to 0,01 %, calcium in the range of 0,002 % to 0,01 %, and iron and nickel in the r

25、ange of 0,002 % to 0,05 %. 2 Normative references The following referenced 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.

26、 ISO 3534-1:2006, Statistics Vocabulary and symbols Part 1: General statistical terms and terms used in probability 3 Reagents Use only reagents of the highest purity and only double-distilled water or water of equivalent purity. 3.1 Nitric acid, = 1,42 g/ml, diluted 1 + 1. 3.2 Hydrochloric acid, 1,

27、1 g/ml (hydrochloric acid, = 1,19 g/ml, diluted 1 + 1). 3.3 Cesium chloride solution, (20 g/1 000 ml). 3.4 Standard solutions, (1,000 g/1 000 ml) for calibration purposes for each element to be determined. 4 Procedure 4.1 Test portion Weigh, to the nearest 0,001 g, approximately 1 g of the sample. 4

28、.2 Dissolution of the test portion Add 20 ml of nitric acid (3.1) and 10 ml of hydrochloric acid (3.2) and heat gently until the test portion is completely dissolved. DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 4 4.3 Dilution volume 4.3.1 Add 5 ml of the cesium chloride solution (3.3) and dilute

29、to 100 ml. 4.3.2 Shake the analysed volume with 20 ml of freshwater and filter using appropriate filter media over a plug of cotton wool into a 50 ml or 100 ml volumetric flask. Depending on the concentration of the determined elements in the sample and/or the sensitivity of the photometer, the dilu

30、tion volume may be either 50 ml or 100 ml in volumetric flask. 4.4 Preparation of calibration and blank solutions 4.4.1 Prepare at least three solutions according to 4.2 with a matrix as similar as possible to the test portion to be analysed but without making up to volume. Then add increasing volum

31、es of property diluted standard solutions of the elements to be determined according to the concentration ranges to be covered. Make up to 100 ml and mix. 4.4.2 Prepare at least two blank solutions (see 4.4.1) without the addition of the relevant element to be determined. 4.5 Adjustment of the atomi

32、c absorption spectrometer SAFETY PRECAUTIONS Follow the manufacturers recommendation on igniting and extinguishing the flame. Optimize the response of the instrument at the wavelength given for the element to be determined (see Table 1). Preheat the burner for about 5 min and adjust the fuel and cor

33、rect the burner to obtain maximum absorption while aspirating a calibration solution. Make sure that the absorbance reading is not drifting. Aspirate water and set the initial reading to zero absorbance. Table 1 Parameters for atomic flame absorption Element Wavelength nm Oxidant/fuel Ca 422,7 N2O/a

34、cetylene Cu 324,8 air/acetylene Fe 248,3 air/acetylene K 766,5 air/acetylene Mg 285,2 N2O/acetylene Mn 279,5 air/acetylene Na 589,0 air/acetylene Ni 232,0 air/acetylene Zn 213,9 air/acetylene NOTE Use slit recommended by the manufacturer. 4.6 Atomic absorbance measurement 4.6.1 Aspirate first the bl

35、ank solution and then the calibration and test solutions consecutively and record the reading. Aspirate water between each solution. Make at least two measurements for each solution. Solids which build up at the burner slit shall be removed; otherwise they cause a decrease in sensitivity. 4.6.2 Prep

36、are a calibration curve by plotting the obtained absorbance values of the calibration solutions corrected for the blank against the concentration. 4.6.3 Convert the absorbance values of the test solution corrected for the blank to milligrams of the element per litre by means of the calibration curve

37、. DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 5 5 Expression of results 5.1 Calculation The mass fraction of the element, expressed as a percentage, is given by the following formula: 10 000cVmwhere c is the concentration, in milligrams per litre (mg/l), of the element in the test solution; V is

38、the dilution volume, in millilitres (ml); m is the mass of the test portion, in grams (g). 5.2 Permissible tolerances The deviations between three independent determinations shall not exceed the values in Table 2. Table 2 Lower and upper limits of mass fraction of the element as a percentage Element

39、 Lower limit Upper limit Calcium 0,000 5 % 50 % (CV) 0,010 0 % 20 % (CV) Copper 0,000 5 % 50 % (CV) 0,010 0 % 20 % (CV) Iron 0,000 5 % 50 % (CV) 0,015 0 % 20 % (CV) Potassium 0,000 5 % 50 % (CV) 0,010 0 % 20 % (CV) Magnesium 0,000 5 % 50 % (CV) 0,010 0 % 20 % (CV) Sodium 0,000 5 % 50 % (CV) 0,005 0

40、% 20 % (CV) Nickel 0,000 5 % 50 % (CV) 0,020 0 % 20 % (CV) Zinc 0,000 5 % 100 % (CV) 0,010 0 % 10 % (CV) CV: coefficient of variation (see ISO 3534-1:2006, 2.38) 5.3 Final result Report the arithmetic mean of acceptable determinations, rounded to a mass fraction of 0,001 % and a mass fraction of 0,0

41、02 %. 6 Test report The test report shall include the following information: a) a reference to this International Standard; b) all details necessary for identification of the test sample; c) the results obtained; d) all operations not specified in this International Standard, or regarded as optional

42、; e) details of any occurrence which may have affected the result. DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 6 Bibliography 1 ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions 2 ISO 5725-2, Accuracy (trueness and precisio

43、n) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 3 ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measu

44、rement method 4 SO 5725-4, Accuracy (trueness and precision) of measurement methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method 5 ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method 6 ISO 5725-6, Accuracy (trueness and precision) of measurement methods and results Part 6: Use in practice of accuracy values DIN EN ISO 11876:2010-12 EN ISO 11876:2010 (E) 7