EN 27627-3-1993 en Hardmetals - Chemical Analysis by Flame Atomic Absorption Spectrometry - Part 3 Determination of Cobalt Iron Manganese and Nickel in Contents from 0 01 to 0 5 % .pdf

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1、CEN ENx27b27-3 93 D 3404589 0047182 O29 EUROPEAN STANDARD EN 27627-3 NORME EUROPENNE EUROPISCHE NORM April 1993 UDC 669.018.25 : 620.1 : 543.422 Descriptors: Powder metallurgy, hard metals, chemical anaipis, determination of content, transition metais, cobalt, iron, manganese, nickel, spectrometric

2、analysis, atomis absorption spectrophotometry English version Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Part 3: Determination of cobalt, iron, manganese and nickel in contents from 0,Ol to 0,5 % (m/m) (IS0 7627-3 : 1983) Mtaux-durs - Analyse chimique par spectromtrie d

3、absorption atomique dans la flamme - Partie 3: Dosage du cobalt, du fer, du manganse et du nickel des teneurs comprises entre 0,Ol et 0,5 % (m/m) Hartmetalle - Chemische Analyse durch Flammenatomabsorptionsspektrometrie - Teil 3: Bestimmung des Cobalt-, Eisen-, Mangan- und Nickelgehaltes von 0,Ol bi

4、s 0,5 % (m/m) (IS0 7627-3 1983) (IS0 7627-3 : 1983) This European Standard was approved by CEN on 1993-04-02. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alter

5、ation. 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 exists in three official versions (English, French, German). A version in any other language made by transl

6、ation 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 bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg

7、, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: re de Stassart 36, B-1050 Brussels O 1993 Copyright reserved to CEN members Ref. No. EN 27627-

8、3 : 1993 E CEN EN*27b27-3 93 m 3404589 0047383 Tb5 m Page 2 EN 27627-3 : 1993 Foreword In 1992, IS0 7627-3 : 1983 Hardmetals - Chemical analysis byjme atomic absorption spectrometry - part 3 : Determination of cobalt, iron, manganese and nickel in contents frm 0,Ol to 0,s % (dm) was submitted to the

9、 CEN Primary Questionnaire procedure. Following the positive result of the CENES Proposal IS0 7627-3 : 1983 was submitted to the CEN Formal Vote. The result of the Formal Vote was positive. This European Standard shall be given the status of a national standard, either by publication of an identical

10、 text or by endorsement, at the latest by October 1993, and conflicting national standards shal be withdrawn at the latest by October 1993. According to the Internal Regulations of CENKENELEC, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland,

11、Flance, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, United Kingdom. NOTE. The European references to international publications are given in annex ZA (normative). CEN ENr27627-3 93 W 3404589 0047184 9T1 Page 3 EN 27627-3 : 1993 1 T

12、his part of IS0 7627 specifies the method to be used for the determination of cobalt, iron, manganese and nickel contents of hardmetals within the range 0,Ol to 0,5 % (rn/rn) by flame atomic absorption spectrometry. Scope and field of application General requirements concerning the field of applicat

13、ion, prin- ciple, interfering elements, apparatus, sampling and test report are given in IS0 7M7/ 1. 2 Reference IS0 762711, Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Pari 7: General requirements. 3 Reagents 3.1 Hydrofluoric acid, e 1,12 g/ml. 3.2 Nitric acid, e 1,42 g

14、lml. 3.3 Ammonium fluoride, 0.1 glml solution, 3.4 Caesium chloride, 0,Ol g/ml solution. 3.5 High-purity stock solutions, for calibration purposes for each element to be determined, containing 1,ooO g of the element per litre. NOTE - This value is understood to establish a maximum limit of 1,OOO 5 g

15、 and a minimum limit of 0,999 5 g. 4 Procedure 4.1 Test portion Weigh, to the nearest 0.001 g, approximately 1 g of the test sample. Transfer it to a 100 ml polytetrafluorethylene beaker or a beaker of other suitable material. Cover the beaker. 4.2 Dissolution of the test portion Add 10 ml of water,

16、 5 ml of the hydrofluoric acid (3.11. and then 5 ml of the nitric acid (3.21, drop by drop, to the beaker containing the test portion (4.1) and heat gently until the test portion is completely dissolved. Add 10 ml of the caesium chloride solution (3.4) and 10 ml of the ammonium fluoride solution (3.

17、3). Then transfer the solution totally to a 100 ml polypropylene one-mark volumetric flask and dilute to the mark. 4.3 Dilution volume Prepare the relevant dilution volume for the analysis according to table 1 as follows: 4.3.1 Dilution volume 100 ml: use the solution in 4.2. 4.3.2 The concentration

18、 of the solution may be reduced by a factor of 10 for instruments of higher sensitivity by transferring 10 ml of the solution in 4.2 to a 100 ml polypropylene one-mark volumetric flask. Add 10 ml of the caesium chloride solution (3.4). Add 10 ml of the ammonium fluoride solution (3.3) and dilute to

19、the mark. 4.4 Preparation of calibration and blank solutions 4.4.1 Prepare at least six solutions according to 4.2 with a matrix composition as similar as possible to the test portion to be analysed, but without making up to volume. Then add in- creasing volumes of properly diluted stock solutions o

20、f the elements to be determined according to the concentration ranges to be covered. Make up to 100 ml and mix. 4.4.2 Also prepare calibration solutions with a diluted matrix in accordance with 4.3 for dilution volumes of 1 o00 ml, if necessary. CEN ENlc27627-3 93 340q589 0047385 838 Page 4 EN 27627

21、-3 : 1993 Dilution volume i Vi Reciprocal sensitivity, Element for 1 g test portion” Oxidant Wavelength for 1 % absorption1 Linear range1) ml nm Wml % Co 100 NZO 240.7 0.7 0,007 to 0,5 0.003 to 0,05 248.3 0.3 248.3 0.3 0,03 to 2.0 Fe 100 NZO 279,8 0.1 0,001 to 0,03 loo0 NZO 0,Ol to 2.0 Mn 100 NZO 27

22、9.8 o, 1 232.0 0,3 0,003 to 0,05 loo0 NZO 0,05 to 5,O Ni 100 NZO 1000 NZO 232.0 0.3 Table 1 - Instrumental parameters and characteristics of calibration functions Notes 1 2 2 3 3 4.4.3 Prepare one or more blank solutions (see 4.4.1 without the addition of the relevant element to be determined. 4.5 A

23、djustment of the atomic absorption spectrometer SAFETY PRECAUTION : Follow the manufacturers recommendation on igniting and extinguishing the flame. Optimize the response of the instrument at the wavelength given for the element being determined. See table 1. Preheat the burner for about 5 min and t

24、hen adjust the fuel and correct 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. 4.6 Atomic absorbance measurements 4.6.1 Aspirate first the blank sol

25、ution and then the calibration and test solutions consecutively and record the readings. Aspirate water between each solution. Make at least Wo measurements for each solution. Solids which build up on the burner slit must be removed, otherwise they will cause a decrease of sensitivity. 4.6.2 Prepare

26、 a calibration curve by plotting the obtained ab- sorbance values of the calibration solutions corrected for the blank against the concentration, in milligrams per litre, of the element. 4.6.3 Convert the absorbance values of the test solutions corrected for the blank to milligrams of the element pe

27、r litre by means of the calibration curve. 5 Expression of results 5.1 Calculation The element content, expressed as a percentage by mass, is given by the formula cx v 104 x m where c is the concentration, in milligrams per litre, of the element in the test solution; Y is the dilution volume, in mil

28、lilitres; m is the mass, in grams, of the test portion. 5.2 Permissible tolerances The deviations between three independent determinations shall not exceed 0,2 times the element content in per cent (absolute value). 5.3 Final result Report the arithmetical mean of acceptable determinations rounded t

29、o the nearest value as shown in table 2. Table 2 - Rounding of results Content Round to the nearest % (mim) % imlrn from 0.01 to 0,l over 0,l to 0.5 If the element content is below 0,Ol % (m/m), report it as less than 0.01 % (m/m). CEN ENx2b27-3 93 m 3404589 0047LBb 774 m Page 5 EN 27627-3 : 1993 An

30、nex ZA (normative) Normative references to international publications with their relevant European publications 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 pu

31、blications 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 amendments). Publication Year Title - Year IS0 7627-1 Hardmetals - Chemical analysis by flame EN 27627-1 atomic absorption spectrometry - Part 1 : General requirements