EN 27627-5-1993 en Hardmetals - Chemical Analysis by Flame Atomic Absorption Spectrometry - Part 5 Determination of Cobalt Iron Manganese Molybdenum Nickel Titanium and Vanadium in.pdf

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1、CEN ENx27627-5 93 3404589 0043192 T78 9 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 27627-5 April 1993 UDC 669.018.25 : 620.1 : 543.422 Descriptors: Powder metallurgy, hard metals, chemical analysis, determination of content, transition metals, cobalt, iron, manganese, molybdenum, nickel, t

2、itanium, vanadium, spectrometric analysis, atomic absorption spectrophotometry English version Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Part 5 : Determination of cobalt, iron, manganese, molybdenum, nickel, titanium and vanadium in contents from 0,5 to 2 % (m/m) (IS0

3、7627-5 1983) Mtaux-durs - Analyse chimique par spectromtrie dabsorption atomique dans la flamme - Partie 5: Dosage du cobalt, du fer, du manganse, du molybdne, du nickel, du titane et du vanadium des teneurs Hartmetalle - Chemische Analyse durch Flammenatomabsorptionsspektrometrie - Teil 5: Bestimmu

4、ng des Cobalt-. Eisen-, Mangan-, Molybdn-, Nickel-, Titan- und Vanadiumgehaltes von 0,5 bis 2 % (m/m) comprises entre 0,5 et 2 % (m/m) (IS0 7627-5 : 1983) (IS0 7627-5 : 1983) This European Standard was approved by CEN on 1993-04-02. CEN members are bound to comply with the CENKENELEC Internal Regula

5、tions 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 Central Secretariat or to any CEN member. This Eur

6、opean 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 Central Secretariat has the same status as the official versions. CEN members are the nat

7、ional standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr N

8、ormung Central Secretariat: rue de Stassart 36, B-1050 Brussels O 1993 Copyright reserved to CEN members Ref. No. EN 27627-5 : 1993 E CEN ENSZ7627-5 93 m 3404589 0047193 904 m Page 2 EN 27627-5 : 1993 Foreword In 1992, IS0 7627-5 : 1983 Hardmetals - Chemical analysis byjame atomic absorption spectro

9、metry - part 5: Deterrnination of cobalt, iron, manganese, molybden, nickel, titanium and vanadium in contents fmmz 0,5 to 2 % (mim) was submitted to the CEN Primary Questionnnaire procedure. Following the positive result of the CEN/CS Proposal IS0 7627-5 : 1983 was submitted to the CEN Formal Vote.

10、 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 text or by endorsement, at the latest by October 1993, and conflicting national standards shail be withdrawn at the latest by October 1993. Acco

11、rding to the Internal Regulations of CENKENELEC, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. NCYT

12、E. The European references to international publications are given in annex ZA (normative). CEN EN*27627-5 93 H 3404589 0047l194 40 Page 3 EN 27627-5 : 1993 1 Scope and field of application This part of IS0 7627 specifies the method to be used for the determination of cobalt, iron, manganese, molybd

13、enum, nickel, titanium and vanadium contents of hardmetals within the range 0,5 to 2 % (m/m) by flame atomic absorption spectrometry. General requirements concerning the field of application, prin- ciple, interfering elements, apparatus, sampling and test report are given in IS0 7627/ 1. NOTE - Dete

14、rmination of element contents in high concentration by the atomic absorption spectrophotometry method yields a wider scat- tering of results than are obtainable by other methods, .e. IS0 3909, 4501, 4503 and 4883. See also clause 4.2. 2 Reference IS0 762711, Hardmetals - Chemical analysis by flame a

15、tomic absorption spectrometry - Part I: General requirements. 3 Reagents 3.1 Hydrofluoric acid, g 1.12 glml. 3.2 Nitric acid, 1,42 g/ml. 3.3 Ammonium fluoride, 0,l g/ml solution. 3.4 Caesium chloride, 0,Ol g/ml solution. 3.5 High-purity stock solutions, for calibration purposes for each element to b

16、e determined, containing 1,ooO g of the element per litre. NOTE - This value is understood to establish a maximum limit of 1,ODO 5 g 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 polytetrafl

17、uorethylene beaker or a beaker of other suitable material. Cover the beaker. 4.2 Dissolution of the test portion Add 10 ml of water, 5 ml of the hydrofluoric acid i3.1). and then 5 ml of the nitric acid (3.2). drop by drop, to the beaker containing the test portion (4.1) and heat gently until the te

18、st portion is completely dissolved. Add 10 ml of the caesium chloride solution (3.4) and 10 ml of the ammonium fluoride solution (3.3). 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 vol

19、ume for the analysis according to table 1 in the following way. 4.3.1 Dilution volume 100 ml: use the solution in 4.2. 4.3.2 The concentration 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

20、 one-mark volumetric flask. Add 10 ml of the caesium chloride solution (3.4). Add 10 ml of the ammonium fluoride solution 13.3) and dilute to 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 pos

21、sible to the test portion to be analysed, but without making up to volume. Then add in- creasing volumes of properly diluted stock solutions of the elements to be determined according to the Concentration ranges to be covered. Make up to 100 ml and mix. CEN EN*2?62?-5 93 m 3404589 0047195 787 m Dilu

22、tion volume (Y) Reciprocal sensitivity, Element for 1 g test portion” Oxidant Wavelength for 1 % absorption” Linear range) ml nm Ciglml % 352,7 20 0.1 to 15 248.3 03 0,03 to 2.0 Co 100 N2O Fe lo00 N2O Mn lo00 N2O Mo 100 N2O Ni loo0 N2O Ti 100 N2O V lo00 N2O 279.8 o, 1 0.01 to 2.0 313,3 6 0.06 to 10.

23、0 232,o 0.3 0,051 to 5.0 364.3 318,4 1 .o 0,l to 5,O 30 0.2 to 10 Page 4 EN 27627-5 : 1993 Notes 1 2 3 and 4 2 1 Content Round to the nearest % mlm % (mim) from 0,5 to 1 0,02 over 1 to 2 0,05 4.4.2 Also prepare calibration solutions with a diluted matrix in accordance with 4.3 for dilution volumes o

24、f 1 o00 ml, if necessary. 7 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 Adjustment of the atomic absorption spectrometer SAFETY PRECAUTION : Follow the manufacturers recommendation on igniting and extinguishing the flame. O

25、ptimize 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 then adjust the fuel and correct the burner to obtain maximum absorption while aspirating a calibration solution. Make sure that the absorbance reading

26、 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 solution and then the calibration and test solutions consecutively and record the readings. Aspirate water between each solution. Make at least two measu

27、rements 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 a calibration curve by plotting the obtained ab- sorbance values of the calibration solutions corrected for the blank against the concentration, in

28、 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 per 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

29、by the formula cx Y 104 x m where c is the concentration, in milligrams per litre, of the element in the test solution; V is the dilution volume, in millilitres; m is the mass, in grams, of the test portion. 5.2 Permissible tolerances The deviations between three independent determinations shall not

30、 exceed 0,l times the element content in per cent (absolute value). 5.3 Final result Report the arithmetical mean of acceptable determinations rounded to the nearest value as shown in table 2. If the element content is below 0,5 % (mim), use the relevant part of this standard. If the element is grea

31、ter than 2 % (m/m), report it as greater than 2 % (mlm. CEN EN+27627-5 93 m 3404589 004719b bL3 m Page 5 EN 27627-5 : 19921 Annex ZA (normative) Normative references to international publications with their relevant European publications This European Standard incorporates by dated or undated refere

32、nce, provisions from other publications. These normative references are cited at the appropriate places 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 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 Title EN/HD IS0 7627-1 Hardmetalc - Chemical analysis by flame EN 27627-1 atomic absorption spectrometry - Part 1 : General requirements