1、International Standard ( 4740 0 Q 4 4igie INTERNATIONAL ORGANIZATION FOR STANDARDIZATION*MEXYHAPOHAR OPrAHH3AUHR n0 CTAHAAPTH3AUH!4*ORGANlSATlON INTERNATIONALE DE NORMALISATION Copper and copper alloys - Determination of zinc content - Flame atomic absorption spectrometric method Cuivre et alliages
2、de cuivre - Dosage du zinc - Mkhode par spectromktrie dabsorption atomique dans la flamme First edition - 1966-07-01 Gi UDC 669.3 : 643.422 : 546.47 Ref. No. IS0 4740-1966 (E) Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction
3、 or networking permitted without license from IHS-,-,-Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees.
4、Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by
5、 the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the IS0 Council. They are approved in accordance with IS0 procedures requiring at least 75 % approval by the member bodies voting. International Standard IS0 4740 was prep
6、ared by Technical Committee ISO/TC 26, Copper and copper alloys. 0 International Organization for Standardization, 1999 l Printed in Switzerland Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted withou
7、t license from IHS-,-,-INTERNATIONAL STANDARD IS0 4740-1985 (E) Copper and copper alloys - Determination of zinc content - Flame atomic absorption spectrometric method 1 Scope and field of application This international Standard specifies a flame atomic absorption spectrometric method for the determ
8、ination of the zinc content of all types of copper and copper alloys excluding copper alloys containing more than IO % h/m) of lead. The method is applicable to the determination of zinc contents between 0,001 and 6 % (m/m). 2 Reference ISO/R 1811, Chemical analysis of copper and copper alloys - Sam
9、pling of copper refinery shapes. 1) 3 Principle Dissolution of a test portion in fluoroboric-nitric acid, followed by aspiration into the air/acetylene flame of a flame atomic ab- sorption spectrometer. Comparison of the absorption of the resonance energy of zinc at 213,8 nm with those of standard m
10、atching solutions of zinc. 4 Reagents During the analysis, use only reagents of recognized analytical grade, and only distilled or deionized water. 4.1 Fluoroboric-nitric acid, attack solution. Mix together 300 ml of boric acid solution (40 g/l), 30 ml of hydrofluoric acid 40 % (V/V), 500 ml of nitr
11、ic acid l l/Ml g/ml) and 150 ml of water. 4.2 Copper, base solution Weigh IO,0 g of copper containing not more than 0,000 2 % (m/m) zinc into a 1 000 ml PTFE beaker. Add 400 ml of the attack solution (3.1) and warm until the copper is dissolved. Boil the solution until all brown fumes have been ex-
12、pelled. Cool and transfer the solution to a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. 50 ml of this solution contains 1 g of copper and 40 ml of at- tack solution (4. I). 4.3 Zinc, standard stock solution, corresponding to 5 g of Zn per litre. Transfer 2,5 + 0,000 1 g
13、of zinc metal (99,99 % purity) to a 250 ml tall-form beaker. Add 50 ml of nitric acid solution (Q 1.40 g/ml, diluted 1 + I), cover and heat gently until the metal is dissolved. Boil the solution for several minutes to expel nitrous fumes, then cool. Transfer the solution to a 500 ml one- mark volume
14、tric flask, dilute to the mark with water and mix. 1 ml of this standard solution contains 5 mg of Zn. 4.4 Zinc, standard solution, corresponding to 0,5 g of Zn per litre. Transfer 100.0 ml of the zinc standard solution (3.3) to a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and
15、 mix. 1 ml of this standard solution contains 0,5 mg of Zn. 4.5 Zinc, standard solution, corresponding to 0,05 g of Zn per litre. Transfer 10.0 ml of the zinc standard stock solution (3.3) to a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix. 1 ml of this standard solution
16、contains 0,05 mg of Zn. 1) Under revision 1 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 4740-1985 (El 4.6 Zinc, standard solution, corresponding to 0,Ol g of Zn u
17、tion (4.2) shown in table 2. Dilute to the mark with water and per litre. mix. Transfer 20,O ml of the zinc standard solution (3.4) to a 1 000 ml one-mark volumetric flask. Table 2 Dilute to the mark with water and mix. Volume of zinc standard solution (4.6) Volume of copper base solution (4.2) Mass
18、 of zinc per 100 ml after dilution 1 ml of this standard solution contains 0,Ol mg of Zn. t ml ml w 0” 50 0 5 Apparatus Ordinary laboratory apparatus, and 5.1 PTFE beakers, of capacity 250 ml. 5.2 Burette, graduated in 0,05 ml. 5.3 Flame atomic absorption spectrometer, including a light source emitt
19、ing characteristic zinc spectral lines, for exam- ple a hollow-cathode or electrodeless discharge lamp. 5.4 Compressed air supply. 5.5 Cylinder of acetylene. 6 Sampling Sampling shall be carried out in accordance with ISO/R 1811. The sample should preferably be in the form of drillings with a maximu
20、m thickness of 0,3 mm. 7 Procedure 7.1 Preparation of standard matching solutions 7.1.1 Zinc contents between 0,001 and 0.01 % (m/m) Into a series of four 100 ml one-mark volumetric flasks, in- troduce the volumes of the zinc standard solution (4.6) and base solution (4.2) shown in table 1. Dilute t
21、o the mark with water and mix. Table 1 Volume of zinc standard solution (4.6) ml Volume of copper base solution (4.2) ml Mass of zinc per 100 ml after dilution w 0* 50 ? 1 50 0.01 5 50 0,05 10 50 0.10 * Blank test on reagents for calibration. 7.1.2 Zinc contents between 0,005 and 0.06 % (m/m) Into a
22、 series of six 200 ml one-mark volumetric flasks, introduce the volumes of the zinc standard solution (4.5) and base sol- 2 * Blank test on reagents for calibration. 7.1.3 Zinc contents between 0,05 and 0.60 % (m/m) Into a series of six 200 ml one-mark volumetric flasks, introduce the volumes of the
23、 zinc standard solution (4.4) and base sol- ution (4.2) shown in table 3. Dilute to the mark with water and mix. Transfer 100,O ml of these solutions to each of six 1 000 ml one-mark volumetric flasks, dilute to the mark and mix. Table 3 Volume of I Volume of 1 Mass of zinc zinc standard solution (3
24、.4) ml 0” 1 2 4 a 12 copper base solution (3.2) ml 50 50 50 50 50 50 per 106 ml after final dilution w 0 0,025 0,05 0,lO 0,20 0.30 * Blank test on reagents for calibration. 7.1.4 Zinc contents between 0.5 and 6 % imImI Into a series of six 200 ml one-mark volumetric flasks, introduce the volumes of
25、the zinc standard stock solution (4.3) and base solution (4.2) shown in table 4. Dilute to the mark with water and mix. Transfer IO,0 ml of these solutions to each of six 1 Ooo ml one-mark volumetric flasks, dilute to the mark and mix. Table 4 Volume of Volume of zinc standard copper base stock solu
26、tion (4.3) solution (4.2) ml ml 0” 50 1 50 2 50 4 50 a 50 12 50 * Blank test on reagents for calibration. Mass of zinc per 160 ml after final dilution 43 0 0,025 0,05 0,lO 0,20 0,30 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reprod
27、uction or networking permitted without license from IHS-,-,-IS0 4740-1985 (El 7.2 Preparation of test solution 7.2.1 Transfer a test portion of 1 f 0,000 2 g to a PTFE beaker (5.1). If heating is carried out in a water bath, polypropylene or low-density polyethylene beakers may be used. 7.2.2 Add 40
28、 ml of the attack solution (4. I), cover, and warm gently until the test portion is dissolved, then heat at about 80 OC until nitrous fumes have been expelled. Wash down the cover and sides of the beaker and cool. 7.2.3 For zinc contents between 0,001 and 0,Ol % imImI, transfer the solution (7.2.2)
29、quantitatively to a 100 ml one-mark volumetric flask, dilute to the mark and mix. 7.2.4 For zinc contents between 0,005 and 0,06 % (m/m), transfer the solution (7.2.2) quantitatively to a 200 ml one-mark volumetric flask, dilute to the mark and mix. 7.2.5 For zinc contents between 0,05 and 0,60 % (m
30、/m), transfer the solution (7.2.2) quantitatively to a 200 ml one-mark volumetric flask, dilute to the mark and mix. Transfer 100 ml of this solution to a 1 000 ml one-mark volumetric flask. Dilute to the mark and mix. 7.2.6 For zinc contents between 050 and 6 % (m/m), transfer the solution (7.2.2)
31、quantitatively to a 200 ml one-mark volumetric flask, dilute to the mark and mix. Transfer 10,O ml of this solution to a 1 000 ml one-mark volumetric flask. Dilute to the mark and mix. 7.3 Spectrometric measurements 7.3.1 Preparation of apparatusl) Turn on the electric system and allow it to warm up
32、. Adjust the zinc hollow-cathode lamp and set the wavelength drum to 213,8 nm. Regulate the air/acetylene flame. 7.3.2 Measurement of standard matching solutions Transfer portions of the standard matching solutions to small beakers and atomize into the flame. Take care to maintain a constant rate of
33、 aspiration over the full range of standard mat- ching solutions. Record the absorbance of each standard mat- ching solution. After each aspiration of a standard matching solution, atomize a small amount of water to clean the burner. Signal amplification may be necessary for the series of standard m
34、atching solutions having the lowest concentration of zinc (7.1.1). 7.3.3 Plotting of calibration curves Using the measurements from 7.3.2, plot calibration curves with the zinc concentrations (mg/lOO ml) on the abscissa and corresponding absorbance values on the ordinate axis, subtracting the blank
35、value from each standard value. NOTE - Recent work has demonstrated that calibration graphs may suffer from excessive curvature. A non-acceptable curvature would result when the mid-point calibration absorbance exceeds 0.55 times the absorbance of the maximum calibration solution. If this situation
36、is encountered, the calibration solutions (7.1) should be diluted to the minimum standard volume needed to attain the curvature criterion stated. The test solutions (7.2) should also be diluted in the same pro- portion. 7.3.4 Measurement of test solution Measure the absorbances of the test solution
37、and blank in the same manner as the standard matching solutions (7.3.2). Bracket the test solution by two appropriate standard matching solutions. Carry out all measurements consecutively and without interruption in order to minimize instrumental fluctua- tions. 7.4 Blank test Carry out a blank test
38、 at the same time as the determination and following the same procedure, using the same quantities of reagents and of pure copper as for the determination but omit- ting the test portion. 7.5 Check test Make a preliminary check of the apparatus by preparing a sol- ution of standard material or a syn
39、thetic sample containing a known amount of zinc and of composition similar to the material to be analysed, and carrying out the procedure as specified in 7.2 and 7.3. 8 Expression of results Using the appropriate calibration curve (7.3.31, determine the amount of zinc in the test solution correspond
40、ing to the measured absorbance. Calculate the zinc content, as a percent- age by mass, according to the formula (rn2 - ml) xf x V 1000 x m. where m, is the mass, in grams, of the test portion (1 g); 1) Refer to the manufacturers manual for specific details of optimum instrument settings. 3 Copyright
41、 International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 4740-1985 (E) ml is the mass, in milligrams, of zinc found in the blank test solution; m2 is the mass, in milligrams, of zinc f
42、ound in the test solution; f is the ratio between the volume of the first flask, in millilitres, and the volume, in millilitres, transfered to the se- cond flask; f = 1 when the first flask contains the final test solution, i.e., if no successive dilution is made. V is the volume, in millilitres, of
43、 the flask containing the final test solution. 9 Test report The test report shall include the following particulars : a) an identification of the sample; b) the reference of the method used; c) the results and the method of expression used; d) any characteristics noted during the determination; e) any operations not included in this International Stan- dard, or regarded as optional. Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
