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GB/T 5121.22-2008: Methods for chemical analysis of copper and copper alloys -- Part 22: Determination of cadmium content
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Methods for chemical analysis of copper and copper alloys -- Part 22: Determination of cadmium content
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GB/T 5121.22-2008
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| GB/T 5121.22-1996 | English | 199 |
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Copper and copper alloys--Determination of cadmium content
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Basic data | Standard ID | GB/T 5121.22-2008 (GB/T5121.22-2008) | | Description (Translated English) | Methods for chemical analysis of copper and copper alloys -- Part 22: Determination of cadmium content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H13 | | Classification of International Standard | 77.120.30 | | Word Count Estimation | 11,17 | | Date of Issue | 2008-06-17 | | Date of Implementation | 2008-12-01 | | Older Standard (superseded by this standard) | GB/T 5121.22-1996; GB/T 13293.3-1991 | | Adopted Standard | ISO 5960-1984, MOD | | Regulation (derived from) | National Standard Approval Announcement 2008 No.10 (Total No.123) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies the method for determination of copper and copper alloy cadmium content. This method is suitable for the determination of copper and copper alloy cadmium content. Measuring range: 0. 00005% to 0. 0010%. Method Two flame atomic absorption spectrometry determination of the method provides copper and copper alloy cadmium content. This method is suitable for the determination of copper and copper alloy cadmium content. Measuring range: 0. 50% to 1. 50%. | GB/T 5121.22-2008: Methods for chemical analysis of copper and copper alloys -- Part 22: Determination of cadmium content
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Methods for chemical analysis of copper and copper alloys Part 22. Determination of cadmium content
ICS 77.120.30
H13
National Standards of People's Republic of China
Replacing GB/T 5121.22-1996
Partially replace GB/T 13293.3-1991
Copper and copper alloys -
Determination of cadmium content. Part 22
(ISO 5960. 1984, Copperaloys-Determinationofcadmiumcontent-
Flameatomicabsorptionspectrometricmethod, MOD)
Posted 2008-12-01 2008-06-17 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
GB/T 5121 "Copper and copper alloy chemical analysis method" a total of 27 sections.
--- Part 1. Determination of copper content;
--- Part 2. Determination of phosphorus content;
--- Part 3. Determination of lead content;
--- Part 4. Carbon, Determination of sulfur content;
--- Part 5. Determination of nickel content;
--- Part 6. Determination of bismuth content;
--- Part 7. Determination of arsenic content;
--- Part 8. Determination of oxygen content;
--- Part 9. Determination of iron content;
--- Part 10. Determination of tin content;
--- Part 11. Determination of zinc content;
--- Part 12. Determination of antimony content;
--- Part 13. Determination of aluminum content;
--- Part 14. Determination of manganese content;
--- Part 15. Determination of cobalt content;
--- Part 16. Determination of chromium content;
--- Part 17. Determination of beryllium content;
--- Part 18. Determination of magnesium content;
--- Part 19. Determination of silver content;
--- Part 20. Determination of zirconium content;
--- Part 21. Determination of titanium content;
--- Part 22. Determination of cadmium content;
--- Part 23. Determination of silicon content;
--- Part 24. selenium, tellurium content was measured;
--- Part 25. Determination of boron content;
--- Part 26. Determination of mercury content;
--- Part 27. Inductively coupled plasma atomic emission spectrometry.
Part is divided into 22 sections.
This section includes a method, Method II.
The second method to modify the part using ISO 5960. 1984 "copper alloys - Determination of cadmium content - Flame Atomic Absorption Spectrometry", mainly within technology
The volume, and ISO 5960. 1984 the same structure does not correspond exactly to the preparation of the specific technical differences, see Appendix A, Appendix B.
This Part replaces GB/T 5121.22-1996 "Copper and copper alloys chemical analysis of cadmium content - Flame - Atomic Absorption Spectrometry
Law "and GB/T 13293.3-1991" Determination of chromium, manganese, cadmium purity copper cathode Zeeman effect electrothermal atomic absorption spectrometry
the amount".
This portion of the GB/T 5121.22-1996, GB/T 13293.3-1991 compared to the main changes are as follows.
--- One method of GB/T 13293.3-1991 amendment complements the quality assurance and control provisions, increasing the precision of the terms;
--- Second method is GB/T 5121.22-1996 amendments, supplements the provisions of quality assurance and control, increasing the precision of the terms.
This section in Appendix A, Appendix B is an informative annex.
This part is proposed by the China Nonferrous Metals Industry Association.
The non-ferrous metal part by the National Standardization Technical Committee.
This section Chinalco Luoyang Copper Co., Ltd., Beijing General Research Institute of Mining and Metallurgy, China Nonferrous Metals Industry is responsible Institute of Standards Metrology and Quality
Drafted.
A method in this section was drafted by Beijing General Research Institute of Mining and Metallurgy.
A method in this section by the Jiangxi Copper Group Co., Ltd., Jinchuan Group Co., Ltd. participated in the drafting.
The main drafters of this section a method. Feng advanced Lihua Chang Feng Yu Qing, high dielectric level, Yangsu Zhi.
The main part of a method of verification of people. Percentage light cents, Shen Guang Xin, Lv Qingcheng, Zhang Jihong.
This section Method Two Chinalco Luoyang Copper Co. drafted.
The second method section by the Beijing Nonferrous Metal Research Institute, Beijing General Research Institute of Mining and Metallurgy participated in the drafting.
Method Two main drafters of this section. Wang Yan, Zhang Hui, Deng Wan Mei.
The two main methods in this section to verify. Zhang Ying new Tangshu Fang, Zhang Li, in force.
This part of the standard replaces the previous editions are.
--- GB/T 5121.22-1996, GB/T 13293.3-1991.
Copper and copper alloys -
Determination of cadmium content. Part 22
Method 1 a Zeeman effect electrothermal atomic absorption spectrometry
1.1 Scope
This method specifies the method for determination of copper and copper alloy cadmium content.
This method is applicable to the determination of copper and copper alloy cadmium content. Measurement range. 0.00005% to 0.0010%.
1.2 Principle of the method
Sample dissolved in nitric acid, a volume of the test solution injected into the electrothermal atomizer with Zeeman effect atomic absorption spectrometer
228.8nm wavelength absorbance measurement of cadmium, cadmium mass fraction calculated by working curve method.
1.3 Reagents
Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity. experiment
The utensils were soaked 12h, washed thoroughly with water and nitric acid (1.3.3).
1.3.1 Copper (Cu mass fraction ≥99.99%, cadmium mass fraction < 0.00005%).
1.3.2 nitric acid (1 + 1) BVⅢ.
1.3.3 nitric acid (1 + 19).
1.3.4 copper substrate solution (100g/L). mass fraction is called 20.00g copper metal (copper ≥99.99%, mass fraction of cadmium
< 0.00005%) were placed in 400mL beaker was added in 160mL nitric acid (1.3.2), Leng Rong. After intense stop the reaction, add cold
Heat to dissolve completely, purge nitrogen oxides boiling, cooled to room temperature. Transferred to 200mL volumetric flask, dilute with water to volume, and mix.
1.3.5 cadmium standard stock solution. Weigh 0.2500g metal cadmium (cadmium mass fraction ≥99.95%) placed in 150mL beaker,
10mL of nitric acid (1.3.2), the cover sheet pan, on low heat until completely dissolved, cooled to room temperature. Transferred to 500mL volumetric flask, diluted with water
To the mark, and mix. This solution 1mL containing 500μg cadmium.
1.3.6 Cadmium standard solution A. Pipette 5.00mL cadmium standard stock solution (1.3.5) in 500mL flask, diluted with water to the mark,
Mix well. This solution 1mL containing 5μg cadmium.
1.3.7 Cadmium standard solution B. Pipette 10.00mL cadmium standard solution A (1.3.6) in 250mL volumetric flask, dilute to the mark with water, mix
uniform. This solution 1mL containing 0.2μg cadmium.
1.4 Instrument
1.4.1 graphite furnace atomic absorption spectrometer. with electrothermal atomizer, micro sampler or autosampler, cadmium hollow cathode lamp and Zeeman effect
Background correction shall devices.
1.4.2 The graphite furnace atomic absorption spectrometer should meet the following specifications.
--- Lowest sensitivity. curve used in the arithmetic series of standard solution of greatest concentration, absorbance should not be less than 0.300.
--- Correlation coefficient curve is not less than 0.995.
--- Low precision requirements. the highest concentration of standard solution, the absorbance measured 10 times, calculate the mean and standard deviation. The standard
Standard deviation should not exceed 1.5% of the average absorbance. The lowest concentration of standard solutions (not zero concentration standard solution
Solution), 10 times the absorbance measured, calculating the standard deviation. The standard deviation should not exceed the average absorbance of the highest concentration of the standard
0.5% of the value.
1.5 Sample
Sample processed into crumb-like.
1.6 Analysis Steps
1.6.1 Sample
Table 1. Weigh the sample (1.5), accurate to 0.0001g.
Table 1 Sample volume and minute volume of test solution to take
Cadmium mass fraction /% Sample volume/g dispensing volume of test solution/mL
The total amount of 0.00005 to 0.0001 1.000
> 0.0001 0.0005 2.000 25
> 0.0005 0.0010 2.000 10
1.6.2 Determination of the number of
Independent secondary measurement averaged.
1.6.3 Blank test
Weigh the same quantity of pure copper test (1.3.1), along with sample blank test, "zero" concentration solution standard solution as the test series
Material blank.
1.6.4 Determination
1.6.4.1 The sample (1.6.1) in 150mL beaker, add 8mL nitrate (1.3.2), low-temperature heating until complete dissolution, boiling flooding
In addition to oxides of nitrogen, cooled to room temperature. Transferred to 100mL volumetric flask, dilute with water to volume, and mix.
1.6.4.2 when cadmium concentration above 0.0001%, according to Table 1 points to take the test solution (1.6.4.1) in 100mL flask, diluted with water
To the mark, and mix.
1.6.4.3 according to the manufacturer's instructions recommended conditions, to choose the best parameter cadmium electrothermal atomization and injection volume.
1.6.4.4 The instrument was adjusted to best condition, according to selected criteria (1.6.4.3) to adjust the electrothermal atomizer.
1.6.4.5 with a predetermined heating process air burning graphite tube 2 times.
1.6.4.6 predetermined sample volume, the test solution (1.6.4.1 or 1.6.4.2) injected into the atomizer, atomic technology, and measuring the absorbance of cadmium
degree. Each test solution measured 2 times the mean value, subtracting the mean absorbance of the blank test solution, to identify appropriate qualitative cadmium from the working curve
The amount of concentration.
1.6.5 Draw the curve
Pipette respectively 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL cadmium standard solution B (1.3.7) in a group
100mL flask, adding the appropriate amount of press Sample volume copper matrix solution (1.3.4), diluted with water to volume, and mix. In the test solution and measurement phase
Under the same conditions, while measuring the absorbance series of standard solution, standard solution each measuring 2 times the mean value, minus "zero" concentration of the solution
The average absorbance. In the mass concentration of cadmium as abscissa, absorbance ordinate, drawing working curve cadmium.
1.7 Calculation of Analytical Results
According to equation (1) to calculate the mass fraction of cadmium (Cd), expressed in%.
(Cd) = ρ
· V0 · Vp 2 × 10-6
M1 · Vp 1 ×
100 (1)
Where.
Mass concentration ρ --- from the working curve Richard cadmium in micrograms per milliliter (μg/mL);
--- Test solution a total volume V0, in milliliters (mL of);
Vp 1 --- dispensing volume of test solution, in milliliters (mL);
Vp 2 --- volume measurement of test solution, in milliliters (mL);
M1 --- quality of sample in grams (g).
The obtained results are shown to fourth place after the decimal point. If the cadmium content of less than 0.0010%, indicating to fifth place after the decimal point.
1.8 Precision
1.8.1 Repeatability
Test value two independent test results obtained under repeated conditions, within the average range Table 2 shows the two test results must
Obtained.
Table 2 Repeatability limit
Cadmium mass fraction /% 0.00005 0.00053 0.0010
1.8.2 Reproducibility
Test value two independent test results obtained under reproducibility conditions, the average value in the range given in Table 3, the two test results
The absolute difference does not exceed the reproducibility limit (R), exceeds reproducibility limit (R) does not exceed 5%, reproducibility limit (R) linear data in Table 3
Obtained by interpolation.
Table 3 reproducibility limit
Cadmium mass fraction /% 0.00005 0.00053 0.0010
Reproducibility limit (R) /% 0.00004 0.00023 0.0005
NOTE. reproducibility limit (R) is 2.83SR, SR for the reproducibility standard deviation.
1.9 Quality assurance and control
Application of national standards or industry-standard sample samples (both currently no time, can also be used to control standard alternative), weekly or biweekly school
Nuclear once this standard analytical methods effectiveness. When the process is out of control, we should find out why, after correcting errors, re-checked.
2 Method Two Flame Atomic Absorption Spectrometry
2.1 Scope
This method specifies the method for determination of copper and copper alloy cadmium content.
This method is applicable to the determination of copper and copper alloy cadmium content. Measuring range. 0.50% to 1.50%.
2.2 Principle of the method
Sample dissolved in nitric acid, using air - acetylene flame to flame atomic absorption spectrometer at a wavelength of 228.8nm, cadmium measuring absorbance.
2.3 Reagents
Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.
2.3.1 nitric acid (1 + 1).
2.3.2 hydrochloric acid (1 + 3).
2.3.3 copper solution (1.6g/L). Weigh 0.4000g copper (cadmium content of not more than 0.001%) were placed in 150mL beaker,
Added 5mL nitric acid (2.3.1) and heated to dissolve completely transferred to 250mL volumetric flask, dilute with water to volume, and mix.
2.3.4 Cadmium standard solution. Weigh 0.1000g pure cadmium (cadmium mass fraction ≥99.95%), placed in 250mL beaker, add 20mL
Hydrochloric acid (2.3.2) and heated until completely dissolved and transferred to 1000mL volumetric flask, dilute to the mark with water, mix this solution containing 1mL
100μg cadmium.
2.4 Instrument
2.4.1 flame atomic absorption spectrometer. a cadmium hollow cathode lamp.
2.4.2 The following indicators were in optimum working conditions, who can be used to achieve.
--- Sensitivity. measurement solution matrix consistent solution, characteristic concentration of cadmium should be less than 0.034μg/mL;
--- Precision. standard solution with the highest concentration of 10 times the absorbance measurements, the standard deviation should not exceed the average absorbance of 1.0%;
The lowest concentration of standard solution used (instead of "zero" standard solution) absorbance measured 10 times, and the standard deviation should not exceed the maximum concentration
0.5% of the mean absorbance of the standard solution;
--- Linear curve. The curve is divided into five sections according to concentration, absorbance difference between the absorbance difference between the highest and the lowest segment of the segment
Ratio of not less than 0.7.
2.5 Sample
Thickness of less than 1mm debris.
2.6 Analysis Steps
2.6.1 Sample
Weigh 0.400g sample (2.5), accurate to 0.0001g.
2.6.2 Determination of the number of
Independent secondary measurement averaged.
2.6.3 Blank test
Along with the sample (2.6.1) blank test.
2.6.4 Determination
2.6.4.1 The sample (2.6.1) in 150mL beaker, was added 5mL of nitric acid (2.3.1) cover sheet pan, over low heat until completely dissolved
Solutions for removing nitrogen oxides was boiled and cooled. Transferred to 250mL volumetric flask, dilute with water to volume, and mix.
2.6.4.2 Pipette 10.00mL solution in 100mL flask, add 5mL nitric acid (2.3.1) diluted with water to volume, and mix.
2.6.4.3 using air - acetylene flame atomic absorption spectrometer at a wavelength of 228.8nm, and series of standard solution at the same time, water-zero,
Measuring the absorbance of the solution. The absorbance is measured by subtracting the absorbance of the blank solution together with the sample, the quality of the corresponding cadmium isolated from the working curve
concentration.
2.6.5 Draw the curve
2.6.5.1 Pipette 0mL, 0.50mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL cadmium standard solution (2.3.4) were placed in a
Set 100mL flask, add 10mL copper solution (2.3.3), 5mL nitric acid (2.3.1), dilute with water to volume, and mix.
2.6.5.2 In the same measurement conditions and sample solution, the standard solution absorbance measurement series, minus the series of standard solution of "zero" concentration
Absorbance of the solution to the mass concentration of cadmium as abscissa, absorbance ordinate drawing working curve.
2.7 Analysis of calculation results
According to equation (2) to calculate the mass fraction of cadmium (Cd), expressed in%.
(Cd) = ρ
· V0 · Vp 2 × 10-6
M1 · Vp 1 ×
100 (2)
Where.
Mass concentration ρ --- from the working curve Richard cadmium in micrograms per milliliter (μg/mL);
--- Test solution a total volume V0, in milliliters (mL of);
Vp 2 --- take partial volumes of test solution diluted in milliliters (mL);
Vp 1 --- dispensing volume of test solution, in milliliters (mL);
M1 --- quality of sample in grams (g).
The results are expressed to second place after the decimal point.
2.8 Precision
2.8.1 Repeatability
Test value two independent test results obtained under repeated conditions, the average value within the range given in Table 4, two test results must
Obtained.
Table 4 repeatability limit
Cadmium mass fraction /% 0.500 0.96 1.44
2.8.2 Reproducibility
Test value two independent test results obtained under reproducibility conditions, the average value in the range given in Table 5, two test results
The absolute difference does not exceed the reproducibility limit (R), exceeds reproducibility limit (R) does not exceed 5%, reproducibility limit (R) linear data in Table 5
Obtained by interpolation.
Table 5 reproducibility limit
Cadmium mass fraction /% 0.500 0.96 1.44
Reproducibility limit (R) /% 0.017 0.04 0.05
NOTE. reproducibility limit (R) is 2.83SR, SR for the reproducibility standard deviation.
2.9 Quality assurance and control
Application of national standards or industry-standard sample samples (both currently no time, can also be used to control standard alternative), weekly or biweekly school
Nuclear once this standard analytical methods effectiveness. When the process is out of control, we should find out why, after correcting errors, re-checked.
Appendix A
(Informative)
This section Method Two reg number and ISO 5960. 1984 reg number control
Table A. 1 shows the method of this section and Chapter II Article No. 5960 ISO . 1984 reg number control list.
Table A. A part of Method II reg number and ISO 5960. 1984 reg number control
This section Method Two reg number ISO 5960. 1984 reg number
2.1 1
2.2 2
2.3 3
2.4 4
2.5 5
2.6 6
2.6.1 6.1
2.6.2 -
2.6.3 6.4
2.6.4 6.3
2.6.5 6.2
2.7 7
2.8 -
2.9 6.5
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