GB/T 4103.14-2009 English PDF (GB/T4103.14-2009)

GB/T 4103.14-2009: Methods for chemical analysis of lead and lead alloys -- Part 14: Determination of cadmium content -- Flame atomic absorption spectrophotometry
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GB/T 4103.14-2009
GB
National Standard
of the People's Republic of China
Methods for chemical analysis of lead and lead
alloys - Part 14. Determination of cadmium content
­ Flame atomic absorption spectrophotometry
ISSUED ON. APRIL 8, 2009
IMPLEMENTED ON. FEBRUARY 1, 2010
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of People's Republic of China;
China National Standardization Management Committee
Table of Contents
Preface ... 3
1 Scope ... 5
2 Methods and Principles ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Analytical Steps ... 7
6 Calculation of analytical results ... 8
7 Precision ... 9
8 Quality assurance and control ... 10
References and Original Chinese Documents ... 11
Preface
GB/T 4103 " Methods for chemical analysis of lead and lead alloys" is divided
into 16 parts.
Part 1. Determination of tin content;
Part 2. Determination of antimony content;
Part 3. Determination of copper content;
Part 4. Determination of iron content;
Part 5. Determination of bismuth content;
Part 6. Determination of arsenic content;
Part 7. Determination of selenium content;
Part 8. Determination of tellurium content;
Part 9. Determination of calcium content;
Part 10. Determination of silver content;
Part 11. Determination of zinc content;
Part 12. Determination of thallium content;
Part 13. Determination of aluminum content;
Part 14. Determination of cadmium content ­ Flame atomic absorption
spectrophotometry;
Part 15. Determination of nickel content - Flame atomic absorption
spectrometry;
Part 16. Determination of copper, silver, bismuth, arsenic, antimony, tin, zinc
contents - Photoelectric direct-reading emission spectroscopy.
This is Part 14.
This Part was proposed by the China Nonferrous Metals Industry Association.
This part is administered by the National Standardization Technical Committee
for nonferrous metals.
The responsible drafting organizations of the Part. Zhuzhou Smelter Group Co.,
Ltd., and Henan Yuguang Gold and Lead Co., Ltd.
The participated drafting organizations of the Part. Shenzhen Lingnan
Nonferrous Metals Corporation Limited Shaoguan smelter, MCC Huludao
Nonferrous Metals Group, Shaanxi Dongling Zinc Industry Co., Ltd..
The main drafters of this Part. Zhong Yong, Zong Pu, the De Lei, Kong Jianmin,
Li Lijun, Liu Yingjing, painted red, Yang Yan, Liu Limin, and Wang Honggang.
Methods for chemical analysis of lead and lead alloys
Part 14. Determination of cadmium content
Flame atomic absorption spectrophotometry
1 Scope
This Part of GB/T 4103 specifies the determination of cadmium content in lead
and lead-cadmium alloys.
This Part applies to the determination of cadmium content in lead and lead-
cadmium alloys.
Measuring range. 0.000 1% -0.01%; 0.3% – 2.0%.
2 Methods and Principles
Samples shall be dissolved in nitrate; USE lead sulfate to precipitate and
separate lead; USE air-acetylene flame, at wavelength 228.8 nm of atomic
absorption spectrometer, to measure absorbance of cadmium. USE standard
curve method to calculate cadmium content.
3 Reagents
Unless otherwise stated, water used to prepare the solution and analysis in this
test shall be Grade 1 Water; all test utensils used in the test shall be immersed
with dilute nitrate (1 + 4), and shall be thoroughly washed with Grade 1 Water.
3.1 Nitrate (ρ 1.42 g / mL), superior grade purity.
3.2 Sulfate (ρ 1.84 g / mL); superior grade purity.
3.3 Nitrate (1 + 1).
3.4 Nitrate (1 + 3).
3.5 Sulfate (1 + 1).
3.6 Cadmium standard storage solution. WEIGH 0.500 0 g of metal cadmium
(mass fraction of cadmium ≥ 99.99%) into 250 mL beaker; ADD 20 mL of nitrate
(3.1); COVER with watch glass; HEAT it until completely dissolved; BOIL to
expel nitrogen oxides; COOL it; MOVE into 1 000 mL volumetric flask; USE
water to dilute the volume to the mark; SHAKE well. 1 mL of this solution
contains 0.5 mg of cadmium.
3.7 Cadmium standard solution. PIPETTE 10.00 mL of cadmium standard
storage solution (3.6) into 500 mL volumetric flask; ADD 20 mL of nitrate (3.3);
USE water to dilute the volume to the mark; MIX well; 1 mL of this solution
contains 10 μg of cadmium.
4 Instruments
Atomic absorption spectrometer, attached with cadmium hollow cathode lamp.
Under the optimum working conditions; those instruments which can achieve
the following targets may be used.
- Characteristic concentration. In solution consistent with the matrix of
measuring sample solution, the characteristic concentration of cadmium shall
be less than 0.05 μg / mL;
- Precision. USE standard solution of the highest concentration to measure
absorbance for 10 times, its standard deviation shall not exceed 1.0% of the
average absorbance; USE standard solution of the lowest concentration (not
the standard solution of “zero” concentration) to measure absorbance for 10
times, its standard deviation shall not exceed 0.5% of the average absorbance
of standard solution of the highest concentration;
- Linearity of working curve. DIVIDE the working curve into five sections
equally, based on concentration; the ratio between the absorbance difference
of the highest section AND the absorbance difference of the lowest section shall
not be less than 0.8;
Reference operating conditions of the instruments are shown in Table 1.
Table 4
Mass factor of
cadmium / %
0.0002 0.0020 0.0050 0.50 1.00 1.50
R / % 0.0001 0.0005 0.0010 0.04 0.05 0.06
Note. Reproducibility (R) is 2.8SR; SR is the reproducibility standard deviation.
8 Quality assurance and control
Standard samples of national-level or industrial-level shall be used (when these
2 samples are not available, controlled standard sample may be used for
substitution); effectiveness of this analytical method shall be calibrated weekly
or biweekly. When the process is out of control, root cause shall be found out;
After the error is corrected, calibration shall be repeated.
References and Original Chinese Documents
[1] GB/T 4103.14-2009 Methods for chemical analysis of lead and lead alloys - Part
14. Determination of cadmium content - Flame atomic absorption
ID=GB/T%204103.14-2009
GB/T 4103.14-2009
GB
National Standard
of the People's Republic of China
Methods for chemical analysis of lead and lead
alloys - Part 14. Determination of cadmium content
­ Flame atomic absorption spectrophotometry
ISSUED ON. APRIL 8, 2009
IMPLEMENTED ON. FEBRUARY 1, 2010
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of People's Republic of China;
China National Standardization Management Committee
Table of Contents
Preface ... 3
1 Scope ... 5
2 Methods and Principles ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Analytical Steps ... 7
6 Calculation of analytical results ... 8
7 Precision ... 9
8 Quality assurance and control ... 10
References and Original Chinese Documents ... 11
Preface
GB/T 4103 " Methods for chemical analysis of lead and lead alloys" is divided
into 16 parts.
Part 1. Determination of tin content;
Part 2. Determination of antimony content;
Part 3. Determination of copper content;
Part 4. Determination of iron content;
Part 5. Determination of bismuth content;
Part 6. Determination of arsenic content;
Part 7. Determination of selenium content;
Part 8. Determination of tellurium content;
Part 9. Determination of calcium content;
Part 10. Determination of silver content;
Part 11. Determination of zinc content;
Part 12. Determination of thallium content;
Part 13. Determination of aluminum content;
Part 14. Determination of cadmium content ­ Flame atomic absorption
spectrophotometry;
Part 15. Determination of nickel content - Flame atomic absorption
spectrometry;
Part 16. Determination of copper, silver, bismuth, arsenic, antimony, tin, zinc
contents - Photoelectric direct-reading emission spectroscopy.
This is Part 14.
This Part was proposed by the China Nonferrous Metals Industry Association.
This part is administered by the National Standardization Technical Committee
for nonferrous metals.
The responsible drafting organizations of the Part. Zhuzhou Smelter Group Co.,
Ltd., and Henan Yuguang Gold and Lead Co., Ltd.
The participated drafting organizations of the Part. Shenzhen Lingnan
Nonferrous Metals Corporation Limited Shaoguan smelter, MCC Huludao
Nonferrous Metals Group, Shaanxi Dongling Zinc Industry Co., Ltd..
The main drafters of this Part. Zhong Yong, Zong Pu, the De Lei, Kong Jianmin,
Li Lijun, Liu Yingjing, painted red, Yang Yan, Liu Limin, and Wang Honggang.
Methods for chemical analysis of lead and lead alloys
Part 14. Determination of cadmium content
Flame atomic absorption spectrophotometry
1 Scope
This Part of GB/T 4103 specifies the determination of cadmium content in lead
and lead-cadmium alloys.
This Part applies to the determination of cadmium content in lead and lead-
cadmium alloys.
Measuring range. 0.000 1% -0.01%; 0.3% – 2.0%.
2 Methods and Principles
Samples shall be dissolved in nitrate; USE lead sulfate to precipitate and
separate lead; USE air-acetylene flame, at wavelength 228.8 nm of atomic
absorption spectrometer, to measure absorbance of cadmium. USE standard
curve method to calculate cadmium content.
3 Reagents
Unless otherwise stated, water used to prepare the solution and analysis in this
test shall be Grade 1 Water; all test utensils used in the test shall be immersed
with dilute nitrate (1 + 4), and shall be thoroughly washed with Grade 1 Water.
3.1 Nitrate (ρ 1.42 g / mL), superior grade purity.
3.2 Sulfate (ρ 1.84 g / mL); superior grade purity.
3.3 Nitrate (1 + 1).
3.4 Nitrate (1 + 3).
3.5 Sulfate (1 + 1).
3.6 Cadmium standard storage solution. WEIGH 0.500 0 g of metal cadmium
(mass fraction of cadmium ≥ 99.99%) into 250 mL beaker; ADD 20 mL of nitrate
(3.1); COVER with watch glass; HEAT it until completely dissolved; BOIL to
expel nitrogen oxides; COOL it; MOVE into 1 000 mL volumetric flask; USE
water to dilute the volume to the mark; SHAKE well. 1 mL of this solution
contains 0.5 mg of cadmium.
3.7 Cadmium standard solution. PIPETTE 10.00 mL of cadmium standard
storage solution (3.6) into 500 mL volumetric flask; ADD 20 mL of nitrate (3.3);
USE water to dilute the volume to the mark; MIX well; 1 mL of this solution
contains 10 μg of cadmium.
4 Instruments
Atomic absorption spectrometer, attached with cadmium hollow cathode lamp.
Under the optimum working conditions; those instruments which can achieve
the following targets may be used.
- Characteristic concentration. In solution consistent with the matrix of
measuring sample solution, the characteristic concentration of cadmium shall
be less than 0.05 μg / mL;
- Precision. USE standard solution of the highest concentration to measure
absorbance for 10 times, its standard deviation shall not exceed 1.0% of the
average absorbance; USE standard solution of the lowest concentration (not
the standard solution of “zero” concentration) to measure absorbance for 10
times, its standard deviation shall not exceed 0.5% of the average absorbance
of standard solution of the highest concentration;
- Linearity of working curve. DIVIDE the working curve into five sections
equally, based on concentration; the ratio between the absorbance difference
of the highest section AND the absorbance difference of the lowest section shall
not be less than 0.8;
Reference operating conditions of the instruments are shown in Table 1.
Table 4
Mass factor of
cadmium / %
0.0002 0.0020 0.0050 0.50 1.00 1.50
R / % 0.0001 0.0005 0.0010 0.04 0.05 0.06
Note. Reproducibility (R) is 2.8SR; SR is the reproducibility standard deviation.
8 Quality assurance and control
Standard samples of national-level or industrial-level shall be used (when these
2 samples are not available, controlled standard sample may be used for
substitution); effectiveness of this analytical method shall be calibrated weekly
or biweekly. When the process is out of control, root cause shall be found out;
After the error is corrected, calibration shall be repeated.
References and Original Chinese Documents
[1] GB/T 4103.14-2009 Methods for chemical analysis of lead and lead alloys - Part
14. Determination of cadmium content - Flame atomic absorption
ID=GB/T%204103.14-2009