YS/T 555.6-2009Methods for chemical analysis of molybdenum concentrate. Determination of copper, lead, bismuth and zinc content. Flame atomic absorption spectrometry (English PDF)
钼精矿化学分析方法铜、铅、铋、锌量的测定火焰原子吸收光谱法
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Issued by
Ministry of Industry and Information Technology of the People's Republic of China
Level / Type
National · Recommended
Issue date
December 4, 2009
Implementation date
June 1, 2010
Scope
YS/T 555.6-2009 is the English-translated version of 钼精矿化学分析方法铜、铅、铋、锌量的测定火焰原子吸收光谱法.
YS/T 555.6-2009 - This Part specifies the methods for determining the content of copper, lead, bismuth and zinc in molybdenum concentrate. This Part applies to the determination of copper, lead, bismuth, and zinc content in molybdenum concentrate.
The determination ranges for copper. 0.0050%~2.50%; lead. 0.010%~3.00%; bismuth. 0.0050%~2.50%; and zinc. 0.0050%~1.00%.
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Document preview — YS/T 555.6-2009
National Standard of the People's Republic of China
- ICS
- 77.120.99
- Classification
- H 14
Issued by: Ministry of Industry and Information Technology of the People's Republic of China
Contents
- Foreword...3
- 1 Scope...5
- 2 Method summary...5
- 3 Reagents...5
- 4 Instruments...6
- 5 Specimen...7
- 6 Analysis steps...7
- 7 Calculation of analysis results...8
- 8 Precision...9
- 9 Quality assurance and control...10
Foreword
YS/T 555 "Methods for chemical analysis of molybdenum concentrate" comprises 11
parts.
YS/T 555.1, Methods for chemical analysis of molybdenum concentrate.
Determination of molybdenum content. Lead molybdenum gravimetry;
YS/T 555.2, Methods for chemical analysis of molybdenum concentrate.
Determination of silicon dioxide content. Silicon molybdenum blue
spectrophotometry and gravimetry;
YS/T 555.3, Methods for chemical analysis of molybdenum concentrate.
Determination of arsenic content. Atomic fluorescence spectrometry;
YS/T 555.4, Methods for chemical analysis of molybdenum concentrate.
Determination of tin content. Atomic fluorescence spectrometry;
YS/T 555.5, Methods for chemical analysis of molybdenum concentrate.
Determination of phosphorus content. Phosphorus molybdenum blue
spectrophotometry;
YS/T 555.6, Methods for chemical analysis of molybdenum concentrate.
Determination of copper, lead, bismuth and zinc content. Flame atomic
absorption spectrometry;
YS/T 555.7, Methods for chemical analysis of molybdenum concentrate.
Determination of calcium oxide content. Flame atomic absorption spectrometry;
YS/T 555.8, Methods for chemical analysis of molybdenum concentrate.
Determination of tungsten content. Thiocyanate spectrophotometry;
YS/T 555.9, Methods for chemical analysis of molybdenum concentrate.
Determination of potassium and sodium content. Flame atomic absorption
spectrometry;
YS/T 555.10, Methods for chemical analysis of molybdenum concentrate.
Determination of potassium and sodium content;
YS/T 555.11, Methods for chemical analysis of molybdenum concentrate.
Determination of oil and moisture content. Gravimetry.
This is Part 6.
This Part replaces YS/T 555.6-2006 "Molybdenum concentrates. Determination of
copper and lead content" (formerly GB/T 15079.6-1994) and YS/T 555.9-2006
"Molybdenum concentrates. Determination of bismuth content" (formerly GB/T
15079.9-1994).
Compared with YS/T 555.6-2006 and YS/T 555.9-2006, the main changes in this Part
are as follows.
- The determination of zinc content has been added;
- The sample preparation method for bismuth content has been changed;
- The upper limit range for bismuth content determination has been expanded;
- The lower limit range for lead content determination has been expanded;
- The sample preparation and determination methods for copper, lead, bismuth, and
zinc have been standardized;
- The clauses on precision have been added.
This Part was proposed by and shall be under the jurisdiction of National Technical
Committee on Non-ferrous Metals of Standardization Administration of China.
Main drafting organizations of this Part. Jinduicheng Molybdenum Group Co., Ltd.,
and China Nonferrous Metals Industry Standards, Metrology and Quality Research
Institute.
The drafting organizations of this Part. Hunan Shizhuyuan Nonferrous Metals Co., Ltd.,
Luoyang Luanchuan Molybdenum Group Co., Ltd., and Jiangxi Copper Corporation
(Dexing) Mining New Technology Development Co., Ltd.
Main drafters of this Part. Tian Wenhui, Wang Guoliang, Wang Zhongqi, Zhang
Jiangfeng, Su Xiong, Lu Qingxiang.
Main verifiers of this Part. Zhou Yinhua, Wu Xia, Tian Yonghong, and Li Hongjun.
Versions of standard substituted by this Part are.
- GB/T 15079.6-1994, GB/T 15079.9-1994;
- YS/T 555.6-2006, YS/T 555.9-2006.
Methods for chemical analysis of molybdenum concentrate -
- Determination of copper, lead, bismuth and zinc content --
Flame atomic absorption spectrometry
1 Scope
This Part specifies the methods for determining the content of copper, lead, bismuth
and zinc in molybdenum concentrate.
This Part applies to the determination of copper, lead, bismuth, and zinc content in
molybdenum concentrate. The determination ranges for copper. 0.0050%~2.50%; lead.
0.010%~3.00%; bismuth. 0.0050%~2.50%; and zinc. 0.0050%~1.00%.
2 Method summary
The specimens are decomposed with hydrochloric acid and nitric acid. In a dilute
hydrochloric acid medium, the absorbance is measured using the air-acetylene flame
method at wavelengths of 324.7 nm for copper, 283.3 nm for lead, 223.1 nm for bismuth,
and 213.9 nm for zinc on an atomic absorption spectrometer.
3 Reagents
Unless otherwise specified, only reagents confirmed to be analytically pure and distilled
or deionized water or water of equivalent purity shall be used in the analysis.
3.1 Nitric acid (rho 1.42 g/mL), guaranteed reagent.
3.2 Hydrochloric acid (rho 1.19 g/mL), guaranteed reagent.
3.3 Nitric acid solution (1+1).
3.4 Hydrochloric acid solution (1+1).
3.5 Copper standard solution. weigh 0.1000 g of metallic copper (mass fraction
>=99.99%) into a 250 mL beaker. Slowly add 30 mL of nitric acid solution (3.3). Heat to
dissolve, then cool. Transfer to a 1000 mL volumetric flask. Dilute to the mark with
water and mix well. 1 mL of this solution contains 100 µg of copper.
3.6 Lead standard solution. weigh 0.1000 g of metallic lead (mass fraction >=99.99%)
into a 250 mL beaker. Add 30 mL of nitric acid solution (3.3). Heat to dissolve, then
cool. Transfer to a 1000 mL volumetric flask. Dilute to the mark with water. Mix well.
1 mL of this solution contains 100 µg of lead.
3.7 Bismuth standard solution. weigh 0.1000 g of metallic bismuth (mass fraction
>=99.99%) into a 250 mL beaker. Add 20 mL of nitric acid (3.1). Dissolve by heating at
low temperature, then cool. Transfer to a 1000 mL volumetric flask. Dilute to the mark
with water. Mix well. 1 mL of this solution contains 100 µg of bismuth.
3.8 Zinc standard stock solution. weigh 0.1000 g of metallic zinc (mass fraction
>=99.99%) into a 250 mL beaker. Add 30 mL of hydrochloric acid solution (3.4).
Dissolve by heating at low temperature, then cool. Transfer to a 1000 mL volumetric
flask. Dilute to the mark with water. Mix well. This solution contains 100 µg of zinc
per mL.
3.9 Zinc standard solution. transfer 50.00 mL of zinc standard stock solution (3.8) to a
500 mL volumetric flask. Add 15 mL of hydrochloric acid solution (3.4). Dilute to the
mark with water. Mix well. This solution contains 10 µg of zinc per mL.
4 Instruments
Atomic absorption spectrometer, equipped with copper, lead, bismuth, and zinc hollow
cathode lamps.
Under optimal operating conditions, any instrument that meets the following
specifications may be used.
- Minimum precision requirements. measure the absorbance of the highest standard
solution 10 times. The standard deviation should not exceed 1.0% of the average
absorbance. Measure the absorbance of the lowest standard solution (not the
"zero" standard solution) 10 times. The standard deviation should not exceed 0.5%
of the average absorbance of the highest standard solution;
- Characteristic concentrations. in a solution consistent with the matrix of the test
solution, the characteristic concentration of copper should not exceed 0.025
µg/mL; the characteristic concentration of lead should not exceed 0.16 µg/mL;
the characteristic concentration of bismuth should not exceed 0.14 µg/mL; and
the characteristic concentration of zinc should not exceed 0.05 µg/mL;
- Linearity of the working curve. divide the working curve into five equal segments
according to concentration. The ratio of the absorbance difference of the highest
segment to the absorbance difference of the lowest segment should not be less
than 0.7.
5 Specimen
The specimen should be pre-treated to remove oil and moisture. Its particle size should
be less than 0.090 mm. The specimen should be dried at 100°C~105°C for 1 h and then
cooled to room temperature in a desiccator.
6 Analysis steps
6.1 Test material
Weigh 0.2 g of the specimen, accurate to 0.0001 g. Perform two independent
determinations and take the average value.
6.2 Blank test
Conduct a blank test along with the test material.
6.3 Determination
6.3.1 Place the test material (6.1) in a 250 mL beaker. Wet with water. Add 15 mL of
hydrochloric acid (3.2) and 10 mL of nitric acid (3.1). Cover with a watch glass.
Dissolve by heating at low temperature. Evaporate to dryness. Cool. Add 8 mL of
hydrochloric acid solution (3.4) and 20 mL of water. Heat to dissolve the salts. After
cooling, transfer to a 100 mL volumetric flask. Dilute to the mark with water. Mix well.
Filter on dryness.
6.3.2 Transfer the solution (6.3.1) according to Table 1 and add hydrochloric acid
solution (3.4) to a 100 mL volumetric flask. Dilute to the mark with water. Mix well.
Table 1
6.3.3 Analyze the solution (6.3.2) using an atomic absorption spectrometer at
wavelengths of 324.7 nm for copper, 283.3 nm for lead, 223.1 nm for bismuth, and
213.9 nm for zinc, using an air-acetylene flame and zeroing with a "zero" standard
solution. The corresponding concentrations of copper, lead, bismuth, and zinc are then
determined from the working curve.
6.4 Drawing the working curve
6.4.1 Transfer 0 mL, 1.00 mL, 1.50 mL, 2.00 mL, 2.50 mL, 3.00 mL, and 4.00 mL of
copper standard solution (3.5), and 0 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00
mL, and 10.00 mL of lead standard solution (3.6), bismuth standard solution (3.7), and
zinc standard solution (3.9) into separate 100 mL volumetric flasks. Add 8 mL of
hydrochloric acid solution (3.4) to each flask. Dilute to the mark with water. Mix well.
6.4.2 Under the same conditions as the specimen determination, the absorbance of the
standard solution is measured. Working curves are plotted with the concentrations of
copper, lead, bismuth, and zinc on the x-axis and absorbance on the y-axis, respectively.
7 Calculation of analysis results
Calculate the mass fractions of copper, lead, bismuth, and zinc according to formula (1).
The values are expressed as a percentage (%).
Element for determination Mass fraction / % Volume of solution transferred / mL
Volume of added hydrochloric acid solution
(3.4) / mL
Copper
Lead
Zinc
Bismuth
Full amount
Full amount
Full amount
Full amount
Where,
rho1 - The concentration of copper, lead, bismuth, or zinc in the test solution obtained
from the working curve, in micrograms per milliliter (µg/mL);
rho2 - The concentration of copper, lead, bismuth, or zinc in the blank solution obtained
from the working curve, in micrograms per milliliter (µg/mL);
V0 - Total volume of the test solution, in milliliters (mL);
V1 - The volume of test solution transferred, in milliliters (mL);
V2 - The volume of test solution tested, in milliliters (mL);
m0 - The mass of test material, in grams (g).
The calculation result is expressed to two decimal places. When it is less than 0.10%,
it is expressed to three decimal places.
8 Precision
8.1 Repeatability
For two independent determination results obtained under repeatability conditions, the
absolute difference between the two determination results should not exceed the
repeatability limit (r) within the range of the average values given below, and the
occurrence of differences exceeding the repeatability limit (r) should not exceed 5%.
The repeatability limit (r) is obtained by linear interpolation using the following data.
Mass fraction of copper, lead, bismuth, and zinc / %. 0.020 0.10 2.0
Repeatability limit (r) / %. 0.003 0.010 0.10
NOTE. The repeatability limit (r) is 2.8Sr, where Sr is the repeatability standard deviation.
8.2 Allowable difference
The difference between laboratory analytical results should not exceed the allowable
difference listed in Table 2.
Table 2
Table 2 (continued)
9 Quality assurance and control
Use national or industry-level standard samples (or control standard samples if neither
is available). Verify the validity of this analytical method weekly or bi-weekly. If the
process goes out of control, identify the cause. Correct the error and re-verify.
Element Content / % Allowable difference / %
Element Content / % Allowable difference / %
Copper
Bismuth
Lead
Zinc
......
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.
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Related Standards
YS/T 555.1-2009 — Methods for chemical analysis of molybdenum concentrate. Determination of molybdenum content. Lead molybdenum gravimetry
YS/T 555.10-2009 — Methods for chemical analysis of molybdenum concentrate. Determination of rhenium content. Thiocyanate spectrophotometry
YS/T 555.11-2009 — Methods for chemical analysis of molybdenum concentrate. Determination of oil and moisture content. Gravimetry
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