GB/T 23273.3-2009Methods for chemical analysis of cobalt oxatate - Part 3: Determination of arsenic content - Hydride generation-atomic fluorescence spectrometry (English PDF)
草酸钴化学分析方法 第3部分:砷量的测定 氢化物发生-原子荧光光谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
January 5, 2009
Implementation date
November 1, 2009
Scope
GB/T 23273.3-2009 is the English-translated version of 草酸钴化学分析方法 第3部分:砷量的测定 氢化物发生-原子荧光光谱法.
GB/T 23273.3-2009 is the Chinese standard "Methods for chemical analysis of cobalt oxatate - Part 3: Determination of arsenic content - Hydride generation-atomic fluorescence spectrometry".
Its scope clause reads: GB/T 23273 provisions of this part of the determination of the amount of arsenic, cobalt oxalate. This section applies to the determination of arsenic content of cobalt oxalate.
Measurement range. 0.0001% to 0.004%. Its clauses include method summary; reagents; instrument.
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Document preview — GB/T 23273.3-2009
National Standard of the People's Republic of China
- ICS
- 77.120.70
- Classification
- H 13
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- 1 Scope
- 2 Method summary
- 3 Reagents
- 4 Instrument
1 Scope
GB/T 23273 provisions of this part of the determination of the amount of arsenic, cobalt oxalate.
This section applies to the determination of arsenic content of cobalt oxalate. Measurement range. 0.0001% to 0.004%.
2 Method summary
Sample decomposition with hydrochloric acid, hydrochloric acid medium with thiourea - ascorbic acid pre-reduction, arsenic hydride generator is potassium borohydride
Reduction of hydride with argon gas was introduced into the atomizer, the fluorescence intensity measured on the atomic fluorescence spectrometer, by matching cobalt matrix standard song
Line method to calculate the content of arsenic.
3 Reagents
Analysis of water are two of water or equivalent purity. After dilute nitric acid used in the experiment containers are treated with hot, clean water.
3.1
hydrochloride (rho1.19g/mL).
3.2
HCl (1 + 1).
Hydrochloride 3.3 (1 + 3).
Nitrate 3.4 (rho1.42g/mL).
3.5
nitric acid (1 + 1).
Thiourea 3.6 - ascorbic acid solution (100g/L). Weigh 10.0g of thiourea, was added 80mL of water was heated to about dissolved, cooled
10.0g ascorbic acid, dissolved diluted to 100mL, and mix using now.
3.7 solution of potassium borohydride (20g/L)
Weigh 2.0g of potassium borohydride is added 100mL sodium hydroxide solution (5g/L) were dissolved, and mix. use
When existing service.
3.8 cobalt matrix solution (cobalt-containing 16g/L)
Weigh 1.6000g metal cobalt (cobalt content >=99.98%, wherein the mass fraction of arsenic
< 0.0001%), was added 20mL of nitric acid (3.5) were dissolved, coolish, was added 10mL of hydrochloric acid (3.1) was dissolved to a small volume, and cooled to remove
At room temperature and transferred to 100mL volumetric flask, constant volume of water.
3.9 arsenic standard stock solution
Weigh 0.1320g trioxide (arsenic trioxide mass fraction >=99.9%, sulfuric acid in a dry beforehand
Is dried to constant weight) in 150mL beaker, 5mL sodium hydroxide solution (200g/L), cover the dish table, low dissolved, add 5mL
Water, 2 drops of phenolphthalein ethanol solution (1g/L), washed with hydrochloric acid (3.2) to the red and then disappear just excess 2mL, moved 1000mL volumetric flask
The constant volume of water. This solution 1mL containing 100µg arsenic.
3.10 arsenic standard solution
Pipette 10.00mL arsenic standard stock solution (3.9) in 1000mL volumetric flask, was added 20mL of hydrochloric acid (3.2), constant volume of water. This solution 1mL containing 1µg of arsenic.
3.11
argon (Ar>=99.99%).
4 Instrument
Atomic fluorescence spectrometer, with a high-intensity arsenic hollow cathode lamp.
Under optimum working conditions for those who reach the following indicators can be used.
--- Detection limit. less than 0.5ng/mL.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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Related Standards
GB/T 23273.1-2009 — Methods for chemical analysis of cobalt oxalate - Part 1: Determination of cobalt content - Potentiometric titration method
GB/T 23273.2-2009 — Methods for chemical analysis of cobalt oxalate - Part 2: Determination of lead content - Electrothermal atomic absorption spectrometry
GB/T 23273.4-2009 — Methods for chemical analysis of cobalt oxalate - Part 4: Determination of silicon content - Molybdenum blue spectrophotometry
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