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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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