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GB/T 23273.2-2009Methods for chemical analysis of cobalt oxalate - Part 2: Determination of lead content - Electrothermal atomic absorption spectrometry (English PDF)

草酸钴化学分析方法 第2部分:铅量的测定 电热原子吸收光谱法

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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 23273.2-2009 is the English-translated version of 草酸钴化学分析方法 第2部分:铅量的测定 电热原子吸收光谱法.

GB/T 23273.2-2009 is the Chinese standard "Methods for chemical analysis of cobalt oxalate - Part 2: Determination of lead content - Electrothermal atomic absorption spectrometry".

Its scope clause reads: GB/T 23273 provisions of this part of the determination of the amount of lead in cobalt oxalate. This section applies to the determination of lead content of cobalt oxalate.

Measurement range. 0.001% to 0.01%. Its clauses include method summary; reagents; instrument.

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Document preview — GB/T 23273.2-2009

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 lead in cobalt oxalate.

This section applies to the determination of lead content of cobalt oxalate. Measurement range. 0.001% to 0.01%.

2 Method summary

Sample decomposition with nitric acid, in dilute nitric acid medium, graphite furnace atomic absorption spectrometer at a wavelength of 283.3nm, Zeeman effect deduction back

King, measuring the absorption peak area, according to the standard curve matching cobalt matrix calculations lead content.

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

nitrate (rho1.42g/mL), pure class distinctions.

3.2

nitric acid (1 + 1).

Nitrate 3.3 (2 + 3).

3.4

nitric acid (1 + 99).

3.5 cobalt matrix solution

Weigh 16.50g metal cobalt (cobalt content >=99.98%, lead < 0.0005%) in 1000mL beaker

Was added 40mL of nitric acid (3.2), cover sheet pan, on low heat until completely dissolved, oxides of nitrogen purge boiling, remove the cooled to room temperature, washed with water

Flush table dish and cup wall, moved into 1000mL volumetric flask, constant volume of water. This solution 1mL containing 16.5mg cobalt.

3.6 lead standard stock solution

Weigh 0.2000g metallic lead (Pb mass fraction >=99.95%), placed in 150mL beaker, add

20mL of nitric acid (3.3), cover sheet pan, a hot plate set at low temperature, is heated until complete dissolution, boiling rid of nitrogen oxides, was cooled to room temperature,

Transferred to 200mL volumetric flask, add 20mL of nitric acid (3.2), constant volume of water. 1mL solution containing 1mg lead.

3.7

lead standard solution A. Pipette 10.00mL lead standard stock solution (3.6), in 1000mL flask, add 10mL of nitric acid (3.2), constant volume of water. This solution 1mL containing 10µg lead.

3.8 lead standard solution B

Pipette 10.00mL lead standard solution A, in 100mL flask, 10mL of nitric acid was added (3.2), water

Volume, 1mL solution containing 1µg lead.

4 Instrument

Atomic absorption spectrometer with graphite furnace atomizer with Zeeman effect background subtraction function, autosampler, with the female lead in hollow

Pole lamp.

Under optimum working conditions for those who can reach the following indicators can be used.

--- Sensitivity. basically the same test solution and measurement solution, characteristic mass of lead should be less than 50pg.

--- 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 0.70.

......
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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