YS/T 226.11-2009Methods for chemical analysis of selenium. Part 11: Determination of lead content. Flame atomic absorption spectrometry (English PDF)

Foreword

YS/T 226 "selenium chemical analysis method" is divided into 13 parts.

--- Part 1. Determination of bismuth content - Hydride Generation - Atomic Fluorescence Spectrometry

--- Part 2. Determination of antimony content Hydride Generation - Atomic Fluorescence Spectrometry

--- Part 3. Determination of aluminum content Chromazurol S- cetylpyridinium bromide spectrophotometric method

--- Part 4. Determination of mercury content of dithizone - CTC colorimetric titration

--- Part 5. Determination of the amount of silicon molybdenum blue spectrophotometry

--- Part 6. Determination of sulfur content symmetrical diphenyl semicarbazide spectrophotometry

--- Part 7. Determination of magnesium content - Flame atomic absorption spectrometry

--- Part 8. Determination of copper content - Flame atomic absorption spectrometry

--- Part 9. Determination of iron content by flame atomic absorption spectrometry

--- Part 10. Determination of nickel content by flame atomic absorption spectrometry

--- Part 11. Determination of lead content by flame atomic absorption spectrometry

--- Part 12. Determination of the amount of selenium sodium thiosulfate volumetric method

--- Part 13. silver, aluminum, arsenic, boron, mercury, bismuth, copper, cadmium, iron, gallium, indium, magnesium, nickel, lead, silicon, antimony, tin, tellurium, titanium, zinc contents Inductively Coupled Plasma Mass Spectrometry this section YS/T Part 11 226.

The partial replacement of YS/T 226.12-1994 "selenium determination of lead content oscillopolarographic law." Compared with YS/T 226.12-1994, this section has the following main changes.

--- Analysis by the oscillopolarographic law was changed to flame atomic absorption spectrometry;

--- Supplementary terms of quality assurance and control;

--- Increased repeatability, reproducibility will be changed to allow the poor.

The non-ferrous metal part by the National Standardization Technical Committee and centralized.

This section is responsible for drafting unit. Jinchuan Group Limited.

Participated in the drafting of this section. Beijing Nonferrous Metal Research Institute, Guangzhou Nonferrous Metal Research Institute.

1 Scope

This section YS/T 226 specifies the method for determination of selenium in lead content.

This section applies to the determination of selenium in lead content. Measurement range. 0.0002% to 0.04%.

2 Method summary

Sample decomposition with nitric acid at 320 °C volatile selenium was removed in dilute hydrochloric acid medium, with air - acetylene flame atomic absorption spectrometer wave Long 217.0nm at measuring the absorbance, the standard curve method to calculate the amount of lead.

3 Reagents

Unless otherwise indicated, the second part of the water are distilled water, reagents were pure class distinctions.

Nitrate 3.1 (rho1.42g/mL).

3.2 nitric acid (1 + 1).

3.3 hydrochloric acid (1 + 2).

3.4 lead standard stock solution. Weigh 1.0000g of lead (Pb mass fraction >=99.5%) placed in 500mL beaker, add 20mL nitrate Acid (3.2) is completely dissolved, boil expelled nitrogen oxides. Remove, cool to room temperature and transferred to 1000mL volumetric flask, constant volume of water. This solution 1mL containing 1mg lead.

3.5 Lead standard solution. Pipette 25.00mL lead standard stock solution (3.4) in 1000mL volumetric flask, add 50mL of hydrochloric acid (3.3) Constant volume of water. This solution 1mL containing 25µg lead.

4 Instrument

4.1 Atomic absorption spectrometer, with a lead hollow cathode lamp.

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

--- Characteristic concentration. the test solution is consistent with the measurement of the solution, the characteristic concentration of lead should not exceed 0.09µg/mL;

--- Precision. with the highest concentration of the standard solution absorbance measurements 10 times the standard deviation should not exceed 1.0% of their mean absorbance;

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 0.80.

Atomic absorption spectrometer operating conditions refer to Table 1.

Table 1 instrument conditions

Wavelength/nm lamp current/mA monochromator passband/nm observation height/mm flame type 217.0 7 0.5 7 stoichiometric flame

4.2 Selenium volatile furnace (see Figure 1).