YS/T 226.8-2009Methods for chemical analysis of selenium. Part 8: Determination of copper 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 Section 8 226.

The partial replacement of YS/T 226.11-1994 "magnesium, copper, iron, nickel content - Flame atomic absorption spectrometric method" determination of the copper content.

Compared with YS/T 226.11-1994, this section has the following main changes.

--- Measured by the scope of 0.0002 percent to 0.02 percent to 0.0002 to 0.01%;

--- Supplementary terms of quality assurance and control;

--- Increase the repeatability limit, will be allowed to poor reproducibility limit.

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 copper content of selenium.

This section applies to the determination of copper content of selenium. Measurement range. 0.0002% to 0.01%.

2 Method summary

Sample decomposition with nitric acid at 320 °C volatile removing selenium, 3% hydrochloric acid medium, with air - acetylene flame, respectively, at a wavelength of 324.7nm Absorbance was measured at copper, calculated according to the amount of copper working curve method.

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 hydrochloride (rho1.19g/mL).

3.3 hydrochloric acid (1 + 2).

3.4 copper standard stock solution. Weigh 1.0000g copper (mass fraction of copper >=99.95%), placed in 250mL beaker, add 20mL nitrate Acid (1 + 1), heated until completely dissolved, remove cooling, hydrochloric acid was added 10mL (3.2) and transferred to 1000mL volumetric flask, dilute to the mark with water Degree, shake. 1mL solution containing 1mg of copper.

3.5 Copper standard solution. Pipette 20.00mL copper standard stock solution (3.4), placed 1000mL volumetric flask, dilute to the mark, Shake well. This solution 1mL containing 20µg copper.

4 Instrument

4.1 Atomic absorption spectrometer, with copper 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 copper is not greater than 0.05µg/mL.

--- 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 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 0.85.

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 324.7 5 0.5 7 stoichiometric flame

4.2 Selenium volatile furnace (see Figure 1).