YS/T 226.10-2009Methods for chemical analysis of selenium. Part 10: Determination of nickel 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 10 226.

Measuring the amount of nickel present partial replacement of YS/T 226.11-1994 "selenium magnesium, copper, iron, nickel content - Flame Atomic Absorption Spectrometry" in Given portion. Compared with YS/T 226.11-1994, this section has the following main changes.

--- Measured by the scope of 0.0005% to 0.004 percent to 0.0002% to 0.01%;

--- 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 nickel content.

This section applies to the determination of selenium in nickel content. 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 232.0nm Absorbance was measured at a nickel, calculated according to the amount of nickel 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 Nickel standard stock solution. Weigh 1.0000g of nickel (Ni mass fraction >=99.95%), placed in 250mL beaker, add 20mL of nitric acid (1 + 1), heated until completely dissolved, remove cooling, hydrochloric acid was added 10mL (3.2) and transferred to 1000mL volumetric flask, washed with water Dilute to the mark. 1mL solution containing 1mg nickel.

3.5 Nickel standard solution. Pipette 25.00mL Nickel standard stock solution (3.4), placed 1000mL volumetric flask, dilute to the mark, Shake well. This solution 1mL containing 25µg nickel.

4 Instrument

4.1 Atomic absorption spectrometer, with a nickel 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 nickel is not more than 0.1µg/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 232.0 7 0.1 7 stoichiometric flame

4.2 Selenium volatile furnace (see Figure 1).