YS/T 74.1-2010Methods for chemical analysis of cadmium. Part 1: Determination of arsenic content-Hydride generation-atomic fluorescence spectrometry (English PDF)

Foreword

YS/T 74-2010 "cadmium chemical analysis method" is divided into 11 parts.

--- Part 1. Determination of arsenic content by hydride generation - atomic fluorescence spectrometry;

--- Part 2. Determination of antimony content hydride generation - atomic fluorescence spectrometry;

--- Part 3. Determination of nickel content by electrothermal atomic absorption spectrometry;

--- Part 4. Determination of lead content by flame atomic absorption spectrometry;

--- Part 5. Determination of the amount of copper diethyl dithiocarbamate spectrophotometry lead;

--- Part 6. Determination of zinc content - Flame atomic absorption spectrometry;

--- Part 7. Determination of iron content of 1,10 phenanthroline spectrophotometry;

--- Part 8. Determination of thallium content of crystal violet spectrophotometry;

--- Part 9. Determination of tin content by hydride generation - atomic fluorescence spectrometry;

--- Part 10. Determination of the amount of silver by flame atomic absorption spectrometry;

--- Part 11. Inductively coupled plasma atomic arsenic, antimony, nickel, lead, copper, zinc, iron, thallium, tin and silver content of the emitted light Spectroscopy.

This is Part 1.

This section drafted in accordance with GB/T 1.1-2009 given rules.

"Spectrophotometric determination of cadmium molybdenum blue spectrophotometric method for chemical analysis of arsenic amount" in this section instead of YS/T 74.1-1994, this part of the original criteria Ratio, the main changes are as follows.

--- Analytical methods to hydride generation - atomic fluorescence spectrometry;

--- The detection limit of 0.0005% decurrent 0.00020%;

--- Increase the warning prompt;

--- Increasing the test report clause.

The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.

This section is responsible for drafting unit. MCC Huludao Nonferrous Metals Group Co., Ltd.

Participated in the drafting of this section. Beijing Mining Research Institute, Shaanxi Dongling Smelting Co., Ltd., Liaoning Entry Inspection and Quarantine Bureau.

1 Scope

YS/T of the provisions of section 74 of the method for the determination of arsenic content in cadmium.

This section applies to the determination of arsenic content in cadmium. Measurement range. 0.00020% to 0.0025%.

2 Principle of the method

Sample was dissolved in nitric acid, thiourea - Ascorbic Acid prereduced arsenic, while masking copper, iron and other impurity elements, and hydride generator, arsenic it is reduced to potassium borohydride as hydride with argon gas into the quartz furnace atomizer, the fluorescence intensity measured on the atomic fluorescence spectrometer.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled water or equivalent purity.

3.1 potassium borohydride.

3.2 hydrochloric acid (rho1.19g/mL), pure class distinctions.

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

3.4 hydrochloride (11).

3.5 hydrochloride (19).

3.6 nitric acid (11).

3.7 thiourea - ascorbic acid solution. Weigh thiourea, each 25g ascorbic acid dissolved in 500mL of water, the time is now equipped with.

3.8 potassium borohydride solution. Weigh 10g potassium borohydride (3.1) was dissolved in 500mL of potassium hydroxide solution (0.5g/L), filtered spare, with when existing service.

3.9 arsenic standard stock solution. Weigh 0.1320g trioxide (wAs2O3>=99.9%, has been pre-dried in a drier 24h) to 300mL beaker, was added 20mL of sodium hydroxide (10g/L), completely dissolved by heating, addition of hydrochloric acid (3.4) and to slightly cooled, shift Into 1000mL volumetric flask, dilute with water to volume, and mix. This solution 1mL containing 0.1mg arsenic.

Warning. As2O3 toxic, use caution.

3.10 arsenic standard solution. Pipette 2.00mL arsenic standard stock solution (3.9) in 500mL volumetric flask, was added 75mL of hydrochloric acid (3.2), Dilute with water to volume, and mix. This solution 1mL containing 0.4µg arsenic.

4 Instrument

Atomic fluorescence spectrometer, with a high-intensity arsenic hollow cathode lamp. Shielding gas and a carrier gas of argon (>=99.99%).

Under optimum working conditions, who can achieve the following indicators atomic fluorescence spectrometer can be used.