YS/T 555.3-2009Methods for chemical analysis of molybdenum concentrate. Determination of arsenic content. Atomic fluorescence spectrometry (English PDF)

Foreword

YS/T 555 "Methods for chemical analysis of molybdenum concentrate" includes 11 parts.

YS/T 555.1 Methods for chemical analysis of molybdenum concentrate molybdenum content of lead molybdate assay gravimetric method YS/T 555.2 Methods for chemical analysis of molybdenum concentrate - Determination of silicon dioxide content and weight of molybdenum blue spectrophotometric method YS/T 555.3 Methods for chemical analysis of molybdenum concentrate arsenic content - Atomic Fluorescence Spectrometry and DDTC-Ag spectrophotometry YS/T 555.4 Methods for chemical analysis of molybdenum concentrate tin content - Atomic Fluorescence Spectrometry YS/T 555.5 Methods for chemical analysis of molybdenum concentrate phosphorus content of molybdenum blue spectrophotometric determination of phosphorus YS/T 555.6 Methods for chemical analysis of molybdenum concentrate copper, lead, bismuth, zinc content - Flame Atomic Absorption Spectrometry YS/T 555.7 Methods for chemical analysis of molybdenum concentrate calcium oxide content by flame atomic absorption spectrometry YS/T 555.8 Methods for chemical analysis of molybdenum concentrate - Determination of tungsten content - Thiocyanate spectrophotometric method YS/T 555.9 Methods for chemical analysis of molybdenum concentrate the amount of potassium and sodium contents - Flame Atomic Absorption Spectrometry YS/T 555.10 Methods for chemical analysis of molybdenum concentrate rhenium contents - Thiocyanate spectrophotometric Determination of YS/T 555.11 Methods for chemical analysis of molybdenum concentrate oil and moisture content of the total weight of the law this is Part 3.

"The method concentrates - Determination of arsenic content" in this section instead of YS/T 555.3-2006 (formerly GB/T 15079.3-1994).

This portion of YS/T 555.3-2006 compared to the main changes are as follows.

--- Determination method increases the atomic fluorescence spectrometry;

--- Increasing the precision of the terms;

--- Text format has been modified, supplemented with quality assurance and control provisions.

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

This section is responsible for drafting unit. Jinduicheng Molybdenum Group Co., Ltd., China Nonferrous Metals Industry Institute of Standards and Metrology and Quality.

Participated in the drafting of this section. JCC (Dexing) New Mining Technology Development Co., Ltd., Hunan Nonferrous Metals limited liability Shizhuyuan any company.

1 Method, atomic fluorescence spectrometry

1 Scope

This method specifies the method for the determination of arsenic content in Molybdenum Concentrates.

This method is applicable to the determination of arsenic content in Molybdenum Concentrates. Measurement range. 0.00003% to 0.0010%.

2 Method summary

Sample decomposition by aqua regia, in acid medium, with thiourea - ascorbic acid pentavalent arsenic reduced to trivalent, and then potassium borohydride and trivalent Arsenic hydride generation, introduced into the hydride atomizer to hollow cathode lamp as the light source, the determination of arsenic in the atomic fluorescence spectrometer Fluorescence strength. In a certain range, and the amount of the fluorescent intensity is proportional to the measured elements. Iron salt was added to eliminate interference.

3 Reagents

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

3.1 sodium hydroxide.

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

3.3 aqua regia (excellent pure reagent preparation).

3.4 Sodium hydroxide solution (50g/L).

3.5 hydrochloric acid solution (1 + 1), excellent pure reagent preparation.

3.6 tartaric acid solution (80g/L).

3.7 Ferric chloride solution. Weigh 4.5gFeCl3 dissolved in 100mL of hydrochloric acid (3.2), and then added 200mL of water and mix.

3.8 thiourea - ascorbic acid mixture. Weigh 5g 5g ascorbic acid and thiourea was dissolved in 100mL of water, and mix. The time is now equipped with.

3.9 potassium borohydride solution. Weigh 10g of potassium borohydride dissolved in 500mL previously prepared sodium hydroxide solution (5g/L), and dissolved with Cotton filter. The time is now equipped with.

3.10 arsenic standard stock solution. Weigh 0.1320g spectroscopically pure arsenic trioxide dissolved in 10mL of sodium hydroxide solution (3.4) was added 5mL hydrochloric acid (3.5) and transferred to 1000mL volumetric flask, and then hydrochloric acid (1 + 9) diluted to the mark. This solution containing 1mL 100µg arsenic.

3.11 Arsenic standard solution. Pipette 5mL arsenic standard stock solution (3.10) in 500mL volumetric flask, dilute to the mark with hydrochloric acid (1 + 4), shake uniform. This solution 1mL containing 1µg of arsenic.

4 Instrument

Atomic fluorescence spectrometer (arsenic hollow cathode lamp).

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

--- Detection limit. not more than 1 × 10-9g/mL;

--- Precision. The fluorescence intensity was measured with a standard solution of arsenic 0.1µg/mL 10 times, and the standard deviation does not exceed the fluorescence intensity 0.5%;