YS/T 746.6-2010Methods for chemical analysis of lead-free tin-based solders. Part 6: Determination of antimony content. Flame atomic absorption spectrometric method (English PDF)

Foreword

YS/T 746 "non-Pb-based solder chemical analysis method" is divided into 17 parts.

--- Part 1 Determination of tin content Coke sexual gallic acid Covering - lead nitrate titration method

--- Part 2 of silver content - Flame atomic absorption spectrometry and potentiometric titration with potassium thiocyanate

--- Part 3 of copper content - Flame atomic absorption spectrometry and titration with sodium thiosulfate

--- Part 4 of lead content - Flame Atomic Absorption Spectrometry

--- Part 5 of bismuth content - Flame atomic absorption spectrometry and titration Na2EDTA

--- Part 6 of antimony content - Flame Atomic Absorption Spectrometry

--- Part 7 Determination of iron content by flame atomic absorption spectrometry

--- Part 8 of arsenic content of arsenic, antimony molybdenum blue spectrophotometric method

--- Part 9 Determination of zinc content by flame atomic absorption spectrometry and titration Na2EDTA Part 10 Determination of aluminum content --- first electrothermal atomic absorption spectrometry

--- Part 11 of cadmium content - Flame Atomic Absorption Spectrometry

--- Part 12 Determination of indium titration Na2EDTA

--- Part 13 Determination of nickel content by flame atomic absorption spectrometry

--- Part 14 Determination of the phosphorus content of the first crystal violet - heteropoly acid phosphovanadomolybdate spectrophotometry

--- Part 15 Determination of germanium content salicylfluorone spectrophotometry

--- Part 16 Determination of rare earth Arsenazo III spectrophotometry

--- Part 17 silver, copper, lead, bismuth, antimony, iron, arsenic, zinc, aluminum, cadmium, nickel, indium content was measured by inductively coupled plasma optical emission Spectroscopy Part is divided into 6 sections.

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

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

This section is drafted. Guangxi China Tin Group Co., Ltd.

This section participating units. Yunnan Tin Group Co., Ltd., Red River Exit Inspection and Quarantine.

1 Scope

YS/T 746 This section specifies the determination method without Tin Solder by antimony content.

This section applies to the determination of tin-based solder no antimony content. Measurement range. 0.0150% - 5.50%.

2 Method summary

Sample was dissolved with a mixed acid sample, in a mixed acid medium, atomic absorption spectrometer at a wavelength of 217.6nm with flame atomizer, Air - acetylene flame was measured antimony absorbance.

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 hydrochloride (rho1.19g/mL).

Nitrate 3.2 (rho1.42g/mL).

3.3 mixed acid. 30mL nitric acid, 70mL of hydrochloric acid and 100mL of water.

3.4 thiourea solution (50g/L).

3.5 Antimony standard stock solution. Take 0.5986g dried 2h antimony trioxide (99.99%) at 105 °C that burn into 250mL Cup, was added 50mL of hydrochloric acid (3.1), dissolved completely transferred to 500mL volumetric flask, was added 50mL of hydrochloric acid (3.1), diluted with water to Volume, and mix. This solution 1mL 1mg containing antimony.

3.6 Antimony standard solution. Pipette 50.00mL antimony standard stock solution in 500mL flask, add 50mL of hydrochloric acid (3.1), dilute with water Diluted to volume, and mix. This solution 1mL containing 100µg antimony.

4 Instrument

Atomic absorption spectrometer, with antimony hollow cathode lamp.

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

--- Characteristic concentration. a solution in the measurement matrix consistent solution, the concentration of antimony features should not exceed 0.14µg/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%;

With the lowest concentration of standard solution (not "zero" concentration of the standard) measuring the absorbance of 10 times, the standard deviation should not exceed the maximum 0.5% concentration of the standard average absorbance;

--- 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 0.7.