YS/T 746.4-2010Methods for chemical analysis of tin-based lead-free solders. Part 4: Determination of lead 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 this is Part 4.

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. Red CIQ.

Participated in the drafting of this section. High-tech Co., Ltd. Shenzhen Grammy, Kunming Institute Platinum Limited.

1 Scope

YS/T 746 This section provides lead-free tin-based solders Determination of lead content.

This section applies to the determination of non-Pb-based solder lead content. Measurement range. 0.0050% to 0.100%.

2 Method summary

Sample mixed acid decomposition in dilute acid medium mixed with hydrochloric acid - volatile hydrobromide remove tin, antimony, atomic absorption spectrometer wavelength 283.3nm at using air - acetylene flame measured absorbance.

When the test compound indium content of greater than 10%, or otherwise use deuterium lamp background deduction measure.

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 nitric acid (12).

3.4 hydrobromide (rho1.48g/mL).

3.5 hydrochloric acid - hydrobromide. hydrochloric acid (3.1) and bromate (3.4) mixed in equal volumes.

3.6 sulfate (11).

3.7 mixed acid. 300mL of hydrochloric acid (3.1) and 100mL nitric acid (3.2) and mixed.

3.8 lead standard stock solution. Weigh 0.5000g lead (>=99.999%), placed in 250mL beaker, add 20mL of nitric acid (3.3), Cover dish table, micro heat until completely dissolved, remove the cooled to room temperature. Washed with water table dish and cup wall and transferred to 500mL volumetric flask, dilute with water to the mark, and mix. 1mL solution containing 1mg lead.

3.9 Lead standard solution. Pipette 20.00mL lead standard stock solution (3.8) in 200mL flask, add 15mL of nitric acid (3.3), Dilute with water to volume, and mix. This solution 1mL containing 100µg lead.

4 Instrument

Atomic absorption spectrometer with background deduction means attached lead hollow cathode lamp.

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

--- Sensitivity. the substrate solution consistent with the measured solution, characteristic concentration of lead should not exceed 0.24µg/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.