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GB/T 3253.3-2008Methods for chemical analysis of antimony and antimony trioxide - Determination of lead content - Flame atomic absorption spectrometric method (English PDF)

锑及三氧化二锑化学分析方法 铅量的测定 火焰原子吸收光谱法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

March 31, 2008

Implementation date

September 1, 2008

Scope

GB/T 3253.3-2008 is the English-translated version of 锑及三氧化二锑化学分析方法 铅量的测定 火焰原子吸收光谱法.

GB/T 3253.3-2008 specifies the determination of lead in antimony and antimony trioxide by flame atomic absorption spectrometry. Clause 1 states that it applies to lead determination in both materials over a measuring range of 0.0020% to 0.75%.

The method summary in clause 2 describes dissolving the sample in nitric acid or in hydrochloric and hydrobromic acid, evaporating to dryness and repeating the hydrobromic acid addition to volatilise the antimony away, then measuring the absorbance of lead at 283.3 nm in a dilute hydrochloric acid medium with an air-acetylene flame, antimony trioxide and the other impurities not interfering.

Clause 3 lists the reagents, among them hydrochloric, nitric and hydrobromic acids with their densities, a 1 mg/mL lead stock solution prepared from lead of at least 99.99% purity and a 100 µg/mL lead working solution.

Clause 4 covers the instrument, an atomic absorption spectrometer fitted with a lead hollow-cathode lamp, and fixes the indices it must meet: a lead characteristic concentration no higher than 0.20 µg/mL in a matrix-matched solution, limits on the standard deviation of ten absorbance readings taken at the highest and at the lowest standard concentration, and a linearity criterion requiring the absorbance span of the highest of five concentration segments of the curve to be at least 0.8 of that of the lowest, with 283.3 nm given among the reference operating conditions.

The foreword records GB/T 3253 as an eleven-part set of chemical analysis methods for antimony and antimony trioxide, of which this is part 3, and lists what changed in this edition: dithizone spectrophotometry was dropped and atomic absorption spectrometry retained, the detection limit was extended from 0.010% to 0.0020%, and provisions on precision and on quality assurance and control were added.

It was proposed by the China Nonferrous Metals Industry Association, with drafting led by a tin and antimony mining company together with the Standards, Metrology and Quality Institute of the China Nonferrous Metals Industry, and carries ICS 77.120.99 and Chinese classification H13.

It replaces GB/T 3253.3-2001 and GB/T 3254.3-1998, was issued on 31 March 2008 and has applied since 1 September 2008.

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Document preview — GB/T 3253.3-2008

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 13
Replacing
GB/T 3254.3-1998

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword
  • 1 Scope
  • 2 Method summary
  • 3 Reagents
  • 4 Instrument

Foreword

GB/T 3253 "Methods for chemical analysis of antimony and antimony trioxide," a total of 11 parts.

--- GB/T 3253.1 chemical analysis of antimony trioxide and arsenic content of molybdenum blue spectrophotometric determination of arsenic --- GB /antimony trioxide and chemical analysis of iron content measured T 3253.2 phenanthroline spectrophotometry --- GB/T 3253.3 antimony trioxide and chemical analysis of lead content - Flame Atomic Absorption Spectrometry --- Determination of GB/T 3253.4 antimony trioxide and sulfur content of chemical analysis methods --- GB/T 3253.5 antimony trioxide and chemical analysis of copper content - Flame Atomic Absorption Spectrometry --- GB/T 3253.6 and antimony trioxide of selenium content - Atomic Fluorescence Spectrometry --- GB T 3253.7 antimony trioxide and chemical analysis methods Determination of bismuth content / --- Determination of GB/T 3253.8 antimony trioxide and antimony trioxide amount of chemical analysis methods --- Determination of GB/T 3253.9 antimony trioxide and chemical analysis of cadmium content --- Determination of GB/T 3253.10 antimony trioxide and chemical analysis of mercury content Determination --- GB/T 3253.11 antimony trioxide and analysis of lead, copper, bismuth, cadmium, iron, selenium, chromium, arsenic, mercury, tin content This is Part 3:

This Part replaces GB/T 3253.3-2001 "Methods for chemical analysis of lead, antimony, copper content determination" (lead part), GB/T 3254.3-1998 "Methods for chemical analysis of antimony trioxide determination of lead content." Compared with GB/T 3253.3-2001, GB/T 3254.3-1998, This section has the following changes.

--- Canceled dithizone spectrophotometry, atomic absorption spectrometry retention;

--- Detection limit extends from 0.010% to 0.0020%;

--- Complements the precision and quality assurance and control provisions.

1 Scope

This section provides the determination of antimony and antimony trioxide in lead content.

This section applies to the determination of lead content of antimony and antimony trioxide in. Measurement range. 0.0020% to 0.75%.

2 Method summary

Sample with nitric acid or hydrochloric acid and hydrobromic acid dissolved and evaporated to dryness, repeat adding hydrobromide volatile except antimony. In dilute hydrochloric acid medium, using air - B Alkyne flame atomic absorption spectrometer wavelength 283.3nm measured absorbance of lead, antimony trioxide and other impurities do not interfere Determination.

3 Reagents

3.1 Commercially available reagents

3.1.1 Hydrochloric acid (rho 1.19 g/mL)
3.1.2 Nitrate (rho 1.42 g/mL)
3.1.3 Hydrobromic acid (rho 1.50 g/mL)

3.2 Solution

3.2.1 hydrochloric acid (1 + 1)
3.2.2 nitric acid (1 + 1)

3.3 Standard solution

3.3.1 Lead standard stock solution

Weigh 1.0000g lead (>= 99.99%) in 200mL beaker, add 20mL of nitric acid (3.2.2), micro heat to dissolve completely get rid of boiling Oxides of nitrogen, cooled to room temperature. Moved into 1000mL volumetric flask, dilute with water to volume, and mix. 1mL solution containing 1mg lead.

3.3.2 Lead standard solution

Pipette 10.00mL lead standard stock solution (3.3.1) in 100mL flask, add 5mL hydrochloric acid (3.2.1), diluted with water to Volume, and mix. This solution 1mL containing 100µg lead.

4 Instrument

Atomic absorption spectrometer, with a lead 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, characterized in lead concentration should not exceed 0.20µg/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 0.8.

Atomic absorption spectrometer reference operating conditions.

--- Wavelength 283.3nm;

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

Referenced standards

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Editions of GB/T 3253.3

EditionTitleRevisionStatus
GB/T 3253.3-2008Methods for chemical analysis of antimony and antimony trioxide - Determination of lead content - Flame atomic absorption spectrometric methodcurrent editionCurrent
GB/T 3254.3-1998Methods for chemical analysis of antimony and antimony trioxide - Determination of lead content - Flame atomic absorption spectrometric methodprevious editionSuperseded

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