GB/T 16484.11-2009Chemical analysis methods of rare earth chloride and light rare earth carbonate - Part 11: Determination of lead oxide content - Flame atomic absorption spectrometry (English PDF)

Foreword

GB/T 16484-2009 "rare earth chloride and light rare earth carbonate chemical analysis method" is divided into 22 parts.

--- Part 1. Determination of cerium oxide content of ammonium ferrous sulfate titration;

--- Part 2. europium oxide content - Inductively Coupled Plasma Mass Spectrometry;

--- Part 3. 15 with a rare earth element oxide component measured by inductively coupled plasma atomic emission spectrometry;

--- Part 4. Determination of thorium oxide content arsenazo III spectrophotometry;

--- Part 5. Determination of barium oxide by inductively coupled plasma atomic emission spectrometry;

--- Part 6. Determination of calcium oxide content by flame atomic absorption spectrometry;

--- Part 7. Determination of magnesium oxide content - Flame atomic absorption spectrometry;

--- Part 8. Determination of the amount of sodium oxide flame atomic absorption spectrometry;

--- Part 9. Determination of the amount of nickel oxide by flame atomic absorption spectrometry;

--- Part 10. Determination of manganese oxide content by flame atomic absorption spectrometry;

--- Part 11. Determination of lead oxide content by flame atomic absorption spectrometry;

--- Part 12. Determination of the amount of sulfate;

--- Part 13. Determination of the amount of ammonium chloride distillation - titration;

1 Scope

GB/T 16484.11-2009 is the Chinese national standard on chemical analysis methods of rare earth chloride and light rare earth carbonate - part 11: determination of lead oxide content - flame atomic absorption spectrometry, in the field of metallurgy. The /T suffix marks it as a recommended standard: it is not compulsory by itself, but it becomes binding as soon as a contract, a tender or a customer specification calls it up - which in practice is how most foreign buyers meet it. It was issued on 30 October 2009 by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of China, and has been in force since 1 May 2010. Classification: ICS 77.120.99, CCS H14. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

GB/T 16484 provisions of this part of the determination of rare earth chloride, carbonate, light rare earth oxide of lead content. This section applies to earth chloride and light rare earth carbonate was measured in lead oxide content. Measurement range. 0.0050% to 0.020%.

2 Principle of the method

The sample was dissolved by nitric acid in the air - acetylene flame, using high-performance hollow cathode lamp, atomic absorption spectrometer, wavelength 217.0nm Department deducting matrix background absorbance measurement lead with deuterium lamp.

3 Reagents and materials

3.1 Hydrogen peroxide (30%).

3.2 nitric acid (1 + 1).

3.3 lead standard stock solution. Weigh 0.5000g metallic lead [w1 (Pb) > 99.99%], placed in 200mL beaker, add 20mL of nitric acid (3.2), was slowly heated up to complete dissolution, boiled for several minutes in order to get rid of nitrogen oxides. Cooling to room temperature, transferred to 500mL volumetric flask Dilute with water to volume, and mix. 1mL solution containing 1mg lead.

3.4 Lead standard solution. Pipette 10.00mL lead standard stock solution (3.3), in 200mL flask, add 20mL of nitric acid (3.2), with Dilute with water to volume, and mix. This solution 1mL containing 50µg lead.

4 Instrument

Atomic absorption spectrometer, with a lead hollow cathode lamp. Under optimum conditions the instrument, those who can reach the following indicators can be used.

--- Characteristic concentration. in the measurement sample solution matrix consistent solution, characterized in lead concentration of not more than 0.0095µg/mL.

--- Precision. measuring the absorbance of the standard solution 10 times the highest concentration, the absorbance of the standard deviation does not exceed an average of 1.0%; most Low concentrations of the standard solution (not a zero standard solution) absorbance measured 10 times, and the standard deviation should not exceed the maximum average absorption solution 0.5% luminosity.

--- 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.

5 Sample

5.1 Preparation of rare earth chloride sample. A sample was crushed, quickly placed in a weighing bottle immediately weighed.

5.2 Preparation of light rare earth carbonate sample. weigh the sample immediately after the opening. Step

6 Analysis

6.1 Sample Table 1 sample was weighed, accurate to 0.0001g.