GB/T 4103.17-2018Method for chemical analysis of lead and lead alloys—Part 17: Determination of sodium, magnesium contents—Flame atomic absorption spectrometry (English PDF)

Foreword

GB/T 4103 "Chemical Analysis Methods for Lead and Lead Alloys" has 17 parts.

--- Part 1. Determination of the amount of tin;

--- Part 2. Determination of sputum;

--- Part 3. Determination of copper content;

--- Part 4. Determination of iron content;

--- Part 5. Determination of the amount of sputum;

--- Part 6. Determination of the amount of arsenic;

---Part 7. Determination of the amount of selenium;

--- Part 8. Determination of the amount of sputum;

---Part 9. Determination of calcium content;

--- Part 10. Determination of the amount of silver;

--- Part 11. Determination of the amount of zinc;

--- Part 12. Determination of enthalpy;

--- Part 13. Determination of the amount of aluminum;

---Part 14. Determination of cadmium content by flame atomic absorption spectrometry;

---Part 15. Determination of nickel content by flame atomic absorption spectrometry;

---Part 16. Determination of copper, silver, antimony, arsenic, antimony, tin and zinc

---Part 17. Determination of sodium content and magnesium content by flame atomic absorption spectrometry.

This part is the 17th part of GB/T 4103.

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

1 Scope

This part of GB/T 4103 specifies the method for determining the amount of sodium and magnesium in lead and lead alloys.

This part is applicable to the amount of sodium and magnesium in the anode alloy plate for electrolytic deposition, hard lead-bismuth alloy, special hard lead-bismuth alloy, and lead alloy ingot for cable sheathing.

Determination. The amount of sodium is determined to be in the range of 0.0005% to 0.0050%. The amount of magnesium measured ranges from 0.0005% to 0.050%.

2 Method summary

The sample was dissolved with nitric acid and tartaric acid. In a dilute nitric acid medium, using strontium salt as a releasing agent, using an air-acetylene flame, respectively, in the atomic absorption The absorbance of sodium and magnesium was measured at a wavelength of 589.0 nm and 285.2 nm of the spectrometer, and the amount of sodium and magnesium were calculated by a working curve method.

3 Reagents

Unless otherwise stated, the reagents used in this section are excellent grade pure reagents, preparation solutions and analytical waters that meet national or industrial standards.

All are first grade water. The vessels used in the experiment were all soaked in dilute nitric acid (1+4) and cleaned.

3.1 Tartaric acid.

3.2 Barium nitrate.

3.3 Nitric acid (rho=1.40g/mL), MOS reagent.

3.4 Nitric acid (1+2).

3.5 Nitric acid (1+3).

3.6 Tartaric acid solution (200g/L).

3.7 Barium nitrate solution (100g/L).

3.8 Sodium standard storage solution. Weigh 0.2305g of sodium carbonate reference material previously baked at 120 ° C for 1 h in 250 mL of PTFE Add 15 mL of nitric acid (3.4) to the cup. After the solution is completely dissolved, transfer it to a 1000 mL Teflon volumetric flask and dilute to volume with water. This solution 1 mL contains 100 µg of sodium.

3.9 Magnesium standard storage solution. Weigh 0.1000g of magnesium metal (wMg>=99.99%) in a 250mL Teflon beaker and add 10mL nitric acid (3.4), heated to complete dissolution, boiled to remove nitrogen oxides, removed, cooled, transferred to 1000mL of PTFE capacity Dilute to the mark with water and mix well. 1 mL of this solution contained 100 µg of magnesium.

3.10 Sodium standard solution. Pipette 10.00 mL of sodium standard storage solution (3.8) into a 100 mL Teflon volumetric flask and dilute with water until Scale and mix. 1 mL of this solution contained 10 µg of sodium.

3.11 Magnesium standard solution. Pipette 10.00mL of magnesium standard storage solution (3.9) into a 100mL Teflon volumetric flask and dilute with water until Scale and mix. 1 mL of this solution contained 10 µg of magnesium.

4 Instruments

Atomic absorption spectrometer with sodium and magnesium hollow cathode lamps.