Enrichment palladium of palladium catalysts by pyrometallurgy, then dissolve the palladium in admixture acid, the liquid is analyzed by AAS.
2.1 Hydrochloric acid(ρ1.19g/ml)
2.2 Nitric acid(ρ1.42g/ml)
2.3 Admixture acid (Hydrochloric acid and Nitric acid mixed,volume as 3:1)
2.4 Perchloric acid (AR)
2.5 Sodium Chloride solution (50g/L)
2.6 Standard solution of palladium:
Weigh 0.1g palladium(extract to 0.0001g), which is completely dissolved in 40mL admixture acid by low heat. Add 5mL sodium chloride solution into the former solution, evapor it to almost dry, then add 3mL hydrochloric acid, evapor it to almost dry, repeat the two steps three times. Add 10mL hydrochloric acid, switch into capacity bottle, dilute to scale, mix it uniformly, the content of palladium in the solution is 1.0mg/mL.
3.1 AAS, Flame, gas type: acetylene-air. The parameters are set according to the record of cookbook.
3.2 Common lab apparatus.
4. Sample disposal
Place 0.15g(exactly to 0.0001g) of sample disposed by pyrometallurgy in 100mL beaker, make two parallel samples. Add 15mL admixture acid, meantime add 5mL perchloric acid, disslove it by heat, evapor it to almost dry, add 5mL sodium chloride solution, then add 3mL hydrochloric acid, evapor it to almost dry, repeat the two steps three times. Add 10mL hydrochloric acid, switch into capacity bottle, dilute to scale, mix it uniformly, the content of palladium in the sample solution approxately is 1.5mg/mL, switch 10mL of the sample solution into 100mL capacity bottle, add 3mL hydrochloric acid, dilute to scale, the content of palladium in the sample solution approxately is 0.15mg/mL.
5. Determing content
5.1 Apply the composed standard solution into AAS and make the standard curve(standard solution 2,4,6,8,10ppm), determing absorbency of the sample, then calculate the concentration of the sample according to the stanadard curve.
Post time: Apr-30-2022