AS ISO 19976.1:2020 pdf free.Copper, lead and zinc sulfide concentrates – Determination of cadmium Part 1: Flame atomic absorption spectrometric method.
4 Principle
Dissolve the test portion in hydrochloric acid arid nitric acid. Add hydrofluoric acid to remove silicon. Then add perchloric acid and determine the iron concentration in the test portion using an atomic absorption spectrometer (AAS) with a deuterium lamp for background correction at 228,8 nm.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and distilled water or water of equivalent purity.
5.1 Hydrochloric acid, concentrated (P20 1,19 g/ml).
5.2 Hydrochloric acid, diluted 1+1.
Slowly add 500 ml of concentrated hydrochloric acid (5.1) to 500 ml of water, while stirring.
5.3 HydrochlorIc acId, diluted 1+9.
Slowly add 50 ml of concentrated hydrochloric acid (5.1) to 450 ml of water, while stirring.
5.4 Nitric acid, concentrated (p20 1,42 g/ml).
5.5 Hydrofluoric acid, concentrated (p20 1,15 g/ml).
5.6 Perchloric acid, concentrated (P20 1,70 g/ml).
5.7 Cadmium metal, minimum purity 99,99 %.
5.8 Cadmium, standard solution, 1 ml contains 1 mg of Cd.
Weigh, to the nearest 0,1 mg, 1,000 0 g of cadmium metal (5.7) into a 250 ml beaker. Add 10 ml of water and S ml of nitric acid (5.4). Cover and warm gently (if necessary) until the cadmium metal is dissolved. Heat to remove nitrogen oxides, then allow to cool and add about 50 ml of water. Transfer the solution to a 1 000 ml one-mark volumetric flask, add 40 ml of hydrochloric acid (5.2), fill up nearly to the mark with water, mix and cool to room temperature, then fill up exactly to the mark with water and mix again.
5.9 Cadmium, standard solution, 1 ml contains 100 .ag of Cd.
Pipette 10,00 ml of cadmium standard solution (5.8) into a 100 ml one-mark volumetric flask. Add 20 ml of hydrochloric acid (5.2). fill up nearly to the mark with water, mix and cool to room temperature, then fill up exactly to the mark with water and mix again.
5.10 Cadmium, standard solution, 1 ml contains 10 ig of Cd.
Pipette 10,00 ml of cadmium standard solution (5.9) into a 100 ml one-mark volumetric flask. Add 18 ml of hydrochloric acid (5.2), fill up nearly to the mark with water, mix and cool to room temperature, then fill up exactly to the mark with water and mix again.
5.11 Cadmium calibration solutions.
Prepare a series of calibration solutions by adding, from a pipette, 0,0 ml. 2,00 ml, 4,00 ml, 6,00 ml, 7,00 ml, 8,00 ml, 9,00 ml and 10,00 ml of cadmium standard solution (5.10) into a series of 100 ml onemark volumetric flasks. Dilute to the mark with hydrochloric acid (5.3) and mix thoroughly.AS ISO 19976.1 pdf download.