GB/T 36593-2018Method for chemical analysis of iridium powder—Determination of silver, gold, palladium, rhodium, ruthenium, lead, platinum, nickel, copper, iron, tin, zinc, magnesium, manganese, aluminum contents —Inductively coupled plasma atomic emission spectrometry (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This standard specifies silver (Ag), gold (Au), palladium (Pd), rhenium (Rh), ruthenium (Ru), lead (Pb), platinum (Pt), nickel (Ni), copper.

A method for measuring the amount of (Cu), iron (Fe), tin (Sn), zinc (Zn), magnesium (Mg), manganese (Mn), and aluminum (Al).

This standard applies to the determination of silver, gold, palladium, rhodium, iridium, lead, platinum, nickel, copper, iron, tin, zinc, magnesium, manganese and aluminum. Measuring range. 0.0010%~0.10%.

2 Method summary

The sample is digested with hydrochloric acid-potassium chlorate at high temperature and high pressure, and is connected to each element to be tested by inductively coupled plasma atomic emission spectrometry.

The mass fraction of the impurity element is measured and calculated at the wavelength of the wavelength.

3 Reagents and materials

3.1 Potassium chlorate.

3.2 Nitric acid (rho = 1.42 g/mL).

3.3 Hydrochloric acid (rho = 1.19 g/mL).

3.4 Hydrogen peroxide (30%, volume fraction).

3.5 Mixed acid. Three units of hydrochloric acid (3.3) are mixed with one unit volume of nitric acid (3.2).

3.6 Hydrochloric acid (1 4).

3.7 Silver standard storage solution. Weigh 0.1000g of metallic silver (mass fraction >=99.99%) and place it in a 100mL Teflon beaker. Add 2mL of nitric acid (3.2), heat and dissolve completely at low temperature, transfer to a 100mL volumetric flask, add 10mL of nitric acid (3.2), dilute with water to Scale. Mix well. 1 mL of this solution contained 1.0 mg of silver.

3.8 Palladium standard storage solution. Weigh 0.1000g of metal palladium (mass fraction >=99.99%) and place it in a 100mL Teflon beaker. Add 4mL mixed acid (3.5), dissolve completely at low temperature, transfer to a 100mL volumetric flask, add 10mL hydrochloric acid (3.3), dilute with water To the scale. Mix well. 1 mL of this solution contained 1.0 mg of palladium.

3.9 Platinum standard storage solution. Weigh 0.1000g of metal platinum (mass fraction >=99.99%) and place it in a 100mL Teflon beaker. Add 5mL mixed acid (3.5), dissolve completely at low temperature, evaporate to a small volume, take off slightly cold, add 10mL hydrochloric acid (3.3), boil, cold However, transfer to a 100 mL volumetric flask, dilute to the mark with water, and mix. 1 mL of this solution contained 1.0 mg of platinum.

3.10 Rhodium standard storage solution. weigh 0.1000g rhodium powder (mass fraction >= 99.99%), placed in a PTFE microwave digestion tank, add 10 mL of hydrochloric acid (3.3), 3 mL of hydrogen peroxide (3.4), sealed. Dissolve at 210 ° C for about 4 h until the sample dissolves completely and cool to room temperature. Transfer the solution to a 100 mL volumetric flask, add 10 mL of hydrochloric acid (3.3), dilute to the mark with water, and mix. This solution contains 1mL 1.0mg rhodium.

3.11 Ruthenium standard storage solution. weigh 0.1000g ruthenium powder (mass fraction >= 99.99%), placed in 50mL high temperature and high pressure digestion tube, plus […]