GB/T 8152.13-2017Methods for chemical analysis of lead concentrates - Part 13: Determination of thallium content - Inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry (English PDF)

2.1 Method summary

Samples of hydrochloric acid, nitric acid, sulfuric acid decomposition, with 193Ir as internal standard, determined by inductively coupled plasma mass spectrometry, with the standard curve method

Calculate the amount of thallium in the sample.

2.2 Reagents

Only the reagents identified as superior and pure are used in the analysis. The water used is primary water.

2.2.1

Hydrochloric acid (p = 1.19 g/mL).

2.2.2

Nitric acid (p = 1.42 g/mL).

2.2.3

Sulfuric acid (rho = 1.84 g/mL).

2.2.4

nitric acid (1 1).

2.2.5

Nitric acid sulfuric acid mixed acid (1 1) To 500mL nitric acid (2.2.2) was added while stirring 500mL sulfuric acid (2.2.3), after cooling use.

2.2.6

thallium standard stock solution Weigh 0.2795g thallium trioxide (wTl2O3 >= 99.99%) placed in a.200mL beaker, covered with a surface

Dish, slowly add 25mL nitric acid (2.2.4) dissolved at low temperature, drive out nitrogen oxides, remove the cooling to room temperature, wash the watch glass and the cup wall with water,

Into a 250mL volumetric flask, diluted with water to the mark, mix well. 1mL of this solution contains 1mg thallium.

Thallium standard solution A. Thallium standard stock solution (2.2.6) diluted to thallium concentration of 100ng/mL to nitric acid (2 98) as a medium.

Thallium standard solution B. Thallium standard solution A diluted to thallium concentration of 10ng/mL to nitric acid (2 98) as a medium.

2.2.7

Internal standard solution .10ng/mL193Ir solution to nitric acid (2 98) as a medium.

2.2.8

Argon .wAr >= 99.996%.

2.3 Instruments

Inductively Coupled Plasma Mass Spectrometry with a resolution of 0.1 amu ~ 1 amu; 205 T1 isotope response > 105.

2.4 sample

2.4.1

The sample shall pass through a 0.074 mm hole sieve.

2.4.2

The sample should be oven at 105 °C ± 5 °C bake 1h, and placed in a desiccator cooled to room temperature for use.