GB/T 23513.3-2009Chemical analysis methods for germanium concentrate - Part 3: Determination of sulfur content - Barium sulfate gravimetry (English PDF)

3.1

potassium chlorate (KClO3).

3.2

ammonium carbonate ((NH4) 2CO3).

Nitrate 3.3 (rho1.42g/mL).

3.4

hydrochloride (rho1.19g/mL).

3.5

Ammonia (rho1.09g/mL).

3.6

HCl (1 + 1).

Hydrochloride 3.7 (95 + 5).

3.8

barium chloride (100g/L).

3.9

methyl orange indicator (0.2%).

3.10

Sodium chloride (200g/L).

3.11 ferric chloride solution (1%)

Weigh 10g of ferric chloride, add hydrochloric acid (3.4) is dissolved and transferred to 1000mL volumetric flask, dilute with water

Release to the mark.

Step 4 Analysis

4.1 Sample

The samples were ground through 0.125mm (120 mesh) after Sieve Weigh 1.0g sample, accurate to 0.0001g.

4.2

Determination of the number of

Independently two determinations, the mean value.

4.3 blank test

Along with sample blank test.

4.4 Determination of total sulfur

4.4.1

The sample (4.1) into 300mL beaker, add 5g potassium chlorate (3.1) and a small amount of water, so shaken was mashed, added 20mL

Nitric acid (3.3) a table covered dish, place the decomposition 2h at room temperature, heated steam until nearly dry, low temperature shifted to dryness, was added 20mL of hydrochloric acid (3.4), then

After dissolved by heating and steam until nearly dry, repetitive 10mL hydrochloric acid (3.4) evaporated to near dryness, evaporated to dryness at low temperature shift, plus 10mL hydrochloric acid (3.4)

Low heat to dissolve the soluble salts removed [such as iron in a sample of less than 10mg, should be added to 2mL ferric chloride solution (3.11)].

4.4.2

solution (4.4.1) adding water to a volume of about 100mL, was heated to near boiling, removed, generation of ferric hydroxide with stirring under sink with ammonia (3.5) […]