Industrial Hexachloroethane (3)

4.

4.

Weigh an appropriate amount of E-301, dissolve it with chloroform , pour the weighed 6201 carrier into the above solution, mix it, and dry it under an infrared lamp

4.

Into the carrier gas: aging at 120°C for 8 hours

4.

4.

4.

4.

Start the chromatograph, and start the injection after the selected working conditions are stable.

4.

The purity X1 expressed in mass percentage is calculated according to formula (1):

In the formula: f — the relative correction factor of hexachloroethane ;

A—The peak area of ​​hexachloroethane;

fi—the relative correction factor of component i;

Ai—the peak area of ​​component i

Take the arithmetic mean of the two parallel determination results as the determination result

4.

According to the provisions of GB/T617

4.
3 Determination of moisture

According to the regulations of GB/T6283, the solvent in the titration cell is a mixture of 25mL methanol and 25mL carbon tetrachloride (1:1)
.
Take the arithmetic mean of the two parallel determination results as the determination result
.
The relative deviation of the two parallel determination results shall not be greater than 10%
.

4.
4 Determination of Ash

Carry out according to the regulations of GB/T7531, the burning temperature is (750±25)℃, and the residue B after burning is reserved for the determination of iron content
.

4.
5 Determination of iron content

According to the provisions of GB/T3049
.

4.
5.
1 Preparation of test solution

Add 2 mL of (1+1) hydrochloric acid solution to the crucible containing residue B , and heat to dissolve
.

4.
5.
2 Expression of analysis results

The iron content X2 expressed in mass percentage is calculated according to formula (2):

Where: W—the quality of the drink obtained from the standard curve, g;

m—The mass of the sample weighed in 4.
4, g
.

Take the arithmetic mean of the two parallel determination results as the determination result
.
The relative deviation of the two parallel determination results shall not be greater than 15%
.

4.
6 Free chlorine test

4.
6.
1 Principle

The free chlorine in the sample is extracted with water, and the free chlorine reacts with potassium iodide to precipitate iodine, and the iodine is adsorbed by the starch and turns blue
.

Cl ₂ +2KI=2KCl+I ₂

4.
6.
2 Reagents and materials

4.
6.
2.
1 Potassium iodide solution: 100g/L
.

4.
6.
2.
2 Starch indicator solution: 5g/L
.

4.
6.
3 Analysis steps

Weigh 10.
0g sample (accurate to 0.
01g), place it in a 250mL conical flask with a stopper, add 30mL water, shake for 5min and then stand for 20min, filter it in a 50mL colorimetric tube, and shake with appropriate amount of water Shake and wash the filter residue, filter it in the same colorimetric tube, add water to 50mL, add 2.
0mL potassium iodide solution and 1mL starch indicator solution, the solution should be no blue
.
Keeping the color unchanged for 30s is qualified
.

4.
7 Determination of chloride content

Weigh about 10g of sample (accurate to 0.
0002g), place it in a 250mL conical flask with a stopper, add 30mL of water, shake for 5min and then stand for 20min, filter in a 500mL conical flask, shake with 10mL of water Wash the filter residue, add 120mL absolute ethanol to the same Erlenmeyer flask, and all others shall be carried out in accordance with the provisions of GB/T3051
.

Take the arithmetic mean of the two parallel determination results as the determination result, and the relative deviation of the two parallel determination results shall not exceed 15%
.

Related Links: Hexachloroethane for Industrial Use (2)