Industrial Chloromethyl Methyl Ether (2)

4 Test method

The reagents and water used in this standard, unless other requirements are specified, all use analytical reagents and distilled water or water of the same purity

The standard solutions, preparations and products used in this standard shall be prepared in accordance with GB/T601 and GB/T603 when no special requirements are indicated

4.

4.

4.

4.

After the organic chlorine in the sample is converted into inorganic chlorine by sodium hydroxide treatment, add a known excess of silver nitrate standard titration solution, use ferric ammonium vanadium as an indicator, and use ammonium thiocyanate standard titration solution to back drop the excess silver nitrate standard titration solution

The reaction formula is as follows:

4.

4.

4.

4.

4.

4.

4.

4.

General laboratory equipment and

4.
2.
3.
1 Volumetric flask: 50mL;

4.
2.
3.
2 Brown burette: 50mL;

4.
2.
3.
3 Pipette: 20mL, 10mL, 1mL
.

4.
2.
4 Analysis steps

Measure 20mL sodium hydroxide solution (4.
2.
2.
3) in a 50mL volumetric flask and weigh to the nearest 0.
0001g, quickly add 0.
5mL sample, stoppered and shake vigorously until the white smoke in the bottle disappears, weighing after about 10 minutes The amount, accurate to 0.
0002g, add water to dilute to the mark, this solution is A solution
.

Put 50mL water in the Erlenmeyer flask, then pipette 10.
00ml A solution into the Erlenmeyer flask, add 5mL nitric acid solution (4.
2.
2.
2), 5mL nitrobenzene (4.
2.
2.
1), dropwise add 25.
00mL silver nitrate standard titration solution ( 4.
2.
2.
4), add 2ml ferric ammonium sulfate indicator (4.
2.
2.
6), and then titrate with ammonium thiocyanate standard titration solution (4.
2.
2.
5) until brick red appears as the end point
.

4.
2.
5 The total chlorine content expressed by mass percentage (X) is calculated according to formula (1):

In the formula: c ₁ -the actual concentration of the silver nitrate standard titration solution, mol/L;

c ₂ —The actual concentration of ammonium sulfide standard titration solution, mol/L;

V _.
1 - silver nitrate Volume standard titration solution, mL;

V ₂ —The volume of the standard titration solution that consumes ammonium sulphate , mL;

m—the mass of the sample, g;

0.
03545 —The mass of chlorine in grams equivalent to 1.
00 mL of ammonium thiocyanate standard titration solution [c(NH ₄ SCN)=1.
000mol/L], g
.

Take the arithmetic average of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.
1%
.

4.
3 Determination of density

Measure according to the density meter method in section 2.
3.
3 of GB/T4472
.

Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.
001 g/cm ³
.

4.
4 Distillation test

Record the distilled volume between 55°C and 59.
5°C, and control the cooling water outlet temperature not to exceed 15°C
.

Other operating conditions shall be carried out in accordance with Article 4 of GB/T7534
.

Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 1 mL
.

Related Links: Industrial Chloromethyl Methyl Ether (1)