Industrial 1,4-oxazepine (morpholine) (2)

4 sampling

4.

4.

4.

4.

5 Test method

5.

The reagents and water used in this standard shall use analytical reagents and distilled water or water of the same purity when other requirements are not specified

The standard solutions, preparations and products used in this standard shall be prepared in accordance with GB/T601 and GB/T603 unless other requirements are indicated

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Industrial 1,4-oxazepine contains a secondary amine group, which is weakly basic and can be neutralized with hydrochloric acid to form industrial 1,4-oxazepine hydrochloride, according to the consumption standard during neutralization The amount of the solution, calculate the 1,4-oxazepine content

5.

Hydrochloric acid standard titration solution: c(HC1)=0.

5.

Weigh about 1g sample (accurate to 0.
0002g), add it to a 250mL conical flask containing 50mL carbon dioxide- free water, add 1 to 2 drops of methyl orange indicator solution, and titrate with 0.
5mol/L hydrochloric acid standard titration solution To orange-red, 30s does not fade as the end point
.
Do a blank test at the same time
.

5.
3.
4 Calculation of analysis results

The mass percentage (X) of industrial 1,4-oxazepine ( calculated as C ₄ H ₉ NO) is calculated by the following formula:

In the formula: c—the actual concentration of the hydrochloric acid standard titration solution, mol/L;

V—The volume of the standard titration solution of hydrochloric acid consumed by the sample, mL;

m—the mass of the sample, g;

0.
08712—The mass of 1,4-oxazepine expressed in grams equivalent to 1.
00mL hydrochloric acid standard titration solution [c(HCl)=1.
000mol/L]
.

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.
2%
.

5.
4 Determination of boiling range

Accurately read the temperature when the distillate volume is 5mL and 95mL.
After calibration, the temperature value should be within the specified range to be qualified
.
The following operations are carried out in accordance with the provisions of GB/T7534
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The indication range of the main thermometer is 100℃～150℃, and the condenser specification meets the requirements of 3.
4.
1 in GB/T7534
.
The K value of industrial 1,4-oxazepine at 741mmHg～800mmHg is 3.
38×10 ^-4 ℃/Pa
.

5.
5 Determination of density

According to the provisions 2.
3.
3 densimeter method of GB / T4472, the densitometer shown values ranging from 0.
960 g / cm & lt ^.
3 ~ 1.
050 g / cm & lt ^.
3
.

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.
0005 g/cm ³
.

5.
6 Determination of chromaticity

According to GB/T3143 regulations
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6 Marks, labels, packaging

6.
1 The packaging barrels of industrial 1,4-oxazepine should be painted with a strong mark
.
The basic content of the tag: product name, standard number, trademark, manufacturer name and address, date or production lot (available in place of the certificate or other means), quality grade, weight and so on
.

6.
2 The packaging barrel should be marked with "flammable liquid" according to GB190
.

6.
3 Industrial 1,4-oxazepine is packed in steel drums conforming to GB/T325, and the net weight of each drum is 200kg±0.
5kg, and the average net weight of batch products is not less than 200kg
.

6.
4 Industrial 1,4-oxazepine should be handled with care during handling to avoid impact and violent vibration
.

6.
5 Industrial 1,4-oxazepine should be stored in a dry, clean and ventilated warehouse, and should not be stored in the open air
.