Industrial p-chlorophenol (1)

1 Subject content and scope of application

This standard specifies the technical requirements, test methods, inspection rules and signs, packaging, transportation and storage requirements for industrial p-chlorophenol

This standard applies to p-chlorophenol produced by the direct chlorination of phenol and sulfuryl chloride

Molecular formula: C ₆ H ₅ OC1

Structural formula:

Relative molecular mass: 128.

2 Reference standards

GB190 dangerous goods packaging mark

Preparation of preparations and products used in GB/T603 chemical reagent test method

The expression method and judgment method of GB/T1250 limit value

GB/T6283 Determination of water content in chemical products Karl Fischer method (general method)

GB/T6678 General Rules for Sampling of Chemical Products

GB/T6679 General Rules for Sampling of Solid Chemical Products

GB/T7533 Test Method for Crystallization Point of Organic Chemical Products

3 Technical requirements

3.

3.

4 Test method

The reagents used in the test methods of this standard, unless other requirements are specified, all use analytical reagents

The preparations and products used in the test were prepared in accordance with the provisions of GB/T603 when other special requirements were not indicated

4.

4.

The sample was dissolved in ethyl acetate , and the sample was injected for analysis under the specified chromatographic operating conditions

4.

4.

4.

4.

4.

a) Fixing solution: polycyanoalkylsiloxane (OV-225);

b) Carrier: Chromosorb W AW DMCS, 0.

c) Chromatographic column tube: stainless steel spiral tube column, column length 1m, inner diameter 4mm;

d) Preparation and aging of chromatographic column:

Prepare the stationary phase according to the ratio of Chromosorb WAW DMCS:OV-225=100:5;

Dissolve OV-225 in ethyl acetate whose volume is slightly larger than the volume of the carrier , and then pour the pre-weighed carrier into it and mix well
.
Stir gently under infrared light to completely volatilize the solvent, then place in an oven to dry at 40℃～60℃ for 4h; fill the prepared stationary phase into the chromatographic column by pumping column method, the filling amount is about 3g /m, the two ends of the column are plugged tightly with glass fiber, and then aging for 12 hours under the condition of 30℃ higher than the column temperature, nitrogen gas flow rate 20mL/min;

It is required that the resolution of the peak width of the difficult-to-separate substances is ≥1.
8;

When the above analysis requirements can be met, other suitable chromatographic columns can also be used
.

4.
1.
2.
5 Carrier gas and auxiliary gas

a) Carrier gas: nitrogen , with a purity of not less than 99.
95%, dried and purified by silica gel and molecular sieve;

b) Combustion gas: hydrogen , with a purity of not less than 99.
9%;

c) Combustion gas: air, dried and purified by silica gel and molecular sieve
.