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5 Test method
5.
Some test procedures specified by the test method may lead to dangerous situations
5.
Unless otherwise specified, only reagents confirmed to be analytically pure and grade 3 water specified in GB/T6682-1992 are used in the analysis
5.
5.
Using gas chromatography, under selected working conditions, the sample is vaporized and passed through a capillary chromatographic column to separate its components, and detected by a hydrogen flame ionization detector.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
3.
4 Chromatographic analysis conditions
The recommended chromatographic column and typical chromatographic operating conditions are shown in Table 2
.
The typical chromatogram of the capillary column is shown in Appendix A, Figure A.
1, and the relative retention value of each component is shown in Appendix A, Table A.
1
.
Other chromatographic columns and color-harmonic operating conditions that can achieve the same degree of separation can be used
.
Table 2 Recommended analysis conditions for capillary columns
5.
3.
5 Analysis steps
5.
3.
5.
1 Determination of relative correction factor
Refer to Appendix B for the determination method of relative correction factor
.
5.
3.
5.
2 Start the gas chromatograph and debug the instrument according to the chromatographic operating conditions listed in Table 2.
After the baseline is stable, use the micro syringe injector for sample analysis, and use the chromatographic data processor or chromatographic workstation to calculate the results
.
5.
3.
6 Result calculation
The mass fraction w i of each tested component , the value is expressed in %, respectively calculated according to formula (1):
Where:
f i — the correction factor of the measured component i;
A i —the peak area of the measured component i;
wH 2 O—The water content measured in accordance with 5.
5 is expressed in mass fraction;
∑f i A i — the sum of the corrected peak areas of each component
.
Take the arithmetic mean of the two parallel determination results as the determination result
.
The absolute difference between the two parallel determination results of cyclohexene content is not more than 0.
2%, and the absolute difference between the two parallel determination results of cyclohexane content, benzene content and chlorocyclohexane content is not greater than the arithmetic mean of the two determination values 5% of the value
.
5.
4 Determination of chromaticity
Measure according to the provisions of GB/T3143-1982 (2004)
.
5.
5 Determination of moisture
Measure according to the regulations of GB/T6283
.
Take the arithmetic mean of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not be greater than 20% of the arithmetic mean of the two determination values
.
Table 3 Recommended analysis conditions for capillary columns
Related Links: Cyclohexene for Industrial Use (1)