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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
The standard titration solution used in the analysis shall be prepared in accordance with the provisions of GB/T601-2002 when other requirements are not specified
5.
5.
Using capillary column gas chromatography
5.
5.
5.
5.
5.
5.
5.
5.
5.
3.
4 Chromatographic column and typical operating conditions
The chromatographic column and chromatographic operating conditions recommended by this standard are shown in Table 2
.
Refer to Figure A.
1 and Table A.
1 in Appendix A for typical chromatograms and relative retention values of each component
.
Other chromatographic columns and chromatographic operating conditions that can achieve the same degree of separation can also be used
.
The chromatographic column should be aged before first use
.
Under the condition of introducing carrier gas (N 2 ), the column temperature is 120°C, and the aging is 8h
.
Table 2 Recommended chromatographic column and chromatographic operating conditions
5.
3.
5 Analysis steps
According to the instrument manual, adjust the instrument to the operating conditions shown in Table 2, and start the measurement after the instrument is stable
.
According to the chromatographic bee area of each component and its relative correction factor, the correction area normalization method is used for quantification
.
For the determination of the relative correction factor, refer to Appendix A, A.
3
.
5.
3.
6 Result calculation
The mass fraction w 1 of nitromethane , the value is expressed in %, calculated according to formula (1):
Where:
A 1 —the area of the chromatographic peak of nitromethane;
f 1 -the relative correction factor of nitromethane;
A i —the area of the chromatographic peak of component i;
f i — relative correction factor of component i;
w Water —The water content in mass fraction measured according to 5.
6, expressed in (%)
.
Note: The value of the relative correction factor of the unknown component in the sample is 1
.
The calculation result is to two decimal places
.
Take the arithmetic mean of the two parallel determination results as the determination result
.
The absolute difference between the two parallel determination results is not more than 0.
1%
.
Related Links: Nitromethane for Industrial Use (1)