This method is suitable for purity greater than99%(mass fraction)Determination of methyl ethyl ketone sample. Using a hydrogen flame ionization detector(FID)When the low detection concentration of impurities in Zen is0.001%(mass fraction)Use thermal conductivity detector(TCD)When the low detection concentration of impurities in Zen is0.01%(mass fraction).
Reagents and materials
1. Carrier gas: useFIDWhen using nitrogen as the carrier gas, useTCDWhen using helium or hydrogen as the carrier gas, with a purity of ≥99.999%(volume fraction).
2. combustion gas(FID)Hydrogen, purity ≥99.999%(volume fraction).
3. Marker substances: Used for determining calibration factors, including methyl ethyl ketone, n-hexane, isopropyl ether, n-propyl ether, acetone, etc1-Xinxi, sec butyl ether, ethyl acetate, tert butanol, methanol, isopropanol, ethanol, n-butyl ether, sec butanol, and n-propanol, etc. Among them, methyl ethyl ketone is used as the base solution for preparing standard samples, and the purity should not be lower than99.7%(mass fraction)The purity of other standard substances should not be lower than99%(mass fraction).
Instruments and equipment
1. gas chromatograph
Prepare hydrogen flame ionization detector(FID)Or thermal conductivity detector(TCD)The gas chromatograph. useFIDAt that time, the instrument0.001%(mass fraction)The peak height generated by impurity components should be greater than twice the noise level; useTCDAt that time, the instrument0.01%(mass fraction)The peak height generated by impurity components should be greater than five times the noise. The dynamic linear range of the instrument should meet quantitative requirements.
2. Column and instrument setup conditions
Column type |
polyethylene glycol(20M) |
Fluorinated propyl methylsiloxane |
polymethylsiloxane |
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column length/m |
60 |
60 |
60 |
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Column inner diameter/mm |
0.25 |
0.25 |
0.25 |
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Fixed liquid film thickness/μm |
0.5 |
0.25 |
0.25 |
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Detector Type |
FID |
TCD |
FID |
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detector temperature/℃ |
250 |
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Type of carrier gas |
N2 |
He |
H2 |
N2 |
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carrier gas flow/(ml/min) |
1.0 |
1.0 |
0.8 |
1.3 |
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Column temperature |
initial temperature/℃ Initial temperature holding time/min heating rate/(℃/min) final temperature/℃ Final temperature holding time/min |
60 10 10 150 11 |
35 8 15 200 1 |
60 7 10 150 4 |
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Vaporization chamber temperature/℃ |
220 |
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Split Ratio |
100:1 |
30:1 |
100:1 |
100:1 |
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Injection volume/μL |
1.0 |
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Chromatographic analysis software:SD-2020Type chromatography workstation
Qualitative analysis of componentsAnalyze the sample and standard sample under the same conditions, and qualitatively determine the components in the sample based on the chromatographic retention time.
The determination, calculation, and instrument repeatability testing of correction factors should be carried out in accordance with the standards of the Chinese petrochemical industrySH/T 1756-2006Execution.