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Determination of purity of industrial methyl ethyl ketone by gas chromatography
Brief description: Determination of purity of industrial methyl ethyl ketone by Shanghai Linghua gas chromatograph
Product details

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

column length/m

60

60

60

Column inner diameter/mm

0.25

0.25

0.25

Fixed liquid film thickness/μm

0.5

0.25

0.25

Detector Type

FID

TCD

FID

detector temperature/

250

Type of carrier gas

N2

He

H2

N2

carrier gas flow/(ml/min)

1.0

1.0

0.8

1.3

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

Vaporization chamber temperature/

220

Split Ratio

100:1

30:1

100:1

100:1

Injection volume/μL

1.0

Sample injection system: Micro injector(1μL~~10μL)

Chromatographic analysis softwareSD-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.

工业甲乙酮组分定性色谱图

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.

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