SY/T 0542-1994 Gas chromatography for analysis of stable light hydrocarbon components

SY/T 0542-1994 Stable light hydrocarbon component analysis by gas chromatography SY/T0542-1994 standard download decompression password: www.bzxz.net

Petroleum and Natural Gas Industry Standard of the People's Republic of China SY/T 0542--94
Analysis of Stable Light Hydrocarbon Components
Published on December 21, 1994
China National Petroleum Corporation
Gas Chromatography
Implementation on June 1, 1995
1 Subject Content and Scope of Application
Petroleum and Natural Gas Industry Standard of the People's Republic of China Analysis of Stable Light Hydrocarbon Components
Gas Chromatography
This standard specifies the analytical method SY/T 0542 for the determination of stable light hydrocarbon components by gas phase Monnot method 94
Non-standard Applicable to the determination of constant light components of stable light hydrocarbons, also applicable to the determination of light components of liquid hydrocarbon mixtures with similar composition
2 Referenced standards
SY/I0543:94 Sampling method for stable light hydrocarbons GB9053·-88 Stable light hydrocarbons
3 Summary of the method
Stable light hydrocarbon samples are separated by paper tubes: detected by flame ionization detector (FID), and the peak areas of the spectrum are recorded by electronic integrator or chromatographic workstation. The spray percentage of the component is calculated by normalization method. Reagents and materials
Fluorine gas purity is not less than 99.99%;
b, hydrogen: purity is not less than -99.99%
C. Room gas: Purified by drying:
d. Standard sample of pure substance and mixed standard sample:
e: Micro-injection solution: 1l or sul:
f. Sampler: 259~[000ml stainless steel bottle or can with oil-resistant rubber pad. The can must be able to withstand a pressure of more than 0.2MPa. Sampler schematic diagram Figure 1:
Pressure cycle with middle hole
Oil-resistant pad
a Steel cylinder
5 Instruments and equipment
Figure 1 Sampler schematic diagram
5.1 Gas chromatograph: Any gas chromatograph that meets the following technical indicators can be used. Approved by China National Petroleum Corporation on December 21, 1994, implementation on June 1, 1995, SY/T 0542---94, 5.1.1 Orderly heating of coke, non-fire box separation, differential flow injection device, 5.1.21 Detection limit not greater than 10×10-g5, less than 5%, 101% and less than 105, 5.2 The chromatographic column must be able to completely separate the delivered gas. Generally, a polymethylsiloxane capillary with an inner diameter of 0.2~0.3111 and a length of 501m is used: 5.3 Electrochemical analyzer or spectrum workstation
6 Operation steps
Instrument preparation
6.1.1 Carrier gas nitrogen: linear velocity 15~20cm/s:6.1.2 Fuel gas: hydrogen: flow rate 30ml/min6.13 Supplementary gas: nitrogen, flow rate 30n1lmin;6.1.4 Auxiliary gas: air, flow rate 300ml/min6.1.5 Split ratio: 1:100 6.1.6 Chromatographic operating conditions are shown in Table 1, where Method 1 is used for general analysis and Method 2 is used for monomer hydrocarbon analysis. Table 1 Chromatographic operating conditions Method 1 Chromatographic column Initial temperature, °C Holding time, min. Temperature rate, min Final temperature, °C Holding time, min Vaporization chamber temperature Vaporizer temperature OV-101 or SE-30
50mx0.22mm
6.1.7 According to the specific situation, select the best integration parameters of the integrator or chromatography workstation. 6.2 Sample preparation
Fangda II
OV101 or SF-30
50mx0.22mm
6.2.1 For stable hydrocarbon samples, use a closed cylinder for sampling: when sampling in a bulk tank or taking a known stable light hydrocarbon sample of No. Ⅱ specified in GB9053, you can use an oil can for direct sampling: sampling method SYT0543. 6.2.2 Sample transfer: Put the sample in the oil can and a clean small sample bottle in the refrigerator, keep the temperature constant for 2h, shake the sample vigorously, put it in the refrigerator and let it stand for 5min, use the sample to clean the small sample bottle 3 times, and then Then quickly transfer the sample, and store the sample at least 80% of the volume of the small sample bottle: Immediately seal the small sample bottle 6.3 Injection
When the various parameters of the chromatograph reach the set values ​​and stabilize, use the micro-injector stored with the sample at low temperature to extract 0.1~1ul of sample from the small companion bottle or steel cylinder, and quickly inject it into the vaporization chamber. The injector stays in the vaporization chamber for about 5s and then quickly withdraws it: While injecting the sample, press the integration key of the integrator or chromatographic workstation, record the spectrum and integrate the drop area. 7 Qualitative
Use relative retention time for qualitative analysis. First, use the mixed standard sample and pure substance to quantify the normal alkanes and important aromatics, cycloalkanes and components of interest in the sample. Other small peaks and peaks that cannot be quantified may not be quantified one by one when it is not necessary. r 0542-94
(, all the qualitative bands between them were taken as isomers (, good, must, single-phase differential analysis was performed by coupling instrument, and the typical chromatographic analysis was accurately recorded as a true reference.
8 Quantification
was quantified by the heart-to-heart method. The relative masses of each component were calibrated by using mixed standard samples. In the absence of mixed standard samples, the literature values ​​given in Appendix B (Reference Positions) may also be used. 7 The mass percentage of the component is calculated by the following formula: Wwww.bzxz.net
Where: W: mass percentage of the component, AF
.4: peak area of ​​a component detected on FID, F: relative mass correction factor of the component on FID. 9 Precision
Repeatability
The difference between the two results of repeated determination of the same sample by the same operator should not be greater than the values ​​given in Table 2. 9.2 Reproducibility
The difference between the results of the same sample determined by different laboratories without adjusting the operator should not be greater than the values ​​given in Table 2. Table 2 Precision
10 Report
Repeatability, %
The arithmetic mean of the results of two or more repeated determinations is taken as the analysis result: Reproducibility, %
Sr/ T 0542 94
Analysis chromatogram of stable light hydrocarbon components
(reference)
Figure A Typical gas chromatogram of the analysis of stable light hydrocarbon components [-7-alkane: 2-propane: 3-isobutane: 4-n-butylene; 5-isobutane; 6-n-butylene: 72-2-dimethylbutane 8-2,3-hexadecane: 9-2-methylcyclohexane: 10-3-methylcyclohexane: 11-n-hexane: 12-hexane: [3 -benzene: 14 - cyclohexane: 15 - 2-methyltrioxane: 16 - 3-methylhexane: 17 - n-heptane: 18 - cyclohexane: 19 - cyclopentane 20 - n-octane: 21 - n-hexadecane; 22 - n-decane: 23 - n-1-oxane: 24 - n-dodecane: 15 -oxane: 26 - tetradecane components
isobutane
pentane
2.2-dimethylbutane
2-methylcyclopentane| |tt||n-Hexane
2-Methylhexane
n-Butane
p-Xylene
n-Xylene
SY/T0542-94
Appendix B
Relative mass correction factors of some components on FID (reference)
Zhou Le (F)
n-Butane
2,3-Dimethylbutane
3-Methyl Pentane
Methylcyclopentane
N-methylhexane
N-cyclohexane
N-octanol
Meta-xylene
O-xylene
Factor (F)
Note: The relative mass correction factor of isoalkanes before n-octanol can adopt the factor of its n-alkane, and the relative mass correction factor of components after n-octanol adopts 1.02.
Additional Note:
This standard is technically managed by the Petroleum Planning and Design Institute. This standard was drafted by the Survey and Design Institute of the Central Plains Petroleum Exploration Bureau. The main drafters of this standard are Li Peijie and Yan Wencan.
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