CN104713975A - Method for simultaneously detecting contents of hydrocarbon impurities and nitrogen impurity in hydrogen - Google Patents
Method for simultaneously detecting contents of hydrocarbon impurities and nitrogen impurity in hydrogen Download PDFInfo
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Abstract
A method for simultaneously detecting contents of hydrocarbon impurities and a nitrogen impurity in hydrogen can solve the problem that the contents of the hydrocarbon impurities and the nitrogen impurity in hydrogen cannot be detected simultaneously in the prior art. With adopting of a gas chromatographic method, and under selected working conditions, a sample introduction valve is used for simultaneously introducing two parts of gas samples to respectively go into two channels, one channel is used for analysis of hydrocarbon substances, the other channel is used for analysis of the content of nitrogen, a chromatography column is used for separating the to-be-detected samples respectively, then the contents of the hydrocarbon impurities and nitrogen in the samples are detected simultaneously by a thermal conducting detector and a hydrogen flame ionization detector, and calculation is carried out by using an external standard method; the method is simple, convenient and quick to operate.
Description
Technical field
The present invention relates to petrochemicals detection technique field, is a kind of method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level specifically.
Background technology
Hydrogen is the main raw material of industry, is also most important industrial gasses and special gas, has a wide range of applications in petrochemical complex, electronics industry, metallurgical industry, food processing, Aero-Space etc.Some refinerys prepare industrial hydrogen by pressure-variable adsorption principle, due in its raw material containing hydrocarbons based on methane and nitrogen, if it is not thorough to prepare magazins' layout in hydrogen process, probably cause containing hydrocarbon impurities and a large amount of nitrogen such as methane in prepared hydrogen, directly affect the purity of hydrogen.At present, the standard of plant hydrogen purity testing is all to oxygen in hydrogen product, the independent mensuration of the materials such as nitrogen, the mensuration of hydrocarbon impurities is also only had to the mensuration of methane one-component, not other hydrocarbon impurities (ethane in hydrogen manufacture, ethene, propane, trimethylene, propylene, normal butane, isobutane, Trans-2-butene, butene-1, isobutylene, maleic, isopentane, n-pentane, 1.3-butadiene etc.) method for measuring, more there is no the method for hydrogen high purity propylene and Nitrogen gas impurity Simultaneously test, this brings a lot of inconvenience to the monitoring in hydrogen manufacture.
Summary of the invention
The object of the invention is a kind of method that hydrocarbons and nitrogen content in Simultaneously test hydrogen are provided for above-mentioned Problems existing exactly, with the hydrocarbons quickly and accurately quantitatively in hydrogen and nitrogen impurity level.
The technical solution adopted in the present invention is: use vapor-phase chromatography to analyze hydrogen high purity propylene and nitrogen impurity level, it is characterized in that: described gas chromatograph should be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) simultaneously, chromatographic column adopts two chromatography columns and a capillary chromatographic column; Carrier gas is high-purity hydrogen and high pure nitrogen.
Described operation condition of chromatogram: injector temperature 100 DEG C ~ 200 DEG C; Column temperature 35 DEG C ~ 190 DEG C, adopts temperature programme pattern, initial temperature: 35 ~ 40 DEG C, keeps 2 ~ 5min, then rises to 100 DEG C with the speed of 4 ~ 7 DEG C/min, then rise to 190 DEG C with the speed of 6 ~ 12 DEG C/min, keeps 20min; Detector temperature is 200 DEG C ~ 300 DEG C, split ratio 10:1 ~ 30:1.
Preferred operation condition of chromatogram: injector temperature 100 DEG C, column temperature 40 DEG C ~ 190 DEG C, adopt temperature programme pattern, Thermal Conductivity actuator temperature is 200 DEG C, and flame ionization ditector temperature is 300 DEG C, and split ratio is 20:1.
Chromatography column is porous polymer gas phase packed column and molecular sieve packed column.
Chromatography column is stainless steel chromatographic column.
Chromatography column is Porapack Q chromatographic column and 5A molecular sieve chromatography post respectively, and wherein 5A molecular sieve chromatography post also can change 13X molecular sieve chromatography post into.
Capillary chromatographic column is the chromatography on alumina post by sodium sulphate deactivation.
Porapack Q column's length 1.5m ~ 2m, internal diameter 3 ~ 4mm, Stationary liquid is 45 ~ 100 orders.
5A molecular sieve chromatography post column length 1.5m ~ 3m, internal diameter 3 ~ 4mm, Stationary liquid is 45 ~ 100 orders.
Capillary chromatographic column is HP-PLOT Al
2o
3/ S.
The column length of capillary chromatographic column is 25m ~ 50m, and Stationary liquid thickness of liquid film is 5 μm ~ 15 μm, and internal diameter is 0.25 mm ~ 0.53mm.
Preferred Porapack Q column's length 1.8288m, internal diameter 3.17mm, Stationary liquid is Porapack Q(80 ~ 100 orders).
Preferred 5A molecular sieve chromatography post column length 1.8288m, internal diameter 3.17mm, Stationary liquid is 5A molecular sieve (45 ~ 60 order).
The column length of preferred capillary chromatographic column is 25m, and Stationary liquid thickness of liquid film is 8 μm, and internal diameter is 0.32mm.
A kind of described method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level, operation steps is:
(1) sample at the scene, under chromatographic column operating conditions, carry out stratographic analysis;
(2) go out peak result according to chromatogram, carry out quantitatively to sample high purity propylene and Nitrogen gas impurity, quantivative approach adopts external standard method.
Hydrogen sample feeding amount is 0.5mL ~ 2.0mL.
The advantage that the present invention has and positive technique effect are: the present invention is that the Simultaneously test of hydrogen high purity propylene and nitrogen impurity level provides one detection method accurately and effectively, adopt such scheme, can easily under selected condition of work, adopt the gas chromatograph being simultaneously furnished with a thermal conductivity detector (TCD) and a flame ionization ditector, utilize sampling valve to introduce two parts of gaseous samples simultaneously, enter two passages respectively, one tunnel is for analyzing hydrocarbons, one tunnel is for analyzing nitrogen content, respectively testing sample is separated by chromatographic column simultaneously, then with thermal conductivity detector (TCD) and flame ionization ditector, the hydrocarbon impurities in sample and nitrogen content are detected simultaneously, for the monitoring in hydrogen manufacture provides conveniently, avoid simultaneously and use multiple stage instrument, the repeatedly trouble of sample introduction operation, use the method is easy and simple to handle, fast.
Accompanying drawing explanation
Fig. 1 is depicted as the inventive method and measures from sample gas high purity propylene content chromatogram simplified schematic diagram;
Figure 2 shows that the inventive method measures hydrogen sample high purity propylene content chromatogram simplified schematic diagram;
Figure 3 shows that the inventive method measures nitrogen content chromatogram simplified schematic diagram in hydrogen.
The present invention to be described in further detail by example below in conjunction with accompanying drawing; but following example is only the present invention's example wherein; do not represent the rights protection scope that the present invention limits, the scope of the present invention is as the criterion with claims.
Embodiment
embodiment 1
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure autogamy standard specimen gas, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in sample gas and nitrogen, the result obtained is that the hydrocarbon impurities content in gas is respectively: methane: 513.7 ppm, ethane: 241.4 ppm, ethene: 553.4 ppm, propane: 54.5 ppm, trimethylene: 12.7 ppm, propylene: 507.6ppm, isobutane: 22.5ppm, normal butane: 23.1 ppm, Trans-2-butene: 50.1 ppm, butene-1: 120.6 ppm, isobutylene: 61.5 ppm, cis-2-butene: 45.1 ppm, isopentane: 8.3 ppm, n-pentane: 9.7 ppm, 1.3-butadiene: 16.33 ppm, propine: 40.1 ppm, as accompanying drawing 1, nitrogen content is 180.5ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 2
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 150 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect (as accompanying drawing 2), nitrogen content is that 20.1ppm(is as accompanying drawing 3).These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 3
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 180 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 19.8ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 4
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 35 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 20.4ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 5
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 4 DEG C/min, then rise to 190 DEG C with the speed of 8 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 20.9ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 6
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 30:1; Sample size: 1.0 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 23.1ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 7
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
13X molecular sieve chromatography column length 3m internal diameter 3mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size 0.5mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 18.6ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 8
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 2m internal diameter 3mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 1.8288m internal diameter 3.17mm Stationary liquid is 45 ~ 60 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 20.1ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
embodiment 9
1) reagent and material:
Carrier gas: nitrogen, purity is greater than 99.99%(V/V)
Combustion gas: hydrogen, purity is greater than 99.99%(V/V)
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification.
2) experimental technique and step:
Gas chromatograph: be furnished with a flame ionization ditector and a thermal conductivity detector (TCD) and gas chromatograph with automatic sampling valve
Chromatographic column: HP-AL/S 19091P-S12 25m × 0.32mm × 8 μm capillary chromatograph 1
Porapack Q column length 1.8288m internal diameter 3.17mm Stationary liquid is 80 ~ 100 order packed column 1
5A molecular sieve chromatography column length 3m internal diameter 4mm Stationary liquid is 60 ~ 80 order packed column 1
Concrete steps:
Chromatographic condition sets:
Injector temperature: 100 DEG C
Initial temperature: 40 DEG C, keeps 2min, then rises to 100 DEG C with the speed of 5 DEG C/min, then rise to 190 DEG C with the speed of 10 DEG C/min, keeps 20min; Thermal Conductivity actuator temperature is 200 DEG C, and reference flow is 30mL/min; Flame ionization ditector: temperature is 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 400mL/min, tail wind drift amount 25mL/min.
Split ratio: 20:1; Sample size: 0.5 mL;
Apply this kind of analytical approach to measure the hydrogen sample that refinery unit produces, carry out quantitatively by external standard method respectively to the hydrocarbon impurities in hydrogen and nitrogen, the result obtained be hydrocarbon impurities content in hydrogen for not detect, nitrogen content is 23.5ppm.These data are that the chromatographic work station directly configured by gas chromatograph calculates automatically, for quantitative criterion sample by the certified reference material of purchase Dalian great Te calibrating gas company limited.
Claims (10)
1. one kind is detected the method for hydrogen high purity propylene and nitrogen impurity level simultaneously, it includes gas chromatograph, it is characterized in that: described gas chromatograph is furnished with a flame ionization ditector and a thermal conductivity detector (TCD) simultaneously, chromatographic column adopts two chromatography columns and a capillary chromatographic column; Carrier gas is high-purity hydrogen and high pure nitrogen, operation condition of chromatogram: injector temperature 100 DEG C ~ 200 DEG C, column temperature 35 DEG C ~ 190 DEG C, adopts initial temperature: 35 ~ 40 DEG C, keeps 2 ~ 5min, then 100 DEG C are risen to the speed of 4 ~ 7 DEG C/min, rise to 190 DEG C with the speed of 6 ~ 12 DEG C/min again, keep the temperature programme pattern of 20min, detector temperature is 200 DEG C ~ 300 DEG C, split ratio 10:1 ~ 30:1, for analyzing hydrogen high purity propylene and nitrogen impurity level;
Operation steps is: sample at the scene, under chromatographic column operating conditions, carry out stratographic analysis; Go out peak result according to chromatogram, carry out quantitatively to sample high purity propylene and Nitrogen gas impurity, quantivative approach adopts external standard method; Hydrogen sample feeding amount is 0.5mL ~ 2.0mL;
Above-mentioned high-purity hydrogen is: purity is greater than 99.99%(V/V);
Above-mentioned high pure nitrogen is: purity is greater than 99.99%(V/V).
2. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 1, it is characterized in that: operation condition of chromatogram: injector temperature 100 DEG C, column temperature 40 DEG C ~ 190 DEG C, adopt temperature programme pattern, Thermal Conductivity actuator temperature is 200 DEG C, flame ionization ditector temperature is 300 DEG C, and split ratio is 20:1.
3. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 1, is characterized in that: described chromatography column is porous polymer gas phase packed column and the molecular sieve packed column of stainless steel.
4. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 1, is characterized in that: described capillary chromatographic column is the chromatography on alumina post by sodium sulphate deactivation.
5. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 4, is characterized in that: described capillary chromatographic column is HP-PLOT Al
2o
3/ S.
6. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 3, is characterized in that: described chromatography column is Porapack Q chromatographic column and 5A molecular sieve chromatography post (or 13X molecular sieve chromatography post) respectively; Wherein: Porapack Q column's length 1.5m ~ 2m, internal diameter 3 ~ 4mm, Stationary liquid is 45 ~ 100 object Porapack Q; 5A molecular sieve chromatography post column length 1.5m ~ 3m, internal diameter 3 ~ 4mm, Stationary liquid is 45 ~ 100 object 5A molecular sieve; 13X molecular sieve chromatography post column length 3m, internal diameter 3mm, Stationary liquid is 45 ~ 60 object 13X molecular sieve.
7. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 6, it is characterized in that: described Porapack Q column's length 1.8288m, internal diameter 3.17mm, Stationary liquid is 80 ~ 100 object Porapack Q; Described 5A molecular sieve chromatography post column length 1.8288m, internal diameter 3.17mm, Stationary liquid is 45 ~ 60 object 5A molecular sieve.
8. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 1, it is characterized in that: capillary chromatography column length used is 25m ~ 50m, Stationary liquid thickness of liquid film is 5 μm ~ 15 μm, and internal diameter is 0.25 mm ~ 0.53mm.
9. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 8, is characterized in that: the column length of described capillary chromatographic column is 25m, and Stationary liquid thickness of liquid film is 8 μm, and internal diameter is 0.32mm.
10. the method simultaneously detecting hydrogen high purity propylene and nitrogen impurity level according to claim 1, is characterized in that:
The hydrocarbon impurities that described employing vapor-phase chromatography is analyzed in hydrogen comprises: methane, ethane, ethene, propane, trimethylene, propylene, normal butane, isobutane, Trans-2-butene, butene-1, isobutylene, cis-2-butene, isopentane, n-pentane, 1.3-butadiene, propine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107525879A (en) * | 2017-09-26 | 2017-12-29 | 国网上海市电力公司 | A kind of method of propane content in measure insulating oil |
| CN109374804A (en) * | 2018-10-31 | 2019-02-22 | 内蒙古中煤蒙大新能源化工有限公司 | The chromatogram analysis method of bromopropane product in a kind of production of MTO technology |
| CN110542725A (en) * | 2018-05-29 | 2019-12-06 | 新疆新特新能材料检测中心有限公司 | Process for detecting nitrogen in hydrogen |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107525879A (en) * | 2017-09-26 | 2017-12-29 | 国网上海市电力公司 | A kind of method of propane content in measure insulating oil |
| CN110542725A (en) * | 2018-05-29 | 2019-12-06 | 新疆新特新能材料检测中心有限公司 | Process for detecting nitrogen in hydrogen |
| CN109374804A (en) * | 2018-10-31 | 2019-02-22 | 内蒙古中煤蒙大新能源化工有限公司 | The chromatogram analysis method of bromopropane product in a kind of production of MTO technology |
| CN109374804B (en) * | 2018-10-31 | 2020-11-03 | 内蒙古中煤蒙大新能源化工有限公司 | Chromatographic analysis method for propane product in methanol-to-olefin process production |
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