CN105092687A - Rare gas all-component content online analysis method - Google Patents
Rare gas all-component content online analysis method Download PDFInfo
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- CN105092687A CN105092687A CN201510408340.2A CN201510408340A CN105092687A CN 105092687 A CN105092687 A CN 105092687A CN 201510408340 A CN201510408340 A CN 201510408340A CN 105092687 A CN105092687 A CN 105092687A
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Abstract
The invention provides a rare gas all-component content online analysis method. The method includes the following steps: carrying out vacuumization and heating degassing treatment on a main pipeline of a rare gas sample preparation device; connecting an air standard sample to a sample introduction port, vacuumizing a connecting pipeline, and controlling the sample introduction pressure of the air standard sample; purifying the air standard sample, and enriching rare gases; sending the enriched rare gases to quadrupole mass spectrometer, and carrying out a series of analysis calculation; repeating the above operations on a natural gas sample; and obtaining correction values of the rare gas all-component contents in the natural gas sample. The method has the characteristics of simple operation, fast analysis, high reliability, good repeatability, high accuracy and the like, and can provide accurate and reliable parameters for evaluation and utilization of the contents of the rare gas all components of He, Ne, Ar, Kr and Xe.
Description
Technical field
The present invention relates to a kind of rare gas full constituent content on-line analysis, particularly rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis in rock gas, belongs to rock gas experimental analysis technical field in petroleum and gas geology and exploration.
Background technology
Rare gas refers to the group 0 element in the periodic table of elements, mainly comprises He, Ne, Ar, Kr, Xe, Rn, and because Rn is radioelement, geological research only relates to He, Ne, Ar, Kr, Xe usually.Rare gas is because of chemical property torpescence, coefficient of heat conductivity and resistance is little, molten boiling point is low, be easy to the specific physical character such as luminous, has essential industry purposes and using value in the fields such as Aero-Space, atomic energy, low-temperature superconducting, deep diving, laser, electronics, medical science, metallurgy, oil-gas exploration or industry.
Rock gas is one of rare gas essential industry source, to carry out in rock gas rare gas full constituent content analysis for clear and definite rare gas full constituent content population distribution feature, to carry out rare gas industrial utilization significant.At present, in rock gas, rare component analysis is analyzed based on He, Ar, lack full appreciation to rare gas He, Ne, Ar, Kr, Xe full constituent content distribution feature in rock gas, constrain carrying out of rare gas He, Ne, Ar, Kr, Xe full constituent content Comprehensive evaluation and exploitation in rock gas.
Therefore, a kind of rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis is provided to become this area technical matters urgently to be resolved hurrily.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis, the method can provide parameter accurately and reliably for rare gas He, Ne, Ar, Kr, Xe full constituent Content evaluation and utilization in rock gas.
For reaching above-mentioned technical purpose, the invention provides a kind of rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis, it comprises the following steps:
A, utilize the mechanical pump in rare gas sample preparation device, molecular pump and the ionic pump Trunk Line to rare gas sample preparation device to vacuumize, and heating is carried out to zirconium base stove, getter pump and the activated carbon furnace in rare gas sample preparation device to degas process;
B, air standard specimen is connected to the injection port of rare gas sample preparation device, the associated line connected between air standard specimen and rare gas sample preparation device is vacuumized, utilizes sample introduction micrometering valve and film rule to control the sample introduction pressure of air standard specimen;
C, the zirconium base stove in rare gas sample preparation device and getter pump is utilized to comprise hydrocarbon gas, N to air standard specimen
2, O
2, CO
2, H
2s and H
2active gases purify, enrichment rare gas;
D, the rare gas of step c enrichment is sent into level Four mass spectrum analyze, obtain rare gas in air standard specimen respectively
4he,
21ne,
40ar,
84kr,
132the isotope ion signal intensity Ai of Xe, utilizes the internationally recognized value C of rare gas full constituent content in air standard specimen
airin i and air standard specimen, the sample introduction dividing potential drop of rare gas He, Ne, Ar, Kr, Xe, calculates the sensitivity S i of level Four mass spectrum to rare gas He, Ne, Ar, Kr, Xe signal response in air standard specimen respectively, wherein, and described i=He, Ne, Ar, Kr or Xe;
E, according to the method for operating described in steps d, above-mentioned air standard specimen is carried out to the Measurement and analysis of at least 6 sensitivity, obtain the sensitivity mean value S of rare gas He, Ne, Ar, Kr, Xe in described air standard specimen respectively
averagei, described i=He, Ne, Ar, Kr or Xe;
F, to gas samples according to after above-mentioned steps a-c process, the rare gas of enrichment is sent into level Four mass spectrum and analyzes, obtain rare gas in gas samples respectively
4he,
21ne,
40ar,
84kr,
132the isotope ion signal intensity A of Xe
gasi, the sensitivity mean value S of rare gas He, Ne, Ar, Kr, Xe in the air standard specimen utilizing step e to obtain
averagethe sample introduction pressure P of i and gas samples
gas, calculate rare gas full constituent content experiment value C in gas samples
gasi, wherein, described i=He, Ne, Ar, Kr or Xe;
G, according to the method for operating described in step f, 6 these operations are at least repeated to air standard specimen, obtain rare gas full constituent content experiment value C in air standard specimen
airmeasuredi, and be worth C with the internationally recognized of rare gas full constituent content in the air standard specimen described in steps d
airi compares, and obtains correction coefficient Ki, described i=He, Ne, Ar, Kr or Xe;
H, utilize correction coefficient Ki in step g to rare gas full constituent content experiment value C in the gas samples in step f
gasi corrects, and obtains rare gas full constituent normalization value C in gas samples
revisedgasvaluei, completes rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis in gas samples.
In the above-mentioned methods, preferably, in step a, described Trunk Line is evacuated to 10
-7-10
-8the vacuum tightness of Trunk Line (is set to above-mentioned scope, can reduces the impact on rock gas sample such as tube wall adsorbed gas, improve accuracy and the reliability of the analysis data of rock gas sample by Pa.
In the above-mentioned methods, preferably, in step a, describedly heating process of degassing carried out to zirconium base stove, getter pump and the activated carbon furnace in rare gas sample preparation device comprise the following steps: zirconium base stove is warming up to 800 DEG C of heating degas 2-4 hour, be cooled to 350 DEG C for subsequent use; Getter pump is warming up to 400 DEG C of heating 30 minutes, it is for subsequent use to be down to room temperature; Activated carbon furnace is warming up to 400 DEG C of heating 15 minutes, it is for subsequent use to be down to room temperature.
In the above-mentioned methods, preferably, in stepb, described associated line is evacuated to 10
-2pa; The sample introduction pressure of described air standard specimen is 100-1000Pa.
In the above-mentioned methods, preferably, described step c comprises: open zirconium base stove by-pass valve control and comprise hydrocarbon gas, N to air standard specimen
2, O
2, CO
2, H
2s and H
2active gases purify, enrichment rare gas; Then, getter pump by-pass valve control is opened to comprising H
2residual activity gas purify further, enrichment rare gas.
In the above-mentioned methods, preferably, after steps d terminates, before step e starts, also comprise and utilize the molecular pump in rare gas sample preparation device and ionic pump to take out remaining rare gas, and the step of process of degassing is heated according to the method described in step a to zirconium base stove, activated carbon furnace and the getter pump in rare gas sample preparation device.
In the above-mentioned methods, preferably, before step a starts, the step utilizing high-pressure cylinder to be connected to sampled well collection gas samples is also comprised.
In the above-mentioned methods, preferably, when gathering gas samples, also comprise after utilizing rock gas to rinse high-pressure cylinder, gather the step in the stage casing of rock gas continuous flow; More preferably, described washing time is 4-6 time, and total flush time is 10-15 minute.
In the above-mentioned methods, preferably, before utilizing high-pressure cylinder to be connected to sampled well collection gas samples, the step that high-pressure cylinder is vacuumized also is comprised; More preferably, described high-pressure cylinder is evacuated to 10
-3more than Pa.
The rare gas sample preparation device used in the present invention for the existing device in this area, the patent No. of this device is: ZL201010236355.2.
Beneficial effect of the present invention:
Rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis provided by the invention, have simple to operate, analyze quick, reliability is high, reproducible, accuracy high, can provide parameter accurately and reliably for rare gas He, Ne, Ar, Kr, Xe full constituent Content evaluation and utilization in rock gas.
Accompanying drawing explanation
Fig. 1 is the structural representation of rare gas full constituent content on-line analysis device;
Fig. 2 is rare gas He, Ne, Ar, Kr, Xe full constituent content broken line graph in rock gas sample;
Primary clustering symbol description:
1: high-pressure cylinder; 2: air standard specimen; 3: second voltage regulation valve A; 3 ': second voltage regulation valve B; 4: injection port; 5: mechanical pump; 6: film is advised; 7: sample introduction micrometering valve; 8: molecular pump; 9: zirconium base stove; 10: activated carbon furnace; 11: getter pump; 12: ionic pump; 13: sample valve; 14: level Four mass spectrum; 15: computer control system.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment
Present embodiments provide a kind of rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis, it comprises the following steps (the present embodiment adopts the device shown in Fig. 1 to carry out the on-line analysis of rare gas full constituent content):
1) select volume to be the high-pressure cylinder 1 that 0.7L is with bivalve, before sampling, utilize the vacuum equipment such as mechanical pump 5, molecular pump 8 to be evacuated to 10
-3pa;
2) during on-site sampling, high-pressure cylinder 1 is connected to sampled well by Wellhead sampler, with rock gas repeatedly rinse high-pressure cylinder 5 times, rinse about 12 minutes, finally gather the stage casing of continuous flow, complete rock gas sampling when gaseous tension in steel cylinder reaches 4MPa;
3) utilize mechanical pump 5, molecular pump 8 and ionic pump 12 etc. that device Trunk Line is evacuated to 10
-7pa; Zirconium base stove 9 is warming up to 800 DEG C of heating degas 3 hours, be cooled to 350 DEG C for subsequent use; Getter pump 11 is warming up to 400 DEG C of heating 30 minutes, it is for subsequent use to be down to room temperature; Activated carbon furnace 10 is warming up to 400 DEG C of heating 15 minutes, it is for subsequent use to be down to room temperature;
4) the air standard specimen 2 being collected in Changping County, Beijing boa mountain is connected to device injection port 4 by second voltage regulation valve B3 ', 10 are evacuated to associated line
-2pa, controls air standard specimen 2 sample size by sample introduction micrometering valve 7 and film rule 6 and is about 400Pa;
5) by-pass valve control of zirconium base stove 9 is opened to the hydrocarbon gas in air standard specimen, nitrogen (N
2), oxygen (O
2), carbon dioxide (CO
2), sulfuretted hydrogen (H
2and trace hydrogen (H S)
2) isoreactivity gas carries out purification enrichment rare gas;
6) by-pass valve control of getter pump 11 is opened to hydrogen (H
2) etc. residual activity gas carry out further purification and enrichment rare gas;
7) utilize sample valve 13 that the rare gas of purification enrichment in air standard specimen is sent into level Four mass spectrum 14, obtain rare gas
4he,
21ne,
40ar,
84kr,
132xe isotope ion signal intensity Ai, in conjunction with the internationally recognized value C of rare gas full constituent content in air
airi (He:5.24 × 10
-6, Ne:18.18 × 10
-6, Ar:0.934%, Kr:1.14 × 10
-6, Xe:0.087 × 10
-6) and above-mentioned 5 kinds of rare gas dividing potential drop separately, calculate the sensitivity S i (i=He, Ne, Ar, Kr, Xe) of instrument to above-mentioned 5 kinds of rare gas signal responses;
8) utilize molecular pump 8, ionic pump 12 take out remaining rare gas, and to zirconium base stove 9, activated carbon furnace 10, getter pump 11 according to step (3) described method carry out heating degas wait for after process for subsequent use;
9) repeating step 7,8 utilizes air standard specimen 2 to carry out the Measurement and analysis (more than 6 times) of repeatedly sensitivity, obtains the sensitivity mean value S of instrument to rare gas He, Ne, Ar, Kr, Xe respectively
averagei;
10) high-pressure cylinder 1 acquiring rock gas sample is connected with injection port 4 by second voltage regulation valve A3,10 are evacuated to associated line
-2pa, advises by sample introduction micrometering valve 7 and film the sample size that 6 control rock gas sample in high-pressure cylinder 1 according to the method for operating of step (4);
11) by step (5), (6), (8), (10), rare gas purifying, enrichment are carried out to rock gas sample, obtain rare gas in rock gas sample
4he,
21ne,
40ar,
84kr,
132xe isotope ion stream signal intensity A
gasi, the instrument utilizing preceding step (9) to obtain is to the sensitivity mean value S of above-mentioned 5 kinds of rare gas
averagethe sample introduction pressure P of i and rock gas sample
gas, utilize computer control system 15 and self-editing process control and data processing software to calculate rare gas He, Ne, Ar, kr, Xe full constituent content experiment value C in rock gas sample
gasi (i=He, Ne, Ar, Kr, Xe);
12) repeat step (10), (11) to other rock gas sample experiment Analysis, calculate rare gas full constituent content experiment value in rock gas sample;
13) in rock gas sample analysis process, air standard specimen is repeatedly analyzed (more than at least 6 times) according to the rock gas sample analysis method described in step (11), obtain rare gas full constituent content experiment value C in air standard specimen
airmeasuredi, and be worth C with the internationally recognized of rare gas full constituent content in air standard specimen
airi compares, and asks for correction coefficient Ki (i=He, Ne, Ar, Kr, Xe);
14) utilize correction coefficient Ki to rare gas He, Ne, Ar, kr, Xe full constituent content experiment value C in rock gas sample
gasi corrects, and finally can obtain rare gas He, Ne, Ar, kr, Xe full constituent normalization value C in rock gas sample
revisedgasvaluei (i=He, Ne, Ar, Kr, Xe).
Utilize said method to analyze (result is as shown in table 1) rare gas full constituent content in air standard specimen, the rock gas sample in different pound sign is analyzed, and depicts correlation graph (result is as shown in table 2 and Fig. 2).
Table 1 carries out to the air standard specimen being collected in Changping County, Beijing boa mountain the air standard specimen experiment analysis results and percentage deviation thereof that 12 repeatability analyses obtain for the method that utilizes above-described embodiment to provide.As can be seen from Table 1: 12 replicate analysis results of air standard specimen are very close shows that the method has good repeatability; The experimental analysis value of air standard specimen and the internationally recognized value of air standard specimen is very close and percentage deviation is less shows that analysis result has higher accuracy and reliability.
Rare gas full constituent content analysis repeatability tables of data in table 1 air standard specimen
Rare gas full constituent content data table in table 2 gas samples
Rare gas full constituent content value in multiple gas samples that table 2 obtains for the method utilizing above-described embodiment to provide, and itself and the internationally recognized value of air standard specimen content are contrasted, as can be seen from Table 2: the rare gas content data of different regions gas samples differs greatly; In gas samples, He content value is totally relatively higher than air standard specimen content value, and Ne, Ar, Kr, Xe content is totally relative to air standard specimen content value.
Claims (10)
1. rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis, it comprises the following steps:
A, utilize the mechanical pump in rare gas sample preparation device, molecular pump and the ionic pump Trunk Line to rare gas sample preparation device to vacuumize, and heating is carried out to zirconium base stove, getter pump and the activated carbon furnace in rare gas sample preparation device to degas process;
B, air standard specimen is connected to the injection port of rare gas sample preparation device, the associated line connected between air standard specimen and rare gas sample preparation device is vacuumized, utilizes sample introduction micrometering valve and film rule to control the sample introduction pressure of air standard specimen;
C, the zirconium base stove in rare gas sample preparation device and getter pump is utilized to comprise hydrocarbon gas, N to air standard specimen
2, O
2, CO
2, H
2s and H
2active gases purify, enrichment rare gas;
D, the rare gas of step c enrichment is sent into level Four mass spectrum analyze, obtain rare gas in air standard specimen respectively
4he,
21ne,
40ar,
84kr,
132the isotope ion signal intensity Ai of Xe, utilizes the internationally recognized value C of rare gas full constituent content in air standard specimen
airin i and air standard specimen, the sample introduction dividing potential drop of rare gas He, Ne, Ar, Kr, Xe, calculates the sensitivity S i of level Four mass spectrum to rare gas He, Ne, Ar, Kr, Xe signal response in air standard specimen respectively, wherein, and described i=He, Ne, Ar, Kr or Xe;
E, according to the method for operating described in steps d, above-mentioned air standard specimen is carried out to the Measurement and analysis of at least 6 sensitivity, obtain the sensitivity mean value S of rare gas He, Ne, Ar, Kr, Xe in described air standard specimen respectively
averagei, described i=He, Ne, Ar, Kr or Xe;
F, to gas samples according to after above-mentioned steps a-c process, the rare gas of enrichment is sent into level Four mass spectrum and analyzes, obtain rare gas in gas samples respectively
4he,
21ne,
40ar,
84kr,
132the isotope ion signal intensity A of Xe
gasi, the sensitivity mean value S of rare gas He, Ne, Ar, Kr, Xe in the air standard specimen utilizing step e to obtain
averagethe sample introduction pressure P of i and gas samples
gas, calculate rare gas full constituent content experiment value C in gas samples
gasi, wherein, described i=He, Ne, Ar, Kr or Xe;
G, according to the method for operating described in step f, 6 these operations are at least repeated to air standard specimen, obtain rare gas full constituent content experiment value C in air standard specimen
airmeasuredi, and be worth C with the internationally recognized of rare gas full constituent content in the air standard specimen described in steps d
airi compares, and obtains correction coefficient Ki, described i=He, Ne, Ar, Kr or Xe;
H, utilize correction coefficient Ki in step g to rare gas full constituent content experiment value C in the gas samples in step f
gasi corrects, and obtains rare gas full constituent normalization value C in gas samples
revisedgasvaluei, completes rare gas He, Ne, Ar, Kr, Xe full constituent content on-line analysis in gas samples.
2. method according to claim 1, wherein: in step a, described Trunk Line is evacuated to 10
-7-10
-8pa.
3. method according to claim 1, wherein: in step a, describedly heating process of degassing is carried out to zirconium base stove, getter pump and the activated carbon furnace in rare gas sample preparation device comprise the following steps:
Zirconium base stove is warming up to 800 DEG C of heating degas 2-4 hour, be cooled to 350 DEG C for subsequent use; Getter pump is warming up to 400 DEG C of heating 30 minutes, it is for subsequent use to be down to room temperature; Activated carbon furnace is warming up to 400 DEG C of heating 15 minutes, it is for subsequent use to be down to room temperature.
4. method according to claim 1, wherein: in stepb, described associated line is evacuated to 10
-2pa;
The sample introduction pressure of described air standard specimen is 100-1000Pa.
5. method according to claim 1, wherein: described step c comprises:
Open zirconium base stove by-pass valve control and hydrocarbon gas, N are comprised to air standard specimen
2, O
2, CO
2, H
2s and H
2active gases purify, enrichment rare gas;
Open getter pump by-pass valve control to comprising H
2residual activity gas purify further, enrichment rare gas.
6. method according to claim 1, wherein: after steps d terminates, before step e starts, also comprise and utilize the molecular pump in rare gas sample preparation device and ionic pump to take out remaining rare gas, and the step of process of degassing is heated according to the method described in step a to zirconium base stove, activated carbon furnace and the getter pump in rare gas sample preparation device.
7. method according to claim 1, wherein: before step a starts, also comprises the step utilizing high-pressure cylinder to be connected to sampled well collection gas samples.
8. method according to claim 7, wherein: when gathering gas samples, also comprises after utilizing rock gas to rinse high-pressure cylinder, gathers the step in the stage casing of rock gas continuous flow.
9. method according to claim 8, wherein: described washing time is 4-6 time, total flush time is 10-15 minute.
10. the method according to any one of claim 7-9, wherein: before utilizing high-pressure cylinder to be connected to sampled well collection gas samples, also comprise the step that high-pressure cylinder is vacuumized;
Preferably, described high-pressure cylinder is evacuated to 10
-3more than Pa.
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| CN107167510A (en) * | 2017-05-25 | 2017-09-15 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Xe Isotope Analysis Methods and analytical equipment in a kind of methane rich natural gas |
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Application publication date: 20151125 |