CN101441203A - Gas chromatography system for measuring gas phase component in fluid inclusion and measuring method thereof - Google Patents
Gas chromatography system for measuring gas phase component in fluid inclusion and measuring method thereof Download PDFInfo
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- CN101441203A CN101441203A CNA2007101780015A CN200710178001A CN101441203A CN 101441203 A CN101441203 A CN 101441203A CN A2007101780015 A CNA2007101780015 A CN A2007101780015A CN 200710178001 A CN200710178001 A CN 200710178001A CN 101441203 A CN101441203 A CN 101441203A
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Abstract
The invention relates to a gas chromatography system for measuring gas phase components in a fluid inclusion, which adopts a modified gas chromatograph to extract trace gas from a small amount of samples (0.1g) of the fluid inclusion for analysis, has high sensitivity and good reproducibility, and can measure H by one-time sample introduction and one-time burst2、O2、N2、CO、CH4、CO2、H2O、C2H2、C2H6、C3H8The content of (2) greatly improves the analysis and test efficiency. In addition, compared with the prior method, the method has the most outstanding characteristic that the absolute content of each component can be obtained besides the relative molar concentration of each component, wherein the real water amount can be combined with the fluid inclusion body fluid phase component to obtain the real concentration of each ion in the fluid inclusion, and the method provides more accurate and direct data for the research of the fluid inclusion.
Description
Technical field
The invention belongs to the application of gas phase chromatographic device in geology mineral gas liquid inclusion composition Study.
Technical background
Fluid inclusion is that diagenesis becomes the ore deposit fluid to be wrapped in mineral lattice defective or the cave nest in the crystallizable mineral growth course, still to seal up for safekeeping in host so far and with host that a part of material of boundary is mutually arranged.By the fluid inclusion composition in the analysis and research mineral, can understand the character and the crystallizable mineral environment of paleocurrent body in depth, review diagenesis and become ore deposit fluid origin and migration path, obtain magma system evolutionary process information and lithosphere-earth mantle interaction information, inquire into the mineral deposit origin cause of formation and and guide the mineral deposit to reconnoitre with becoming the ore deposit environment.
Measure colony's fluid inclusion gas phase composition, state-of-the-art technology adopts the four-electrode spectrum method, see Zhu Heping, Wang Lijuan is at Chinese science, 2001,45 (2): the four-electrode spectrum that 586-590 delivers is measured gas phase composition [J] and the Masakatsu S in the fluid inclusion, Takayuki S, Naoto T.Analysis of FluidInclusion Gases from Inclusion Gases from Gethermal Systems, using aRapid-scanning Quadrupole Mass Spectrometry[J] .Eur J.Mineral, 1992,4:895～906.Employing four-electrode spectrum method not only instrument costs an arm and a leg, and only can obtain the relative volumetric molar concentration of the composition of surveying.Measure colony's fluid inclusion gas phase composition, the general vapor-phase chromatography that adopts more, see Lu Huanzhang, Jiang Bangjie, Sun Xinyi is in geochemistry, 1980, (1): the application [J] of the inorganic gas chromatograph that 106-110 delivers in the gas liquid inclusion composition Study, but method therefor is repeatedly sample introduction, repeated detection, that is to say that could to obtain fluid inclusion respectively by at least two colonies organic, the content of inorganic component, the gas phase composition content that can not really reflect same colony fluid inclusion like this brings uncertainty can for inevitably the explanation of data.Gas phase composition is to use two gas chromatographs in the gas chromatography determination fluid inclusion early.One connects TCD detecting device (connecing drying tube before the post) with the molecular sieve separating column, can measure H
2, O
2, N
2, CO, CH
4Another connects fid detector with Porapak-Q separating column (or GDX separating column), can measure CO
2, H
2O.Do price costliness, organic principle like this and only can obtain CH
4Content and sensitivity low, the most important thing is will could obtain the organic and inorganic components contents of fluid inclusion respectively by two colonies inevitably, this can not really obtain the gas phase composition content of same colony fluid inclusion.The method of utilizing the two-dimensional gas chromatography method to measure the fluid inclusion gas phase composition is not appeared in the newspapers.
Summary of the invention
The present invention adopts the gas chromatograph of process repacking to extract minimum gas from fluid inclusion small amount of sample (0.1g) and analyzes, highly sensitive, favorable reproducibility, and single injected sampling, an explosion can be measured H
2, O
2, N
2, CO, CH
4, CO
2, H
2O, C
2H
2, C
2H
6, C
3H
8Content, improved analytical test efficient greatly.In addition, comparing the most outstanding characteristics with previous methods is, except the relative volumetric molar concentration that can obtain each component, also can obtain its absolute content, the wherein true water yield can combine with the fluid inclusion liquid phase ingredient and obtain the actual concentration of each ion in fluid inclusion, and this will provide more accurate, direct data for Study of fluid inclusions.
Technical scheme of the present invention is a kind of two-dimensional gas chromatography law system of measuring gas phase composition in the fluid inclusion, this system is a gas chromatograph through repacking, it comprises carrier gas 1, gas pressure maintaining valve 2, two six-way valves 3,7, thermal spalling stove 4, two damper tubes 5,9, two chromatographic columns 6,8, TCD detecting device 10, fid detector 11, pressure maintaining valve control device 12 are seen accompanying drawing 1.With TCD detecting device 10 and fid detector 11 series connection, and use two six-way valves 3,7 connect chromatographic column 6 with chromatographic column 8, first six-way valve 3 and second six-way valve 7 have " unlatching ", " closing " two states respectively, when first six-way valve 3 and second six-way valve 7 unlatching, the path of system is: carrier gas 1 → gas pressure maintaining valve 2 → pressure maintaining valve control device 12 → 6 → the second six-way valve 7 → chromatographic columns of first six-way valve 3 → explosion stove 4 → chromatographic column, 8 → TCD detecting device, 10 → fid detector 11.When six-way valve 3,7 cut out, the path of system was: carrier gas 1 → gas pressure maintaining valve 2 → pressure maintaining valve control device 12 → 6 → the second six-way valve 7 → damper tubes of first six-way valve 3 → damper tube 5 → chromatographic column, 9 → TCD detecting device, 10 → fid detector 11.When realizing the gas phase composition content of same colony fluid inclusion, the switching by first six-way valve 3 and second six-way valve 7 measures, described TCD detecting device 10 is a thermal conductivity detector (TCD), fid detector 11 is a flame ionization ditector, TCD detecting device 10 and fid detector 11 are cascaded, and the gas that explosion is come out detects H through the TCD detecting device earlier
2, CO
2, H
2O, O
2, N
2, CO, detect CH through fid detector again
4, C
2H
2, C
2H
6, C
3H
8
Gas chromatograph used in the present invention is the gas chromatograph that adopts thermal conductivity detector (TCD) TCD and/or flame ionization ditector FID, and is concrete as day GC-2010 type gas chromatograph of island proper Tianjin company production.Described thermal spalling stove 4 is the thermal spalling stove of room temperature～1500 ℃ controllable temperature, the thermal spalling stove of room temperature～1000 ℃ controllable temperature more preferably, the PIU-F type thermal spalling stove that concrete as Australian SGE company produces.
The chromatographic column of using among the present invention 6 is energy separation of C H
4, C
2H
2, C
2H
6, C
3H
8Chromatographic column, concrete as the Porapak-Q separating column, specification is 178～250 μ m, 2mm * 2m, chromatographic column 8 is the molecular sieve chromatography post, and specifications such as 4A, 5A, 13X are arranged usually.Be preferably 13X molecular sieve separating column, specification is 178～250 μ m, 2mm * 3m.
The used calibrating gas that is provided by State Standard Matter Research Centre of the present invention is CH
4: 1.05 * 10
4μ L/L; C
2H
2: 50.2 μ L/L; C
2H
6: 77.7 μ L/L; C
3H
8: 78.3 μ L/L; CO
2: 2.08 * 10
4μ L/L; O
2: 2.14 * 10
3μ L/L; N
2: 1.05 * 10
4μ L/L; CO:2.04 * 10
4μ L/L;
The standard water that provides is a Mili-Q water: its specification is resistivity 18M Ω cm.
The two-dimensional gas chromatography law system chromatogram condition of work that the present invention measures gas phase composition in the fluid inclusion is 50 ℃ of column temperatures, 150 ℃ of vaporizer temperature, 150 ℃ of thermal conductivity detector (TCD) TCD temperature, 150 ℃ of flame ionization ditector FID temperature, TCD bridge electric current: 50mA, not split sampling.
Sample pre-treatments
At microscopically, pick out purity greater than 98% quartzy simple ore matter sample 0.5g, granularity 178～250 μ m put into the 100mL beaker, add the 20mL chloroazotic acid, 80～90 ℃ of insulation 3h on electric hot plate.Incline remaining acid and clean with Mili-Q water is washed till the cleansing solution electricity and leads and lead consistently with the Mili-Q water power, and Mili-Q water logging bubble spends the night and is adsorbed on sample surfaces and the intracell remaining acid of sample to remove.The soak solution that inclines adds Mili-Q water, with ultrasonic cleaner ultrasonic cleaning sample number minute, and suction filtration immediately, and with the Mili-Q water washing for several times, sample places porcelain dish, in 80 ℃ of oven dry, it is standby to put into the exsiccator preservation.
Test system purges
Sample after the processing still adsorbs a spot of water and air, influences H
2, O
2, N
2, CO, CO
2, H
2The mensuration of O.After sample is put into the thermal spalling stove, purge test system, under 100 ℃, first six-way valve 3 to be opened, second six-way valve 7 cuts out, and purges 15min.This moment, the test system state was seen accompanying drawing 2.Can observe air and H at chromatographic work station TCD passage
2O goes out the peak and finishes, and thinks that adsorbed water and air caught up with to the greatest extent.
Explosion
When burst temperature is higher than 500 ℃, in the fluid inclusion following reaction may take place:
CH
4+2H
2O＝CO
2+4H
2
CH
4+H
2O＝CO+3H
2
When if if organic component content is high in the fluid inclusion, situation can be complicated more.Therefore not only guaranteeing that the selected burst temperature of the present invention is 500 ℃, and first six-way valve 3 cuts out under the prerequisite that each component can discharge fully but also prevent that subsidiary reaction from taking place, second six-way valve 7 opened, explosion 15min, and this moment, the test system state was seen accompanying drawing 3.
The stratographic analysis flow process
After explosion finished, the stratographic analysis flow process began.
When 0.10min: first six-way valve 3, second six-way valve 7 are all opened, and chromatographic column 6, chromatographic column 8 are separated component successively: H
2, O
2, N
2, CO, this moment, the test system state was seen accompanying drawing 4.
When 1.50min: second six-way valve 7 cuts out, with O
2, N
2, CO is enclosed in the chromatographic column 8.The purpose of doing like this is when passing through chromatographic column 6 (Porapak-Q separating column) owing to sample, O
2, N
2, CO can not separate, and an air peak only can occur, chromatographic column 8 (13X molecular sieve separating column) can be separated O
2, N
2, CO, but back H on the horizon
2O can make chromatographic column 8 lose efficacy CO
2In chromatographic column 8 also irreversible adsorption can take place.Therefore, close second six-way valve 7 through testing selected 1.50min; This moment H
2, CH
4, CO
2Also do not enter chromatographic column 8.
All the other component H
2, CH
4, CO
2, H
2O, C
2H
2, C
2H
6, C
3H
8Go out peak: TCD10 successively and detect H
2, CO
2, H
2O, FID11 detects CH
4, C
2H
2, C
2H
6, C
3H
8, this moment, the test system state was seen accompanying drawing 5.
When 20.0min: second six-way valve 7 opened, and TCD detects O
2, N
2, CO, system status when this moment, the test system state was with 0.10min is seen accompanying drawing 4.
Calibrating gas is analyzed: the chromatographic fractionation figure of standard mixture is seen accompanying drawing 6a, 6b.
Linearity, detection limit and precision
CH in the selected respectively real fluid inclusion
4, C
2H
6, C
3H
8, C
2H
2The linearity of the calibrating gas investigation method of content scope sees Table 1.As seen from Table 1, under optimal experimental conditions, in the scope selected according to each component content scope of actual package body sample, each component concentration and peak area have good linear relationship.Therefore can come contained component concentrations in the quantitative Analysis sample with external standard method.
Under optimal experimental conditions, each component is carried out 6 replicate determinations by the hybrid standard gas 500 μ L of selected concentration, calculates the relative standard deviation (RSD) of its chromatographic peak area, is defined as the detection limit (L of method with 3 times of signal to noise ratio (S/N ratio)s
D).As seen from Table 2, this method has better precision and lower detection limit, and illustration method sensitivity, reliable and stable can satisfy the mensuration requirement of composition in the fluid inclusion preferably.
Description of drawings
Fig. 1 is a gas chromatography system synoptic diagram of the present invention.Among the figure: carrier gas 1, gas pressure maintaining valve 2, two six-way valves 3,7, thermal spalling stove 4, two damper tubes 5,9, two chromatographic columns 6,8, TCD detecting device 10, fid detector 11.
Test system constitutional diagram when Fig. 2 is purging.
Test system constitutional diagram when Fig. 3 is explosion.
Fig. 4 is time examination system status figure for 0.10min.
Fig. 5 is time examination system status figure for 1.50min.
Fig. 6 a, 6b are the chromatographic fractionation figure of standard mixture.
The actual quartz specimen of Fig. 7 a, 7b (XD-15) chromatogram.
Embodiment
The two-dimensional gas chromatography law system that adopts the present invention to measure gas phase composition in the fluid inclusion is tested male village, Euripides stage casing, ridge, Tibet cuproaurite bed Quartz inclusion sample, has listed the male village cuproaurite bed Quartz inclusion sample determination result in Euripides stage casing, ridge, Tibet in table 3, the table 4.Wherein XZ3-16 is gold (silver) polymetallic ore stage quartz vein, and other is copper mine stage quartz vein.The analysis result of table 3, table 4 shows fluid inclusion gas phase constituent basically identical in gold (silver) polymetallic ore stage quartz vein and the copper mine stage quartz vein, but the former CH
4And C
2H
6Content is significantly higher than the latter, CO
2Far below the latter, demonstrate gold (silver) polymetallic ore stage one-tenth ore deposit fluid and be in the more environment of reduction than the copper mine stage.
Listed liquid phase ingredient ion chromatography result in the table 5 with table 3, the same division sample of table 4.The water yield by institute's explosion inclusion in the unit mass sample of gas chromatographic analysis acquisition, can converse the ion concentration in the inclusion solution, result of calculation shows that Xiong Cun mining area inclusion solution total ion concentration is 7.5%～46.2%, the salinity ω (NaCl that the micro-thermometric of single inclusion obtains
Eq) scope is 1.23%～36.61%.Calculating gained result slightly height may be because non-homogeneous catching caused, and do not contain non-homogeneous contribution of catching dissolution of crystals to concentration in the micro-temperature-measuring results of single inclusion, and the ion chromatography the possibility of result contains this part.However, the feasibility that has proved this method of the micro-thermometric of single inclusion dry straightly.In a word, both all as one man demonstrate Xiong Cun and become ore deposit fluid salinity variation range bigger, and fluid system is comparatively complicated, has high salinity fluid end member.The actual quartz specimen of Fig. 7 a, 7b (XD-15) chromatogram.
Table 1 equation of linear regression
Table 2 method precision and detection limit
The gas chromatographic analysis (relative content mol%) of fluid inclusion composition in the vein quartz of table 3 Xiong Cun mining area
Fluid inclusion composition gas chromatographic analysis result in the vein quartz of table 4 Xiong Cun mining area (absolute content μ g/g sample)
Fluid inclusion composition ion chromatography result in the vein quartz of table 5 Xiong Cun mining area
Claims (7)
1, a kind of two-dimensional gas chromatography law system of measuring gas phase composition in the fluid inclusion, it is characterized in that, this system is a gas chromatograph, it comprises carrier gas (1), gas pressure maintaining valve (2), two six-way valves (3,7), thermal spalling stove (4), two damper tubes (5,9), two chromatographic columns (6,8), TCD detecting device (10), fid detector (11), pressure maintaining valve control device (12);
With TCD detecting device (10) and fid detector (11) series connection, and use two six-way valves (3,7) that chromatographic column (6) is connected with chromatographic column (8); First six-way valve (3) and second six-way valve (7) have " unlatching ", " closing " two states respectively, when first six-way valve (3) and second six-way valve (7) unlatching, the path of system is: carrier gas (1) → gas pressure maintaining valve (2) → pressure maintaining valve control device (12) → six-way valve (3) → explosion stove (4) → chromatographic column (6) → six-way valve (7) → chromatographic column (8) → TCD detecting device (10) → fid detector (11); When first six-way valve (3) and second six-way valve (7) when closing, the path of system is: carrier gas (1) → gas pressure maintaining valve (2) → pressure maintaining valve control device (12) → six-way valve (3) → damper tube (5) → chromatographic column (6) → six-way valve (7) → damper tube (9) → TCD detecting device (10) → fid detector (11); When realizing the gas phase composition content of same colony fluid inclusion, the switching by first six-way valve (3) and second six-way valve (7) measures;
Described TCD detecting device (10) is a thermal conductivity detector (TCD), and fid detector (11) is a flame ionization ditector.
2, the two-dimensional gas chromatography law system of gas phase composition in the mensuration fluid inclusion according to claim 1, it is characterized in that, described gas chromatograph is for adopting the gas chromatograph of thermal conductivity detector (TCD) and/or flame ionization ditector, and described thermal spalling stove (4) is the thermal spalling stove of room temperature～1500 ℃ controllable temperature.
3, the two-dimensional gas chromatography law system of gas phase composition in the mensuration fluid inclusion according to claim 2 is characterized in that, described thermal spalling stove (4) is the thermal spalling stove of room temperature～1000 ℃ controllable temperature.
4, the two-dimensional gas chromatography law system of gas phase composition in the mensuration fluid inclusion according to claim 2 is characterized in that, described gas chromatograph is a GC-2010 type gas chromatograph, and described thermal spalling stove (4) is a PIU-F type thermal spalling stove.
5, the two-dimensional gas chromatography law system of gas phase composition in the mensuration fluid inclusion according to claim 1 is characterized in that, chromatographic column (6) is can separation of C H
4, C
2H
2, C
2H
6, C
3H
8Chromatographic column, chromatographic column (8) is the molecular sieve chromatography post.
6, the two-dimensional gas chromatography law system of gas phase composition in the mensuration fluid inclusion according to claim 5 is characterized in that chromatographic column (6) is the Porapak-Q separating column, 178～250 μ m, 2mm * 2m, chromatographic column (8) is a 13X molecular sieve separating column, 178～250 μ m, 2mm * 3m.
7, a kind of with claim 1
-One of 6 described two-dimensional gas chromatography law systems are measured the method for gas phase composition in the fluid inclusion, it is characterized in that, comprise the steps:
(A) sample pre-treatments;
(B) sample introduction and test system purge: the sample after the processing still adsorbs a spot of water and air, influences H
2, O
2, N
2, CO, CO
2, H
2The mensuration of O.After sample is put into the thermal spalling stove, purge test system, under 100 ℃, first six-way valve (3) to be opened, second six-way valve (7) cuts out, and purges 15min, can observe air and H at chromatographic work station TCD passage
2O goes out the peak and finishes, and thinks that adsorbed water and air caught up with to the greatest extent;
(C) explosion: with first six-way valve (3) close, second six-way valve (7) open, burst temperature is 500 ℃, explosion 15min;
(D) stratographic analysis flow process: after explosion finished, the stratographic analysis flow process began;
When 0.10min: first six-way valve (3), second six-way valve (7) are all opened, and chromatographic column (6) and chromatographic column (8) are separated component successively: H
2, O
2, N
2, CO;
When 1.50min: second six-way valve (7) cuts out, with O
2, N
2, CO is enclosed in the chromatographic column (8) all the other component H
2, CH
4, CO
2, H
2O, C
2H
2, C
2H
6, C
3H
8Go out the peak successively: TCD detecting device (10) detects H
2, CO
2, H
2O, fid detector (11) detects CH
4, C
2H
2, C
2H
6, C
3H
8
When 20.0min: second six-way valve (7) opened, and TCD detecting device (10) detects O
2, N
2, CO.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101780015A CN101441203A (en) | 2007-11-23 | 2007-11-23 | Gas chromatography system for measuring gas phase component in fluid inclusion and measuring method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101780015A CN101441203A (en) | 2007-11-23 | 2007-11-23 | Gas chromatography system for measuring gas phase component in fluid inclusion and measuring method thereof |
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|---|---|
| CN101441203A true CN101441203A (en) | 2009-05-27 |
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|---|---|---|---|
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| CN109100413A (en) * | 2018-09-13 | 2018-12-28 | 中国地质科学院矿产资源研究所 | System and method for analyzing carbon and hydrogen isotopes oil-free valve of mineral fluid inclusion |
| CN109060932A (en) * | 2018-09-13 | 2018-12-21 | 中国地质科学院矿产资源研究所 | Carbon and hydrogen isotope analysis system and method for mineral fluid inclusion |
| CN109613160A (en) * | 2018-12-26 | 2019-04-12 | 同济大学 | A headspace gas chromatography system and method for simultaneously analyzing dissolved gas H2/O2/N2/CH4 in seawater |
| CN111624281A (en) * | 2020-06-18 | 2020-09-04 | 长安大学 | Device and method for logging by utilizing rock debris oil gas inclusion |
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| CN115112793A (en) * | 2022-06-20 | 2022-09-27 | 核工业北京地质研究院 | Device and method for online determination of carbon dioxide carbon isotope in inclusion by crushing method |
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