CN109406616A - A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite - Google Patents

A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite Download PDF

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CN109406616A
CN109406616A CN201811158308.3A CN201811158308A CN109406616A CN 109406616 A CN109406616 A CN 109406616A CN 201811158308 A CN201811158308 A CN 201811158308A CN 109406616 A CN109406616 A CN 109406616A
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barite
sample
sulfur isotope
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陆珏
陈唯
蒋少涌
赵葵东
皮道会
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China University of Geosciences
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N2001/2893—Preparing calibration standards

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Abstract

The present invention provides a kind of method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite, and steps are as follows: screening YF-2 barite samples, grinding measure sulfur isotope δ in YF-2 barite samples using EA-IRMS method34S value；Take one piece of YF-2 barite samples and one piece of ore sample to be measured that YF-2 barite standard specimen target sample and ore target sample to be measured is made respectively；YF-2 barite standard specimen target sample, which is first measured, using LA-MC-ICP-MS method obtains the first sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32The ratio of S then measures ore target sample to be measured and obtains sulfur isotope in all product of ore target to be measured34S/32The ratio of S, then measure YF-2 barite standard specimen target sample and obtain the second sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32The ratio of S；Sulfur isotope δ in ore sample to be measured is calculated34S value.Method provided by the invention can precisely determine sulfur isotope in sulfate mineral, provide uniform and Matrix Match standard sample for LA-MC-ICP-MS method in-site detecting isotope, and quality when effectively correction measures is discriminated against.

Description

A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite
Technical field
The present invention relates to barite analysis determining technology fields, more particularly to one kind to measure sulphur by standard specimen of YF-2 barite The method of hydrochlorate mineral sulfur isotope.
Background technique
Sulfate is common sulfur-rich mineral, and sulfur isotope composition has many undeveloped potential value information, this A little information facilitate us and understand magma, hydrothermal solution and deposition process.Mine is increasingly interested in recently as geological research Geochemical alteration on object microcell scale, LA-MC-ICP-MS in-site detecting Isotope Analysis Method application are also more and more. This method being used widely in terms of sulfide sulfur isotope, but the research for determining sulphate is compared It is few, one of the main reasons for this is that lacking than more uniform and Matrix Match standard sample.It is first when measuring lightweight with MC-ICP-MS When the isotopics of element, quality discrimination is the important potential error source of accuracy and accuracy.Standard specimen sample cross method (Sample-Standard-Bracketing, SSB) is to be usually used in LA-MC-ICP-MS sulfur isotope quality in recent years to discriminate against school Positive method.SSB method can correct the quality betided in MC-ICP-MS and laser ablation simultaneously and discriminate against.However, this method Generally require the solid standard specimen of suitable Matrix Match.The solid standard specimen can be natural minerals, pressed powder either other Artificial synthesized solid sample.National Institute of Standards and Technology (NIST) and US Geological Survey (USGS) it is artificial Synthesis sulfate sulfur isotope is used in studying previous.However, currently without suitable puritan filler salt electron probe It can be used for sulfur isotope analysis in situ.
Summary of the invention
In view of this, the present invention provides a kind of sides for measuring sulfate mineral sulfur isotope using YF-2 barite as standard specimen Method, this method meet the needs of LA-MC-ICP-MS method analysis sulfate mineral sulfur isotope, bring for numerous analysts It is convenient, while being also to study origin of ore deposit, tracking BIFhosted gold deposit source, look for mine and magmatic evolution etc. to provide advantageous means.
The present invention provides a kind of method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite, including following Step:
S1 screens YF-2 barite samples, and grinding, then measurement obtains sulfur isotope δ in YF-2 barite samples34S value；
S2, take respectively one piece of YF-2 barite samples and one piece of ore sample to be measured be made YF-2 barite standard specimen target sample and Ore target sample to be measured；
S3, measurement YF-2 barite standard specimen target sample obtain the first sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32The ratio of S then measures ore target sample to be measured and obtains sulfur isotope in all product of ore target to be measured34S/32The ratio of S, then Measurement YF-2 barite standard specimen target sample obtains the second sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32The ratio of S；
S4, according to sulfur isotope δ in the YF-2 barite samples34First sample in S value, YF-2 barite standard specimen target sample Point sulfur isotope34S/32Sulfur isotope in the ratio of S, all product of ore target to be measured34S/32The ratio and YF-2 barite standard specimen of S Second sample spot sulfur isotope in target sample34S/32The ratio calculation of S obtains sulfur isotope δ in ore sample to be measured34S value.
Further, in step S1, sulfur isotope δ in YF-2 barite samples is measured34The process of S value are as follows: by YF-2 weight Spar sample is ground to 200 mesh, then weighs YF-2 barite samples and barium sulfate standard sample is individually positioned in tin capsule, to Oxidation catalyst is added in tin capsule, then tin capsule is placed in sample injector by tin capsule closed impaction, by sample injector by tin capsule It puts into combustion reactor, while injecting purity oxygen into combustion reactor, YF-2 barite samples and barium sulfate standard sample It burns in combustion reactor, the gas generated after processing burning, by SO2Gas is separated with other gases, SO2Gas is passed into Measurement obtains sulfur isotope δ in YF-2 barite samples in isotope ratio mass spectrometer34S value.
Further, the oxidation catalyst selects V2O5, by the process of tin capsule closed impaction are as follows: will with curved tweezers Tin capsule is placed on clean flat magnetic sheet, and is allowed to be closed with the side wall of the tweezers gently tight tin capsule of tweezer；By tin capsule side horizontal, with one Tweezers push down its bottom, with the flat horizontal surface of another tweezers suitably firmly scrape tin capsule be allowed to side wall be fully closed into it is flat； Then tin capsule is built up into square or spherical shape, and compressed it.
Further, in step S4, sulfur isotope δ in the ore sample to be measured34The calculation formula of S value are as follows:
In formula, δ34SsampleFor sulfur isotope δ in ore sample to be measured34S value, δ34SYF-2For sulphur in YF-2 barite samples Isotope δ34S value,For sulfur isotope in ore sample target sample to be measured34S/32The ratio of S,For YF-2 barite First sample spot sulfur isotope in standard specimen target sample34S/32The ratio of S and the second sample spot sulfur isotope34S/32The ratio of S is averaged Value.
Further, the ore to be measured includes barite, barytocelestite, celestine and gypsum.
Further, the YF-2 barite samples pick up from Guangxi Yongfu baryte deposit, white or colourless crystal Particle.
Further, in step S3, YF-2 barite standard specimen target sample and ore target sample to be measured are placed on to the sample of laser In product pond, the first sample spot sulfur isotope in plasma mass spectrograph measurement YF-2 barite standard specimen target sample is then utilized34S/32S Ratio, sulfur isotope in all product of ore target to be measured34S/32Second sample spot in the ratio and YF-2 barite standard specimen target sample of S Sulfur isotope34S/32The ratio of S.
Further, the laser is RESOLution laser, the laser parameter of the RESOLution laser Are as follows: laser beam spot diameter is 50 μm, laser energy 8.9Jcm-2, laser frequency 8Hz.
Further, the laser is GeoLasHD laser, the laser parameter of the GeoLasHD laser are as follows: is swashed Light beam spot diameter is 60 μm, laser energy 5Jcm-2, laser frequency 10Hz.
Technical solution provided by the invention has the benefit that method provided by the invention can precisely determine sulfuric acid Salt mineral sulfur isotope provides uniform and Matrix Match standard sample for LA-MC-ICP-MS method in-site detecting isotope, has Effect corrects existing quality when measurement and discriminates against, and YF-2 barite can be used as standard specimen in LA-MC-ICP-MS analysis to correct Other barites, barytocelestite, celestine and gypsum sulfur isotope, be widely used, meet LA-MC-ICP-MS analysis The needs of sulfate mineral sulfur isotope are brought conveniently for numerous analysts, while being also research origin of ore deposit, tracking into mine Fluid origin looks for mine and magmatic evolution etc. and provides advantageous means.
Detailed description of the invention
Fig. 1 is that the present invention is a kind of to be shown by the process of the method for standard specimen measurement sulfate mineral sulfur isotope of YF-2 barite It is intended to.
Fig. 2 is LA-MC-ICP-MS analysis YF-2 barite sulfur isotope result schematic diagram of the present invention.
Fig. 3 is that LA-MC-ICP-MS of the present invention analyzes other barite sulfur isotope result schematic diagrams.
Fig. 4 is that LA-MC-ICP-MS of the present invention analyzes other sulfate sulfur isotope result schematic diagrams.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is further described.
Sulfate mineral sulphur is measured by standard specimen of YF-2 barite referring to FIG. 1, the embodiment provides one kind The method of isotope, comprising the following steps:
Step S1 screens YF-2 barite samples, is ground to 200 mesh or so, then measures YF-2 weight using EA-IRMS method Sulfur isotope δ in spar sample34S value, YF-2 barite samples pick up from Guangxi Yongfu baryte deposit, and white or colourless is big Crystal grain is up to 1 centimetre, and quality is more crisp.
The measurement process of EA-IRMS method are as follows:
It weighs suitable YF-2 barite samples and barium sulfate standard sample is respectively placed in small tin capsule, then into tin capsule The V more than twice is added2O5Powder, V2O5Powder serves as oxidation catalyst；After having weighed sample and oxidation catalyst in tin capsule, Tin capsule is placed on clean flat magnetic sheet with curved tweezers, and gently the tight tin capsule side wall of tweezer is allowed to be closed with tweezers；It is flat with side Tin capsule is set, pushes down its bottom with a tweezers, suitably firmly scraping tin capsule with the flat horizontal surface of another tweezers, to be allowed to side wall complete It is closed into flat；Then tin capsule is built up into small cube or small spherical shape, and compressed it；Then, tin capsule is placed in sample injector In, a tin capsule is put into combustion reactor every time by sample injector, while certain flow is injected into combustion reactor Purity oxygen makes YF-2 barite samples and barium sulfate standard sample burn at 1050 DEG C, the institute then generated after processing burning There is gas (SO2、SO3、SO、H2O、CO2、N2), all gas for generation of burning is brought under helium carrier gas stream and by being filled with height Pure oxygen agent WO3In the single redox quartz ampoule of reducing agent Cu, high-purity oxidant WO3With reducing agent Cu by SO3, SO also It is former and be oxidized to SO2, moisture is by filled with Mg (ClO4)210cm long drier (i.e. water trap) when be removed；Finally, gas Body is heated to 70 DEG C of 50-80 mesh Porapack column for SO by one2With CO2、N2It is separated etc. other gases, by separated SO2It under the drive of helium carrier gas stream, enters in isotope ratio mass spectrometer, obtains sulfur isotope in YF-2 barite samples through measurement δ34S value, 1-3 point of general measure are averaged when measuring at multiple, and sample injector selects 200 autosampler of AS (Fisons Instruments), isotope ratio mass spectrometer select Thermo Fisher Scientific Delta V Plus Isotope ratio mass spectrometer.
YF-2 barite deposit composition granule sample δ34The analysis precision of S is about ± 0.4 ‰ (2s), which is based on repeating Analyze 8557 (δ of NIST SRM34‰) S=21.17 ± 0.09 is obtained with the barium sulfate standard specimen of International Atomic Energy Agency (IAEA) (IAEA-05,δ34S=0.5 ‰ and IAEA-06, δ34S=-34.1 ‰).
In the measurement process of EA-IRMS method, if it is barium-free sulfate sample, sulfur isotope value needs further true It is fixed, barium-free sulfate (celestine, barytocelestite and anhydrite) is first converted into barium sulfate (BaSO4), method particularly includes: it weighs 30mg celestine, barytocelestite and anhydrite are dissolved in 50mmol L-1Diethylene triamine pentacetic acid (DTPA) (DTPA) in, and with HCl acid Change, adjusts pH < 2, be heated to boiling；Then, the 8.5%BaCl of about 25mL is added2Solution makes it sufficiently be precipitated as sulfuric acid Barium.The sulfur isotope value of barite and the barium sulfate of conversion is measured by EA-IRMS, and the long-term reproducibility of measured value is excellent In 0.2 ‰.
Step S2 takes a fritter YF-2 barite samples and fritter ore sample to be measured to be placed in epoxy resin and make respectively At about 1 inch of rounded YF-2 barite standard specimen target sample and ore target sample to be measured.
Step S3, using LA-MC-ICP-MS method to the YF-2 barite standard specimen target sample of step S2 and ore target sample to be measured into The analysis of row original position sulfur isotope, in order to study influence of the matrix effect to result, the present invention uses two in the analysis process A 193nm ArF excimer laser ablation system progress check analysis, respectively RESOLution laser (Resonetics, Canberra, Australia) and GeoLasHD laser (Coherent, German), two laser systems all with Nu Plasma Reception more than II-icp ms (MC-ICP-MS；Nu instruments, Britain) combination, RESOLution Laser, GeoLasHD laser, the instrument setting of plasma mass spectrograph and instrument parameter are shown in Table 1.
Wherein, the laser parameter setting of RESOLution laser are as follows: laser beam spot diameter is 50 μm, corresponding laser energy Amount is 8.9Jcm-2, laser parameter in laser frequency 8Hz, GeoLasHD laser are as follows: laser beam spot diameter is 60 μm, Laser frequency is 10Hz, laser energy 5Jcm-2。
When being measured using LA-MC-ICP-MS method, YF-2 barite standard specimen target sample and ore target sample to be measured are placed on In the sample cell of RESOLution laser and GeoLasHD laser, YF-2 barite standard specimen target sample and ore target sample quilt to be measured Laser distinguishes calcination into aerosol, and aerosol is under the current-carrying of high-purity He gas, with Ar gas and a small amount of N2Gas mixing after enter etc. from Daughter mass spectrograph measures, and first measures YF-2 barite standard specimen target sample and obtains the first sample spot in YF-2 barite standard specimen target sample Sulfur isotope34S/32Then the ratio of S measures ore target sample to be measured and obtains sulfur isotope in all product of ore target to be measured34S/32S Ratio, then measure YF-2 barite standard specimen target sample and obtain the second sample spot sulfur isotope in YF-2 barite standard specimen target sample34S /32The ratio of S, the present invention measure simultaneously34S、33S and32The ion signal of S obtains under the mode of time resolution analysis (TRA) Obtain data.Each sample acquisition includes the washing time for degrading data acquisition and 50s of the background measurement of 30s, 40s.32The back of S Scape intensity is 0.2-0.5V, according to laser ablation beam spot size, the difference of laser frequency and laser intensity, the signal strength of sample For 3-25V, ore sample to be measured measures 5 points or so, and YF-2 barite generally measures 1-3 point every time, when measuring at multiple, It is averaged respectively.
Ore sample to be measured includes barite, barytocelestite, celestine and gypsum.
The instrument parameter of 1 RESOLution laser of table, GeoLasHD laser and plasma mass spectrograph is arranged
Step S4, sulfur isotope δ in the YF-2 barite samples obtained according to step S1 measurement34S value, step S3 are measured To YF-2 barite standard specimen target sample in the first sample spot sulfur isotope34S/32Sulphur is same in the ratio of S, all product of ore target to be measured Position element34S/32Second sample spot sulfur isotope in the ratio and YF-2 barite standard specimen target sample of S34S/32The ratio calculation of S obtain to Survey sulfur isotope δ in ore mineral particle34S value；
Sulfur isotope δ in ore sample to be measured34The calculation formula of S value are as follows:
In formula, δ34SsampleFor sulfur isotope δ in ore sample to be measured34S value, δ34SYF-2For sulphur in YF-2 barite samples Isotope δ34S value,For sulfur isotope in ore sample target sample to be measured34S/32The ratio of S,For YF-2 barite First sample spot sulfur isotope in standard specimen target sample34S/32The ratio of S and the second sample spot sulfur isotope34S/32The ratio of S is averaged Value.
The same position of sulfate mineral sulphur is measured by standard specimen of YF-2 barite to provided by the invention below with reference to verification test The accuracy of the method for element is illustrated.
Verification test 1:
Using isotope uniform and Matrix Match normative mineral to the sulfur isotope of SSB method in-site detecting barite especially It is important.In order to verify potential sulfate standard sample sulfur isotope homogeneity and reproducibility (LA-MC-ICP-MS and EA- IRMS), the present invention carries out replicate analysis to the sulfur isotope of YF-2 barite samples.For EA-IRMS method, reproducibility is measured Refer to the consistency for the result for taking different piece to carry out multiple measurement from bulk sample.The present invention repeats to have surveyed YF-2 in CAS Three times, sulfur isotope value is 18.31 ± 0.06 ‰ (2s) to the sub-fraction sample of barite；YF-2 barite has been surveyed in CUG 11 different pieces, obtain sulfur isotope average value be 18.1 ± 0.4 ‰ (2s), the result measured respectively in two units It is consistent in range of uncertainty.In addition to this, the present invention determines the δ of YF-2 barite also by LA-MC-ICP-MS34S Value, the interior result measured is as shown in Table 2 and Fig. 1 in different times, and table 2 is the sulfur isotope value of different minerals sulfate, Fig. 2 YF-2 barite sulfur isotope is analyzed as a result, can be seen that the δ of YF-2 barite from table 2 and Fig. 2 for LA-MC-ICP-MS method34S Value is 18.0 ± 0.4 ‰ (2s), uncertainty < 0.5 ‰ (2s), and the solid line in Fig. 2 indicates average value.
In conclusion either EA-IRMS method either LA-MC-ICP-MS method, i.e. complete analysis or microcell scale, YF-2 The sulfur isotope of barite shows good homogeneity.Therefore, YF-2 barite can be used as LA-MC-ICP-MS analysis The standard specimen of the sulfur isotope of other barite samples can be used as a new sulfur isotope standard specimen.
The sulfur isotope value of 2 sulfate of table
In table 2, number is YF-1 and the barite of YF-2 picks up from Yongfu (Guangxi) baryte deposit, and the weight that number is WC is brilliant Stone picks up from Wu Chuan (Guizhou) hydrothermal deposit, and the barite of Yongfu YF-1, Yongfu YF-2 and river WC hydrothermal deposit of being engaged in is white or nothing The big crystal grain (being up to 1 centimetre) of color, quality is more crisp；Number is DGD and the barite of GTS picks up from Mianning-Dechang carbonatite Granitic Complex (Sichuan), Mianning-Dechang rare earth mineral deposit DGD and GTS barite contain a small amount of fluorite in light yellow；Number is DSG Barytocelestite pick up from Huanglong paving carbonic acid lithotype rare earth-molybdenum deposit (Shaanxi), barytocelestite DSG be in light brown rhomboidan, matter Brittleness；The celestine that number is BK picks up from Bayan Khushu rare earth mineral deposit, and celestine BK is light blue color；The admant that number is LX Cream picks up from Hubei Ling Xiang iron ore-deposit, and clever township's anhydrite LX is colourless transparent crystal.
Verification test 2:
In LA-MC-ICP-MS analytic approach, in order to verify the applicability of YF-2 barite standard specimen, with YF-2 barite work For standard specimen, using SSB method, to correct the more uniform barite samples of other sulfur isotope ratios (YF-1, DGD and GTS barite), Fig. 3 is that LA-MC-ICP-MS method analyzes other barite sulfur isotope result schematic diagrams, the analysis of YF-1, DGD and GTS barite It the results are shown in Table 2 and Fig. 3 A, 3B, 3C.The result of LA-MC-ICP-MS measurement is consistent with EA-IRMS measurement result, analysis essence Degree is 0.5 ‰.In addition, according to EA-IRMS measurement as a result, discovery WC barite samples sulfur isotope value change greatly, because This also demonstrates its variation on microcell scale, using YF-2 barite as standard specimen, with LA-MC-ICP-MS to the same position of its sulphur Element is measured, and as the result is shown in a small region, sulfur isotope is varied widely, obtained value difference 4 ‰ (see Fig. 3 D and 3E), and what is measured with traditional EA-IRMS analysis method is an average value.Therefore, the advantage of micro-region analysis technique Obviously.
In order to study the matrix effect between different sulfate, standard specimen is made with YF-2 barite, to measure other sulfate The sulfur isotope of (DSG barytocelestite, BK celestine and LX anhydrite) finds the sulphur between YF-2 barite and these sulfate Isotope fractionation be it is negligible, LA-MC-ICP-MS measurement result and EA-IRMS measurement result are in error range It is consistent, is shown in Table 2 and Fig. 4, wherein Fig. 4 is that LA-MC-ICP-MS analyzes other sulfate sulfur isotope result schematic diagrams, figure 4A is DSG sulfur isotope result schematic diagram, and Fig. 4 B is BK sulfur isotope result schematic diagram, and Fig. 4 C is the signal of LX sulfur isotope result Figure.It can be seen that YF-2 barite can also serve as other sulfate sample sulfur isotope measurement standard specimens, the scope of application is non- Normal is wide.
Solid line in Fig. 3 and Fig. 4 indicates average value.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (9)

1. a kind of method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite, which is characterized in that including following Step:
S1 screens YF-2 barite samples, and grinding, then measurement obtains sulfur isotope δ in YF-2 barite samples34S value；
S2 takes one piece of YF-2 barite samples and one piece of ore sample to be measured that YF-2 barite standard specimen target sample and to be measured is made respectively Ore target sample；
S3, measurement YF-2 barite standard specimen target sample obtain the first sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32S Ratio, then measure ore target sample to be measured and obtain sulfur isotope in all product of ore target to be measured34S/32The ratio of S, then measure YF-2 barite standard specimen target sample obtains the second sample spot sulfur isotope in YF-2 barite standard specimen target sample34S/32The ratio of S；
S4, according to sulfur isotope δ in the YF-2 barite samples34First sample spot sulphur in S value, YF-2 barite standard specimen target sample Isotope34S/32Sulfur isotope in the ratio of S, all product of ore target to be measured34S/32The ratio and YF-2 barite standard specimen target sample of S In the second sample spot sulfur isotope34S/32The ratio calculation of S obtains sulfur isotope δ in ore sample to be measured34S value.
2. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as described in claim 1, feature It is, in step S1, measures sulfur isotope δ in YF-2 barite samples34The process of S value are as follows: grind YF-2 barite samples To 200 mesh, then weighs YF-2 barite samples and barium sulfate standard sample is individually positioned in tin capsule, oxygen is added into tin capsule Change catalyst then tin capsule is placed on tin capsule closed impaction in sample injector to, tin capsule is put by combustion reaction by sample injector In device, while purity oxygen is injected into combustion reactor, YF-2 barite samples and barium sulfate standard sample are in combustion reactor Middle burning, the gas generated after processing burning, by SO2Gas is separated with other gases, SO2Gas is passed into isotope ratio mass spectrum Measurement obtains sulfur isotope δ in YF-2 barite samples in instrument34S value.
3. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as claimed in claim 2, feature It is, the oxidation catalyst selects V2O5, by the process of tin capsule closed impaction are as follows: tin capsule is placed in cleaning with curved tweezers On flat magnetic sheet, and it is allowed to be closed with the side wall of the tweezers gently tight tin capsule of tweezer；By tin capsule side horizontal, its bottom is pushed down with a tweezers Portion, with the flat horizontal surface of another tweezers suitably firmly scrape tin capsule be allowed to side wall be fully closed into it is flat；Then tin capsule is folded At square or spherical shape, and compress it.
4. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as described in claim 1, feature It is, in step S4, sulfur isotope δ in the ore sample to be measured34The calculation formula of S value are as follows:
In formula, δ34SsampleFor sulfur isotope δ in ore sample to be measured34S value, δ34SYF-2For the same position of sulphur in YF-2 barite samples Plain δ34S value,For sulfur isotope in ore sample target sample to be measured34S/32The ratio of S,For YF-2 barite standard specimen First sample spot sulfur isotope in target sample34S/32The ratio of S and the second sample spot sulfur isotope34S/32The average value of the ratio of S.
5. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as described in claim 1, feature It is, the ore to be measured includes barite, barytocelestite, celestine and gypsum.
6. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as described in claim 1, feature It is, the YF-2 barite samples pick up from Guangxi Yongfu baryte deposit, white or colourless crystal grain.
7. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as described in claim 1, feature It is, in step S3, YF-2 barite standard specimen target sample and ore target sample to be measured is placed in the sample cell of laser, it is then sharp With the first sample spot sulfur isotope in plasma mass spectrograph measurement YF-2 barite standard specimen target sample34S/32The ratio of S, mine to be measured Sulfur isotope in all product of stone target34S/32Second sample spot sulfur isotope in the ratio and YF-2 barite standard specimen target sample of S34S/32S Ratio.
8. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as claimed in claim 7, feature It is, the laser is RESOLution laser, the laser parameter of the RESOLution laser are as follows: laser beam spot is straight Diameter is 50 μm, laser energy 8.9Jcm-2, laser frequency 8Hz.
9. the method for measuring sulfate mineral sulfur isotope as standard specimen using YF-2 barite as claimed in claim 7, feature It is, the laser is GeoLasHD laser, the laser parameter of the GeoLasHD laser are as follows: laser beam spot diameter is 60 μm, laser energy 5Jcm-2, laser frequency 10Hz.
CN201811158308.3A 2018-09-30 2018-09-30 A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite Pending CN109406616A (en)

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CN112730594A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for determining sulfur isotope of cultivated landscape plant and application
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CN113087007A (en) * 2021-02-25 2021-07-09 广州海洋地质调查局 Device for extracting protogenic carbonate crystal lattice sulfate in carbonate rock
CN114994163A (en) * 2022-06-10 2022-09-02 贵州大学 Method for judging position of barite deposition center by using sulfur isotope value

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CN111638266A (en) * 2020-07-09 2020-09-08 中国测试技术研究院化学研究所 ICP-MS detection method for measuring total sulfur in natural gas based on constant-current control sample injection device
CN111638266B (en) * 2020-07-09 2024-03-29 中国测试技术研究院化学研究所 ICP-MS detection method for measuring total sulfur in natural gas based on constant-current control sample injection device
CN112730585A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for detecting sulfur stable isotope in sulfur monoxide mode
CN112730580A (en) * 2021-01-18 2021-04-30 天津师范大学 Surface water sulfur stable isotope analysis technology and application
CN112730578A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for detecting wetland plant sulfur stable isotope in sulfur monoxide mode
CN112730583A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for analyzing sulfur isotope in sulfate of civil engineering drainage system
CN112730587A (en) * 2021-01-18 2021-04-30 天津师范大学 Tracing method for sulfur element in sludge in river engineering and application
CN112730579A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for detecting sulfur stable isotope of Jinjiang No. 1 garlic
CN112730594A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for determining sulfur isotope of cultivated landscape plant and application
CN112730590A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for detecting sulfur stable isotope in water sample of landscape river
CN112730576A (en) * 2021-01-18 2021-04-30 天津师范大学 Method for detecting stable isotope of garlic sulfur in tissue culture of rachis
CN112730581A (en) * 2021-01-18 2021-04-30 天津师范大学 Sulfur monoxide ion method for detecting sulfur stable isotope in atmosphere
CN113087007A (en) * 2021-02-25 2021-07-09 广州海洋地质调查局 Device for extracting protogenic carbonate crystal lattice sulfate in carbonate rock
CN114994163A (en) * 2022-06-10 2022-09-02 贵州大学 Method for judging position of barite deposition center by using sulfur isotope value

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