30 results about "Sulphur isotope" patented technology

The invention relates to the field of element isotope analysis, and particularly discloses an element isotope analysis system, an analysis method of sulfur isotopes in a trace sulfate sample and application of the analysis method. The system comprises an element analyzer, an enrichment device, a gas chromatographic column, an isotope ratio mass spectrometer and a heating device which are connectedin sequence, and pipelines for connecting or communicating equipment, wherein the pipeline used for connecting or communicating the equipment is a Teflon pipe, the gas chromatographic column is a chromatographic column made of a Teflon material, the enrichment device comprises a multi-way valve, a sample tube and a cooling trap, at least one part of the sample tube can be arranged in the coolingtrap to realize enrichment, and the heating device is arranged around the sample inlet, the sample inlet valve and the ion source of the isotope ratio mass spectrometer. The analysis method is simple,controllable, easy to operate, capable of utilizing the sample to the maximum extent, low in instrument detection limit, high in sensitivity, small in analysis error and high in accuracy.

The invention relates to an analysis system and an analysis method for trace sulfur isotopes in sulfide and sulfate, belongs to the technical field of stable isotope testing, and solves the problems that an existing analysis method is large in sample consumption, low in analysis efficiency and high in consumable cost and cannot realize analysis and testing of the sulfur isotopes in the trace sulfide and sulfate. The analysis system and an analysis method for trace sulfur isotopes in sulfide and sulfate comprises an element analyzer, a gas pre-concentration and purification device and a mass spectrometer; the gas pre-concentration and purification device is used for enriching and purifying SO2 gas, one end of the gas pre-concentration and purification device is connected with the element analyzer, and the other end of the gas pre-concentration and purification device is connected with the mass spectrometer through a universal interface. The system and method have the advantages of smallsample consumption, high analysis efficiency, low consumable cost, realization of analysis and test of sulfur isotopes in trace sulfides and sulfates, analysis precision superior to 0.20% o (1 sigma), and reaching of the advanced level of international similar laboratories.

The invention discloses an ultramicro sulfur isotope analysis system and an ultramicro sulfur isotope analysis method, belongs to the technical field of stable isotope test, and solves the problems oflarge sample consumption, low actual sample utilization rate, high consumable cost and incapability of realizing ultramicro sulfur isotope analysis test in the conventional analysis method. The ultramicro sulfur isotope analysis system comprises an element analyzer, a first gas pre-concentration and purification device, a chromatographic column, a second gas pre-concentration and purification device and a mass spectrometer, wherein the element analyzer is connected with the first gas pre-concentration and purification device, the first gas pre-concentration and purification device is connected with the second gas pre-concentration and purification device through a chromatographic column, and the second gas pre-concentration and purification device is connected with the mass spectrometer through a universal interface. The method has the advantages of less sample consumption, high analysis efficiency, low consumable cost, realization of ultramicro sulfur isotope analysis test, analysisprecision superior to 0.40% o (1 sigma), and reaching of the advanced level of international similar laboratories.

The invention discloses a method for analyzing sulfate sources in atmospheric particulate matter based on sulfur isotopes. The method comprises the following steps that (1) emission sources and winterambient air PM2.5 samples are collected; (2) sulfur isotope compositions in the samples are detected through an MAT-253 isotope mass spectrometer, and an ion chromatograph is used for analyzing ioniccomponents in soil raised-dust particles, biomass combustion emission particles and atmospheric particles; (3) a potential aerosol mass (PAM) is used for studying the sulfur isotope distillation characteristics in the process that SO2 is oxidized into SO4<2->; and (4) on the basis of the step (1) to step (3), the method for analyzing the sulfate sources in the atmospheric particulate matter basedon the sulfur isotopes is established, and primary emission contributions of fire coal and soil raised dust and contributions of fire coal, motor vehicle and biomass combustion emission on secondarysulfate are analyzed. The method has the important scientific significance and important application and promotion value, the new idea is developed for analyzing and studying the atmospheric particulate matter, and the new method is established for analyzing and studying the source of the atmospheric particulate matter.

The invention discloses a method and device for dividing natural gas sources through sulfur isotopes, a medium and electronic equipment. The method comprises the steps that the sulfur isotopes of a rock sample containing an evaporation rock stratum and the carbon isotopes and the oxygen isotopes of a carbonate rock sample adjacent to the rock sample containing the evaporation rock stratum are obtained; based on the carbon isotope, the oxygen isotope, the international geological carbon isotope curve and the international geological oxygen isotope curve, determining the geological age to which the evaporation rock-containing stratum belongs; obtaining the sulfur isotope of the natural gas; and based on the sulfur isotope of the natural gas and the sulfur isotope of the rock sample of the evaporation rock-containing stratum, determining the geological age of natural gas formation. According to the method, the geological age of the evaporation rock stratum is determined through the carbon isotope and the oxygen isotope of the carbonate rock sample adjacent to the rock sample containing the evaporation rock stratum, the sulfur isotope of the natural gas is compared with the sulfur isotope of the rock sample in the evaporation rock stratum, and the geological age formed by the natural gas, namely the source of the natural gas, can be obtained.

The invention discloses a method for judging the source rock age of petroleum by comparing sulphur isotopes of evaporite and petroleum. The method includes the following steps: S101. acquiring a sulfate sample in an evaporite formation and performing sulphur isotope analysis to obtain sulphur isotope data of the evaporite formation; S102. acquiring a carbon isotope sample in a carbonate formationinterbeded with the evaporite formation and analyzing oxygen and carbon isotopes, and then carrying out carbon isotope stratigraphic study to determine the geologic age of the evaporite; S103. completing the international sulfur isotope curve based on the sulphur isotope data of the evaporite formation and the geologic age of the evaporite; S104. analyzing sulfur isotopes in petroleum to obtain sulfur isotope data in the petroleum; and S105. comparing the sulfur isotope data in the petroleum with the sulfur isotope data of the evaporite formation and judging the source rock age of the petroleum according to the international sulfur isotope curve.

The invention discloses a method and a device for analyzing sulfur isotopes of a plurality of single sulfur-containing compounds in crude oil. The method comprises the following steps: after a crude oil sample is vaporized and separated by a gas chromatograph, the crude oil sample and gas of a sulfur-containing standard sample enter a multi-receiving inductively coupled plasma mass spectrometer together to analyze sulfur isotopes; a ratio of the signal intensities of 34S to 32S in the sulfur-containing standard sample and a ratio of the signal intensities of 34S to 32S in different single sulfur-containing compounds in the crude oil sample are analyzed, so as to obtain an isotope ratio of the sulfur elements in different single sulfur-containing compounds. The method is used for simultaneously analyzing sulfur isotopes of a plurality of single sulfur-containing compounds in crude oil by combining a gas chromatograph with an inductively coupled plasma mass spectrometer (ICPMS). According to the method disclosed by the invention, the precision of analyzing the sulfur isotope values of a plurality of single sulfur-containing compounds in the petroleum is 0.01%, and the lower limit ofdetection of the sulfur element is 40pmol / L.

The invention belongs to the technical field of isotope analysis and detection, and relates to a device for detecting sulfur isotopes in gas in a continuous flow mode. The device comprises a gas storage tank for storing a gas sample, a cold trap, an element instrument, an isotope mass spectrometer, a first helium conveying pipeline, a second helium conveying pipeline, a first gas inlet pipeline, an emptying pipeline, an oxygen conveying pipeline and a second gas inlet pipeline; the elemental instrument comprises an automatic solid sample injector, a combustion furnace and a reduction furnace;the first helium conveying pipeline, the gas storage tank, the cold trap, the first gas inlet pipeline, the combustion furnace, the reduction furnace, the second gas inlet pipeline and the isotope mass spectrometer are sequentially communicated; the cold trap is communicated with an emptying pipeline; the second helium conveying pipeline is communicated with the gas inlet end of the cold trap; andthe oxygen conveying pipeline is communicated with the combustion furnace. According to the device, a gas sample does not need to be pretreated, and the sulfur isotope in the gas sample can be calibrated by utilizing the solid standard substance.

The invention discloses a method for detecting sulfur stable isotopes in a surface water sample in an SO+ mode, which comprises the following specific steps: filtering, acidifying, precipitating and evaporating the surface water sample to dryness, filling in a tin cup, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. According to the method, SO+ is generated by utilizing the secondary ionization effect of the ion source high-energy electron flow on SO2+, and the SO+ ion beam is separated and tuned by optimizing the voltage of the quadrupole, so that the sulfur isotope ratio of the surface water sample is efficiently and accurately analyzed, the result precision is high, the repeatability is good, and the operation is easy.

The invention relates to a method for detecting sulfur isotopes in sulfate for experimental teaching management, and discloses a method for detecting sulfur stable isotopes in a water sample for experimental teaching in an SO+ mode, which comprises the following specific steps: filtering, acidifying, precipitating and evaporating the water sample for experimental teaching to dryness, filling a tin cup with the water sample, and wrapping; and detecting the sample to be detected by adopting an element analyzer stable isotope mass spectrometer. According to the invention, the secondary ionization effect of the ion source high-energy electron flow on SO2+ is utilized to generate SO+ to carry out sulfur isotope detection, so that accurate, efficient and comprehensive management of the water sample for experiment teaching is realized.

The invention discloses an elemental analysis-mass spectrometry combined system and a method for testing trace sulfur isotopes. The elemental analysis-mass spectrometry combined system comprises an elemental analyzer, a chromatographic column and a stable isotope ratio mass spectrometer, the element analyzer comprises an automatic sample introduction disc, an oxidation furnace, a reduction furnace and a water removal trap which are connected in sequence; an oxidation reduction pipe in the oxidation furnace adopts a reducing structure, and the inner diameter of an upper pipe is larger than that of a middle pipe and is larger than that of a lower pipe; the inner diameter of an oxygen balance pipe in the reduction furnace does not exceed 4mm; and the inner diameter of the water removal trap does not exceed 4mm, the water removal trap is arranged between the oxygen balance pipe and the chromatographic column, and the output end of the chromatographic column is connected with the stable isotope ratio mass spectrometer. According to the invention, the inner diameters of the oxidation tube, the reduction tube, the water removal tube and the chromatographic column are optimized, the flow velocity of the carrier gas is reduced, and the dilution ratio of the carrier gas to the target gas is reduced under the condition that the peak shape coefficient is basically unchanged, so that the purpose of testing the trace sulfur isotope is realized, and the corrosion strength of sulfur dioxide to the whole system pipeline is reduced.

The invention provides a preparation method of an organic sulfur isotope detection sample. The preparation method comprises the following steps: (1) converting organic sulfur in an organic matter rawmaterial into barium sulfate; (2) enabling the barium sulfate to react in solid acid phosphate and hydroiodic acid to generate hydrogen sulfide gas; (3) moving out the hydrogen sulfide gas and absorbing the hydrogen sulfide gas by an alkaline solution to obtain an absorption solution; and (4) adding a silver salt solution into the absorption solution to convert the sulfur in the absorption solution into silver sulfide precipitates. The invention also provides a method for detecting an organic sulfur isotope in the organic matter raw material. The detection method comprises the steps of preparing the detection sample according to the preparation method, and detecting the sample by adopting an SF6 method.

The invention discloses a method for detecting sulfur isotopes in urban landscaping engineering cultivation soil, which comprises the following specific steps: drying, grinding and filtering a landscaping engineering cultivation soil sample by a screen, filling a tin cup with the sample, wrapping the tin cup, and detecting a sample to be detected by using an element analyzer- stable isotope mass spectrometer. The secondary ionization effect of high-energy electron flow on SO2+ is realized by tuning the voltage of the ion source half plate and the electron bombardment source, and SO+ is generated for sulfur isotope detection, so that the sulfur isotope ratio detection accuracy and the analysis efficiency of the greening engineering cultivation soil sample are improved.

The invention provides a method for extracting natural gas hydrate associated authigenic carbonate rock lattice sulfate. The extraction method can be used for extracting the authigenic carbonate rock lattice sulfate in the natural gas hydrate associated authigenic carbonate rock sample, and is simple to operate and high in extraction precision. The method can be widely applied to various technical fields in which authigenic carbonate rock lattice sulfate needs to be extracted from natural gas hydrate associated authigenic carbonate rock samples. The extracted sulfur isotope in the authigenic carbonate rock lattice sulfate can be used for indicating the sulfur isotope of seawater sulfate in the hydrate formation period or the sulfur isotope of pore water in the mineralization period, so that the formation periods of different authigenic carbonate rock minerals can be divided, and the mineralization period of the natural gas hydrate can be judged.

The invention discloses a method for detecting sulfur stable isotope of Jinjiang No.1 garlic in an SO+ mode, which comprises the following specific steps: drying, grinding and filtering a Jinjiang No.1 garlic bulb sample by a screen, filling into a tin cup, wrapping, and detecting a sample to be detected by adopting an element analyzer- stable isotope mass spectrometer. The secondary ionization effect of high-energy electron flow on SO2+ is realized by tuning the half-plate voltage of the ion source and the pressure of the carrier gas, and SO+ is generated for sulfur isotope detection, so that the efficiency and precision of the sulfur isotope ratio of Jinjiang No.1 garlic are improved, the result reproducibility is good, the accuracy is high, and the operation is simple and convenient.

The invention discloses a technology for detecting sulfur stable isotope of root tip meristem culture garlic in an SO+ mode, which comprises the following specific steps: drying, grinding and filtering a root tip meristem culture garlic bulb sample by using a screen, filling into a tin cup, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. According to the method, secondary ionization and efficient separation of high-energy electron flow to SO2+ are realized by utilizing parameters of the tuning ion source ion lens and the quadrupole mass analyzer, so that the requirement of rapid and accurate detection of the sulfur isotope ratio of the root apex meristem culture garlic is perfected, and the detection result is high in accuracy, good in reproducibility and easy to operate and maintain.

The invention discloses a method for judging the age of petroleum source rocks by comparing evaporite and petroleum sulfur isotopes, comprising the following steps: S101, collecting sulfate samples in evaporite strata and performing sulfur isotope analysis to obtain the sulfur isotope of evaporite strata Data; S102. Collect carbon isotope samples in carbonate strata interbedded with evaporite strata and conduct carbon and oxygen isotope analysis, and then conduct carbon isotope stratigraphic studies to determine the geological age of evaporites; S103. Based on evaporation Sulfur isotope data of rock formations and the geological age of evaporite rocks to improve the international sulfur isotope curve; S104. Analyze sulfur isotope in oil and obtain sulfur isotope data of oil; S105. Combine sulfur isotope data of oil with sulfur isotope data of evaporite formations For comparison, and combined with the international sulfur isotope curve to determine the geological age of petroleum source rocks.

The invention discloses a method for generating SO+ by utilizing secondary ionization of an isotope mass spectrum ion source so as to accurately and efficiently detect sulfur stable isotopes in a cultivated landscape plant sample, which comprises the following specific steps: drying, grinding and filtering the cultivated landscape plant sample by a screen, filling a tin cup with the dried and ground cultivated landscape plant sample, and wrapping; and detecting the sample to be detected by adopting an element analyzer stable isotope mass spectrometer. High voltage of the tuning ion source and filament voltage are utilized to generate high-energy electron flow to perform secondary ionization on SO2+, SO+ is generated to perform sulfur isotope detection, and the result shows that the precision is high, the repeatability is good, and the analysis and test efficiency is high.

The invention provides a method for distinguishing late Neoproterozoic and cambrian period stratums. The method comprises the following steps: S1, sampling a plurality of stratum rocks in a target area; S2, separating out a corresponding gypsum sample in the rock; Ss3, performing sulfur-oxygen isotope analysis on sulfate in the gypsum sample; and S4, according to a mean value range of sulfur isotopes and oxygen isotopes in the sulfate, determining geological times of the plurality of target stratum rocks. The method has advantages that rock cores and rock debris samples of gypsum and anhydritein stratums in a large number of drilling evaporative rocks with different depths or layers in an evaporative rock basin are treated and analyzed; and according to the mean value range of the sulfurisotopes and the oxygen isotopes, the cambrian period stratum and the late Neoproterozoic stratum can be distinguished, the cambrian period stratum is the key point of oil and gas exploration, the accuracy of cambrian period stratum detection can be improved by applying the method, and therefore oil and gas exploration efficiency of the evaporated rock in the basin is increased.

The invention discloses a method for detecting sulfur stable isotopes in a seawater sample in an SO+ mode, which comprises the following specific steps: filtering, acidifying, precipitating and evaporating the seawater sample to dryness, filling a tin cup with the seawater sample, wrapping, and detecting the sample to be detected by using an element analyzer-stable isotope mass spectrometer. By tuning the voltage of the electron bombardment source and the focusing electrode, the high-energy electron flow is utilized to perform secondary ionization on SO2+ so as to generate SO+ for sulfur isotope detection, thereby enhancing the efficiency and accuracy of the sulfur isotope ratio of the seawater sample.

The invention provides equipment and a method for measuring the content of sulfur isotopes. The equipment for measuring the content of the sulfur isotopes comprises a sample combustion device, a gas-liquid reaction device, a solid-liquid separation device and a detection device. The method for measuring the content of the sulfur isotopes is used for measuring by using the equipment for measuring the content of the sulfur isotopes and comprises the following steps: combusting a sample in the sample combustion device to obtain gaseous sulfur dioxide, then inputting the sulfur dioxide into the gas-liquid reaction device for reaction to obtain a solid-liquid mixture containing a sulfur-containing precipitate, separating by using the solid-liquid separation device to obtain the sulfur-containing precipitate, and determining the content of the sulfur isotopes 34S by using the detection device. According to the equipment and the method for measuring the content of the sulfur isotopes, the content of the sulfur isotopes in a sample with relatively low sulfur content can be measured under the condition that the sample amount is not increased.

The invention provides a method for preparing an organic sulfur isotope detection sample, comprising the following steps: (1) converting the organic sulfur in the organic raw material into barium sulfate; (2) making the barium sulfate in solid acid phosphate and hydroiodic acid react to generate hydrogen sulfide gas; (3) hydrogen sulfide gas is removed and absorbed with alkaline solution to obtain an absorption solution, and (4) silver salt solution is added to the absorption solution to convert the sulfur in the absorption solution into Silver sulfide precipitates. The present invention also provides a detection method for organic sulfur isotopes in organic raw materials, including preparing detection samples according to the method of the present invention, and using SF 6 method for testing the sample.

The invention discloses a method for detecting sulfur stable isotope in an atmospheric sample by SO+, which comprises the following steps: filtering and collecting the atmospheric sample, carrying out ultrasonic extraction, precipitating, firing, filling in a tin cup, wrapping, and detecting the sample to be detected by using an element analyzer-stable isotope mass spectrometer. The ion source parameters are optimized, the secondary ionization effect of high-energy electron flow on SO2+ is achieved by tuning the filament and the ion source lens voltage, sulfur isotope detection is conducted in the form of SO+ ions, and therefore accurate detection of the sulfur isotope ratio of an atmospheric sample is achieved, and the method is high in result accuracy, good in repeatability, easy and convenient to operate and high in efficiency.

The invention discloses a method for analyzing sulfur isotopes in sulfate of a civil engineering drainage system, which comprises the following specific steps: filtering, acidifying, precipitating and evaporating a civil engineering drainage sample to dryness, filling into a tin cup, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. By optimizing isotope mass spectrum ion source electric field parameters and tuning the voltage of the reflecting plate and the ion lens, secondary ionization of high-energy electron flow on SO2+ is realized, SO+ is generated for accurate detection of sulfur isotopes, the result accuracy is high, the reproducibility is good, and the operation is simple and convenient.

The invention provides a method for determining oil sources by using sulfur isotopes in monomer sulfur-containing compounds of crude oil. The method comprises the following steps: crude oil is dissolved in ethanol, dichloromethane or dichloroethane, an alkylating reagent is added, and filtrate is obtained after a reaction; ethanol, dichloromethane or dichloroethane are removed from the filtrate, and oily substances are obtained; the oily substances and an alkane solvent of C5-C7 are mixed, and separation is carried out for deposition; the deposition is dissolved in dichloromethane, trichloromethane or acetonitrile, a first dealkylating reagent is added, and a solution A is obtained; extraction is carried out, and a thiophene compound and a solution B are obtained; a second dealkylating reagent is added into the solution B for carrying out a second dealkylation reaction, and a solution C is obtained; extraction is carried out, and a thioether compound is obtained; sulfur isotopic distribution of monomers in the thiophene compound and the thioether compound as well as sulfur isotopic distribution of sulfate in an oil-generating rock stratum system are determined; two sulfur isotopic distributions are compared, and the stratum whose isotopic distribution is most close to is the oil source layer.

The invention provides a device for extracting primary carbonate lattice sulfate in carbonate rock. The device comprises a carbonate rock-acetic acid reaction unit, an acetic acid feeding unit, a sulfate radical-barium salt reaction unit and a barium salt feeding unit, wherein a discharge port of the acetic acid feeding unit is communicated with a feed port of the carbonate rock-acetic acid reaction unit; a discharge port of the carbonate rock-acetic acid reaction unit and a discharge port of the barium salt feeding unit are both communicated with a feed port of the sulfate radical-barium salt reaction unit. All the units of the device are simple in connection and good in sealing performance, air can be effectively isolated, sulfur isotopes are prevented from being separated in the operation process, sulfur elements in other minerals are prevented from influencing the sulfur isotopes in CAS, and therefore high-purity native CAS can be extracted.

The invention discloses a method for detecting a sulfur stable isotope in a wetland plant sample in an SO+ mode, which comprises the following specific steps: drying, grinding and filtering the wetland plant sample by a screen, filling a tin cup with the wetland plant sample, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. Ion source parameters are optimized, secondary ionization of high-energy electron flow on SO2+ is achieved by tuning ion source core voltage and half-plate voltage, SO+ is generated for sulfur isotope detection, rapid and accurate detection of the sulfur isotope ratio of wetland plant samples is further achieved, and the method is high in result accuracy, good in reproducibility and high in efficiency.

The invention discloses a method for detecting sulfur stable isotope of inflorescence axis tissue culture garlic in an SO+ mode, which comprises the following specific steps: drying, grinding and filtering an inflorescence axis tissue culture garlic bulb sample by using a screen, filling into a tin cup, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. According to the method, the secondary ionization effect of ion source high-energy electron flow on SO2+ is utilized, and the generated SO+ is efficiently separated and accurately detected by tuning the voltage-carrying pressure of the quadrupole mass analyzer, so that the aim of efficiently and accurately detecting the sulfur isotope ratio of the garlic subjected to inflorescence axis tissue culture is fulfilled, and the method is high in result precision, good in repeatability and high in efficiency.

The invention discloses a method for analyzing sulfate sources in atmospheric particulate matter based on sulfur isotopes. The method comprises the following steps that (1) emission sources and winterambient air PM2.5 samples are collected; (2) sulfur isotope compositions in the samples are detected through an MAT-253 isotope mass spectrometer, and an ion chromatograph is used for analyzing ioniccomponents in soil raised-dust particles, biomass combustion emission particles and atmospheric particles; (3) a potential aerosol mass (PAM) is used for studying the sulfur isotope distillation characteristics in the process that SO2 is oxidized into SO4<2->; and (4) on the basis of the step (1) to step (3), the method for analyzing the sulfate sources in the atmospheric particulate matter basedon the sulfur isotopes is established, and primary emission contributions of fire coal and soil raised dust and contributions of fire coal, motor vehicle and biomass combustion emission on secondarysulfate are analyzed. The method has the important scientific significance and important application and promotion value, the new idea is developed for analyzing and studying the atmospheric particulate matter, and the new method is established for analyzing and studying the source of the atmospheric particulate matter.

The invention discloses a method for detecting sulfur stable isotopes in a landscape riverway water sample in an SO+ mode, which comprises the following specific steps: filtering, acidifying, precipitating and evaporating the landscape riverway water sample to dryness, filling a tin cup with the dried landscape riverway water sample, wrapping, and detecting a sample to be detected by using an element analyzer-stable isotope mass spectrometer. According to the method, ion source parameters are optimized, secondary ionization of high-energy electron flow on SO2+ is realized by tuning filament voltage to generate SO+, and the generated SO+ is effectively separated by tuning quadrupole voltage, so that the accuracy and efficiency of the sulfur isotope ratio of the landscape river water sample are improved, the result precision is high, the reproducibility is good, and the operation and equipment maintenance are easy.