CN112730583A - Method for analyzing sulfur isotope in sulfate of civil engineering drainage system - Google Patents
Method for analyzing sulfur isotope in sulfate of civil engineering drainage system Download PDFInfo
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- CN112730583A CN112730583A CN202110060267.XA CN202110060267A CN112730583A CN 112730583 A CN112730583 A CN 112730583A CN 202110060267 A CN202110060267 A CN 202110060267A CN 112730583 A CN112730583 A CN 112730583A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 39
- 239000011593 sulfur Substances 0.000 title claims abstract description 39
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title abstract description 19
- 150000002500 ions Chemical class 0.000 claims abstract description 30
- 238000001514 detection method Methods 0.000 claims abstract description 23
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims 1
- 230000020477 pH reduction Effects 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 230000005684 electric field Effects 0.000 abstract 1
- 238000004949 mass spectrometry Methods 0.000 abstract 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 44
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 9
- -1 sulfur dioxide ion Chemical class 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 5
- 230000003446 memory effect Effects 0.000 description 5
- 229910052946 acanthite Inorganic materials 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 4
- 229940056910 silver sulfide Drugs 0.000 description 4
- 238000005303 weighing Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 2
- 229910001626 barium chloride Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Inorganic materials S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- VNWKTOKETHGBQD-OUBTZVSYSA-N carbane Chemical compound [13CH4] VNWKTOKETHGBQD-OUBTZVSYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
本发明公开了土建工程排水系统硫酸盐中硫同位素分析方法，具体步骤为土建工程排水样品经过滤、酸化、沉淀、蒸干后，装入锡杯并包裹，采用元素分析仪‑稳定同位素质谱联用仪检测待测样品。本发明通过优化同位素质谱离子源电场参数，调谐反射板和离子透镜电压实现高能电子流对SO2 +进行二次电离，产生SO+进行硫同位素精准检测，结果准确性高，重现性好，操作简便。The invention discloses a method for analyzing sulfur isotopes in sulfate in a civil engineering drainage system. The specific steps are that after a civil engineering drainage sample is filtered, acidified, precipitated and evaporated to dryness, it is put into a tin cup and wrapped, and an elemental analyzer-stable isotope mass spectrometer is used for coupling. Use the instrument to detect the sample to be tested. The method optimizes the electric field parameters of the isotope mass spectrometry ion source, and tunes the voltage of the reflection plate and the ion lens to realize the secondary ionization of SO 2 + by high-energy electron flow, and generates SO + for accurate detection of sulfur isotopes. The result has high accuracy and good reproducibility. Easy to operate.
Description
The invention obtains the subsidies of Tianjin large-scale education fund (043-.
Technical Field
The invention belongs to the technical field of stable isotope analysis, and particularly relates to a method for analyzing sulfur isotopes in sulfate of a drainage system of civil engineering.
Background
The sulfur stable isotope analysis technology is widely applied to the aspects of environmental protection, agricultural production and the like, and especially plays an important role in the aspects of sulfur element migration and conversion mechanism, pollutant source tracing and the like in water environment sulfate.
At present, the common sulfur stable isotope analysis method is that an element analyzer is used in combination with a mass spectrometer, namely, sulfur in a sample is oxidized into sulfur dioxide by the element analyzer, and then the sulfur dioxide (SO) is oxidized by an ion source of the isotope mass spectrometer2) Conversion to sulfur dioxide ion (SO)2 +) Carrying out sulfurIsotope ratio analysis. But SO involved in the process2 +(and its δ S34 isotope) have a high mass-to-charge ratio of 64, 66 m/e. The stable isotope mass spectrometer generally simultaneously undertakes the carbon-nitrogen isotope detection task, and the mass-to-charge ratios of the carbon dioxide (and the delta C13 isotope thereof) and the nitrogen ion (and the delta N15 isotope thereof) involved in the stable isotope mass spectrometer are respectively CO2 +(m/e 44, 45) and N2 +(m/e 28, 29). Due to SO in conventional sulfur dioxide analysis2 +The mass-to-charge ratio is obviously higher than that of CO2 +And N2 +Mass to charge ratio. When the carbon-nitrogen isotope detection is converted into the sulfur isotope detection, the SO with higher mass-to-charge ratio is influenced by the instrument memory effect2 +It is difficult to focus on the receiver effectively, affecting the detection result. To eliminate the memory effect of the instrument, long-time debugging work is often required to improve the accuracy and reproducibility of sulfur isotope detection, and vice versa.
The invention optimizes ion source parameters, and realizes high-energy electron current to SO by tuning voltage of the reflecting plate and the ion lens2 +The secondary ionization effect of the ions causes the ions to generate sulfur monoxide ions (SO)+)，SO+And δ S34 isotope mass-to-charge ratio of 48, 50, and CO2 +And N2 +The mass-to-charge ratio is closer, which is beneficial to improving the accuracy and the reproducibility of the detection of the sulfur stable isotope, reducing the influence of the memory effect and improving the detection efficiency.
The invention utilizes ion source high-energy electron current to SO2 +Secondary ionization of ions to produce SO+The method provided by the invention supplements the blank of the original sulfur stable isotope detection technology.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for analyzing sulfur isotopes in sulfate of a drainage system of civil engineering, which is characterized by comprising the following steps of:
(1) filtering, acidifying, precipitating and evaporating a civil engineering drainage sample, accurately weighing 1-10 mg of sample, filling the sample into a tin cup and wrapping the sample;
(2) detecting a sample to be detected by adopting an element analyzer-stable isotope mass spectrometer; the elemental analyzer parameters were: the temperature of the oxidation tube is 1000 ℃, the temperature of the chromatographic column is 80 ℃, and the catalysts in the quartz tube in the oxidation furnace are 25 g of tungsten oxide and 50 g of granular pure copper;
(3) ionizing sample by high-energy ion source to generate SO+(ii) a Ion source parameters of the stable isotope mass spectrometer are as follows: the voltage of an ion source filament is-116V, the voltage of an ion source reflecting plate is 5.6V, and the voltage of an ion source lens is 145V;
(4) mass analyzer pair SO+Separating isotope signals; the stable isotope mass spectrometer mass analyzer parameters were: the primary quadrupole voltage is-120V, and the secondary quadrupole voltage is 165V;
(5) and analyzing the isotope value of the sample under the conditions to obtain the sulfur isotope value of the sample, repeatedly detecting for 5 times, and counting the experimental result.
The invention further discloses a method for analyzing sulfur isotopes in the sulfate of the drainage system of the civil engineering, and the method is applied to the aspect of improving the detection accuracy of the stable isotopes of the sulfur in the drainage sample of the civil engineering. The experimental results show that: the method has the advantages of good reproducibility, high analysis efficiency, high accuracy and the like, can meet the requirement of detecting the sulfur stable isotope of the drainage sample of the civil engineering, and can achieve the sulfur stable isotope analysis accuracy SD (thousandths) of 0.05 and the sulfur isotope analysis stability SD (thousandths) of 0.08, which cannot be achieved by the conventional sulfur dioxide mode analysis method.
The invention mainly solves the problem of poor detection accuracy of the stable isotope of sulfur in the drainage sample of civil engineering, and overcomes the influence of sulfur dioxide ions with high mass-to-charge ratio on the detection of the isotope of sulfur due to the memory effect of an instrument. The method mainly considers that sulfur dioxide ions are replaced by sulfur monoxide ions with lower mass-to-charge ratio by controlling the parameters of an ion source and a mass analyzer so as to improve the accuracy and the repeatability of detecting sulfur isotopes in the drainage sample of the civil engineering.
Compared with the prior art, the method for analyzing the sulfur isotope in the sulfate of the civil engineering drainage system has the positive effects that:
(1) the method has the advantages of easy operation, no influence of instrument memory effect on the detection of the sulfur stable isotope ratio, high accuracy, good reproducibility and the like.
(2) Compared with the prior art, the method solves the problem that sulfur dioxide ions with high mass-to-charge ratio have influence on the detection of the sulfur isotope due to the instrument memory effect when the stable isotope in the drainage sample of civil engineering is detected, and improves the accuracy and the repeatability of the detection of the sulfur isotope.
Detailed Description
The invention is described below by means of specific embodiments. Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention. The raw materials and reagents used in the present invention are commercially available.
Example 1
The method for analyzing sulfur isotopes in sulfate of the drainage system of the civil engineering comprises the following steps:
a. filtering and acidifying a civil engineering drainage sample to remove carbonate, adding barium chloride to generate barium sulfate precipitate to fix sulfate radical, filtering again to collect barium sulfate precipitate, evaporating the precipitate to dryness at 50 ℃, accurately weighing 5.0mg of precipitate, filling the precipitate into a tin cup and wrapping.
b. In the detection of the sulfur stable isotope (δ S34), IAEA-S-1 (silver sulfide, δ S34 ═ 0.30 ‰), IAEA-S-3 (silver sulfide, δ S34 ═ 32.3 ‰), and NBS-127 (barium sulfate, δ S34 ═ 20.3 ‰) were used as standards.
c. Detecting a sample to be detected by adopting an element analyzer-stable isotope mass spectrometer; the elemental analyzer parameters were: the oxidation tube is 1000 ℃, the chromatographic column is 80 ℃, and the catalyst in the quartz tube in the oxidation furnace is 25 g of tungsten oxide and 50 g of granular pure copper.
d. Ionizing sample by high-energy ion source to generate SO+(ii) a Ion source parameters of the stable isotope mass spectrometer are as follows: ion source filament voltage-116V, ion source reflector voltage 5.6V, and ion source lens voltage 145V.
e. Mass analyzer pair SO+Separating isotope signals; the stable isotope mass spectrometer mass analyzer parameters were: the primary quadrupole voltage is-120V, and the secondary quadrupole voltage is 165V.
f. And analyzing the isotope values of the standard substance and the sample under the conditions, establishing a standard curve by taking the signal value of the standard substance as a horizontal coordinate and the standard isotope value of the standard substance as a vertical coordinate, and bringing the signal value of the sample into the standard curve to obtain the sulfur isotope value of the sample. And repeating the detection for 5 times, and counting the experimental results.
g. The invention mainly uses the following instruments: nu Horizon type stable isotope mass spectrometer, EuroVector EA3000 type element analyzer.
The civil engineering drainage sample is treated by the steps, and the detection is repeated for 5 times, and the result is shown in table 1.
TABLE 1. results of the accuracy test of. delta. S34
Example 2
The method for analyzing sulfur isotopes in sulfate of the drainage system of the civil engineering comprises the following steps:
a. filtering and acidifying a civil engineering drainage sample to remove carbonate, adding barium chloride to generate a barium sulfate precipitate to fix sulfate radical, filtering again to collect the barium sulfate precipitate, evaporating the precipitate to dryness at 50 ℃, accurately weighing 1.0, 2.5, 4.0, 5.5, 7.0, 8.5 and 10.0mg of precipitate respectively, filling into a tin cup and wrapping.
b. In the detection of the sulfur stable isotope (δ S34), IAEA-S-1 (silver sulfide, δ S34 ═ 0.30 ‰), IAEA-S-3 (silver sulfide, δ S34 ═ 32.3 ‰), and NBS-127 (barium sulfate, δ S34 ═ 20.3 ‰) were used as standards.
c. Detecting a sample to be detected by adopting an element analyzer-stable isotope mass spectrometer; the elemental analyzer parameters were: the oxidation tube is 1000 ℃, the chromatographic column is 80 ℃, and the catalyst in the quartz tube in the oxidation furnace is 25 g of tungsten oxide and 50 g of granular pure copper.
d. Ionizing sample by high-energy ion source to generate SO+(ii) a Ion source parameters of the stable isotope mass spectrometer are as follows: ion source filament voltage-116V, ion source reflector voltage 5.6V, and ion source lens voltage 145V.
e. Mass analyzer pair SO+Separating isotope signals; the stable isotope mass spectrometer mass analyzer parameters were: the primary quadrupole voltage is-120V, and the secondary quadrupole voltage is 165V.
f. And analyzing the isotope values of the standard substance and the sample under the conditions, establishing a standard curve by taking the signal value of the standard substance as a horizontal coordinate and the standard isotope value of the standard substance as a vertical coordinate, and bringing the signal value of the sample into the standard curve to obtain the sulfur isotope value of the sample. And repeating the detection for 5 times, and counting the experimental results.
g. The invention mainly uses the following instruments: nu Horizon type stable isotope mass spectrometer, EuroVector EA3000 type element analyzer.
The civil engineering drainage sample is treated by the steps, the stability of the method is tested, and the result is shown in table 2.
TABLE 2. results of stability test of δ S34(‰)
Example 3
Comparative test
In conclusion, the method has the characteristics of simplicity and convenience in operation, high precision, good repeatability, high efficiency and the like, and can be applied to detection of the sulfur isotope in the drainage sample of the civil engineering.
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