CN116359321A - Method for measuring trace impurity content in nitrous oxide - Google Patents
Method for measuring trace impurity content in nitrous oxide Download PDFInfo
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- CN116359321A CN116359321A CN202310176496.7A CN202310176496A CN116359321A CN 116359321 A CN116359321 A CN 116359321A CN 202310176496 A CN202310176496 A CN 202310176496A CN 116359321 A CN116359321 A CN 116359321A
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- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000012535 impurity Substances 0.000 title claims abstract description 34
- 239000001272 nitrous oxide Substances 0.000 title claims abstract description 29
- 238000010521 absorption reaction Methods 0.000 claims abstract description 133
- 239000007788 liquid Substances 0.000 claims abstract description 71
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 18
- 239000012498 ultrapure water Substances 0.000 claims description 18
- 238000010926 purge Methods 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000011010 flushing procedure Methods 0.000 claims description 7
- 238000004445 quantitative analysis Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 abstract description 22
- 229910052751 metal Inorganic materials 0.000 abstract description 20
- 239000002184 metal Substances 0.000 abstract description 12
- 238000005406 washing Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 146
- 150000002500 ions Chemical class 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 238000009616 inductively coupled plasma Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000001819 mass spectrum Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 239000000443 aerosol Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910021654 trace metal Inorganic materials 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003994 anesthetic gas Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 combustion improvers Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 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
- G01N27/626—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 using heat to ionise a gas
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to the field of analysis and detection, in particular to a method for measuring trace impurity content in nitrous oxide. The method for measuring the trace impurity content in nitrous oxide provided by the invention uses a solution absorption method, can absorb and enrich the trace impurity content in the nitrous oxide by using an absorption liquid in a gas washing bottle, and directly measures the content of corresponding elements in a sample by using a mass spectrometer. The method solves the problem that the detection method in the prior art is not easy to accurately quantify the content of the metal impurities, improves the detection precision and reduces the detection cost.
Description
Technical Field
The invention relates to the field of analysis and detection, in particular to a method for measuring trace impurity content in nitrous oxide.
Background
Nitrous oxide is a colorless odorless anesthetic gas with little sweetness at normal temperature and pressure, and is colorless after liquefaction. The physical properties are very similar to CO 2. Nitrous oxide is relatively stable in nature, does not react with water, acid and alkali solutions, and does not produce dangerous nitrogen dioxide when mixed with oxygen. Nitrous oxide is mainly applied to analgesic and anesthetic gases, leakage detecting agents, refrigerants, combustion improvers, preservatives, chemical raw materials, atomic absorption spectrum gases and semiconductor manufacturing balance gases in dentistry, surgery and obstetrics and gynecology, and is applied to various electrical equipment.
The electron gases are known as "grains" and "sources" of semiconductor material. The purity of the gaseous feed directly affects the quality of the integrated circuit product. Therefore, the monitoring of the electronic gas is enhanced, the purity of the gas raw materials used in each procedure is practically ensured, and the pollution of the gas in a gas distribution system and a process is prevented. Studies have shown that even minute amounts of impurity gases in parts per million enter the process, this can result in reduced product quality. The metal microparticle impurities in the gas cause the semiconductor to generate electric leakage, poor withstand voltage and unchanged surface gram density, and are the main reasons for causing lattice defects and broken lines. The measurement and control of metallic elements in electronic industrial gases are important measures for improving the quality and yield of products, so that the control of the quality of electronic gases has important significance for prolonging the service life of electric operation.
At present, the national standard GBT 14600-2009 'gas nitrous oxide for electronic industry' does not provide technical indexes for metal elements, but in the production and operation process of enterprises, the enterprises are urgently required to accurately quantify trace metal impurities in high-purity gas, and detailed and accurate qualitative and quantitative analysis is performed on impurities contained in the electronic gas before the electronic gas is not used, so that the aim of controlling the quality of the electronic gas is achieved, and a plurality of clients also have the requirement of accurately determining trace metal impurities in the high-purity gas. The method for measuring the metal content in the gas for the electronic industry is provided in GBT 34972-2017 inductively coupled plasma mass spectrometry for measuring the metal content in the gas for the electronic industry, but the content of metal impurities is not easy to accurately quantify.
Disclosure of Invention
The invention provides a method for measuring the content of trace impurities in nitrous oxide, which aims to solve the problem that the detection method in the prior art is not easy to accurately quantify the content of metal impurities. The method for measuring the trace impurity content in nitrous oxide provided by the invention uses a solution absorption method, can absorb and enrich the trace impurity content in the nitrous oxide by using an absorption liquid in a gas washing bottle, and directly measures the content of corresponding elements in a sample by using a mass spectrometer.
The specific technical scheme of the invention is as follows:
the invention provides a method for measuring trace impurity content in nitrous oxide, which is characterized by comprising the following steps:
(S1) sequentially passing the sample gas through one or more absorption containers filled with absorption liquid to enrich the sample gas;
(S2) quantitatively analyzing the sample gas by using a mass spectrometer.
The metal impurities in the gas sample cannot be directly measured by using a mass spectrometer, so that the method selects a solution absorption method, and absorbs and enriches the metal elements in the gas to be measured through absorption liquid. And then introducing the sample to be detected into a mass spectrometer, separating by the mass spectrometer according to the mass-to-charge ratio, and measuring the content of the corresponding element in the sample according to the intensity of the mass spectrum peak of the element.
Preferably, in step (S1), the number of the absorption containers is 2.
According to the invention, the gas washing bottle made of PFA material is selected as the absorption container, and 2 gas washing bottles filled with the absorption solution are connected in series to absorb the sample gas, so that the collection efficiency of metal elements in the water-insoluble sample gas can be improved.
Preferably, in the step (S1), the flow rate of the sample gas is 0.5 to 2.5L/min.
More preferably, in the step (S1), the flow rate of the sample gas is 1.5 to 2.5L/min.
Further, in the step (S1), the flow rate of the sample gas was 2.0L/min.
The team of the invention is based on theoretical and experimental researches, and discovers that when the flow rate of the sample gas is more than 2.5L/min, the absorption efficiency of the absorption liquid on the sample gas is reduced, and the reason is presumably that the incomplete absorption of metal impurities in the sample gas is caused when the flow rate of the sample gas is too high. Based on the method, the flow rate of the sample gas is controlled to be 0.5-2.5L/min, so that the absorption efficiency of the absorption liquid on the sample gas can be improved.
Preferably, in the step (S1), the absorption time of the sample gas by the absorption liquid is 1 to 4 hours.
More preferably, in the step (S1), the absorption time of the sample gas by the absorption liquid is 3 to 4 hours.
Further, in the step (S1), the absorption time of the absorption liquid to the sample gas is 3h.
The team of the invention is based on theoretical and experimental researches, and found that when the absorption time of the absorption liquid to the sample gas is more than 4 hours, the absorption efficiency of the absorption liquid to the sample gas is reduced, and the reason is presumably that the absorption of the absorption liquid to the sample gas is basically complete when the absorption time of the absorption liquid to the sample gas reaches a certain time. Based on the method, the absorption time of the absorption liquid to the sample gas is controlled to be 1-4 hours, and the absorption efficiency of the absorption liquid to the sample gas is improved.
Preferably, in step (S1), the absorption liquid is a nitric acid solution or ultrapure water.
More preferably, in step (S1), the absorption liquid is ultrapure water.
Further, in the step (S1), the absorption liquid is EW-I grade ultrapure water.
GB/T34972-2017 proposes using a 5% nitric acid solution as the absorption liquid for a water-insoluble gas sample. However, the detection has high requirement on the content of trace metal impurities in the nitric acid solution, and the adoption of the common nitric acid solution as the absorption liquid is easy to cause interference, so that the experiment operation is inconvenient. Therefore, the electronic-grade nitric acid reagent needs to be purchased in the experiment, and the cost is high, so that the method is not beneficial to industrial large-scale application. Based on theoretical and experimental researches, the team of the invention discovers that the experimental results are not different when 5% nitric acid and EW-I grade ultrapure water are used as the absorption liquid, so that the EW-I grade ultrapure water is better selected as the absorption liquid by comprehensively considering.
Preferably, in step (S1), the sample gas is passed through an empty absorption vessel as a buffer bottle before passing through the absorption vessel containing the absorption liquid.
The sample gas is first passed through an empty absorber bottle as a buffer bottle and then absorbed in one or more absorber bottles containing an absorbing liquid. The purpose of the buffer vial is to prevent the absorption liquid from being sucked back into the sampling line or cylinder when measuring a gas that is readily soluble in water or dilute acid solution, to avoid the initiation of contamination or risk.
Preferably, in step (S2), the mass spectrometer is an inductively coupled plasma mass spectrometer,
wherein, the collection parameters are: the peak type is 3 points, the repetition number is 3, the scanning/repetition number is 100, and the rapid scanning integration time is 0.3S;
the inductively coupled plasma mass spectrometer operating conditions were as follows:
RF power: 500 to 1500W of the material to be processed,
plasma gas: 15.0L/min of the total weight of the product,
atomizing gas: 1.0L/min of the total weight of the product,
auxiliary gas: 1.0L/min of the total weight of the product,
make-up/dilution gas: 1.0L/min.
And introducing the treated sample into an atomization system to be atomized by taking high-purity argon as carrier gas, introducing the sample into a plasma central area in an aerosol form, desolvating, vaporizing, dissociating and ionizing the sample in high temperature and inert atmosphere to convert the sample into positive ions with positive charges, introducing the positive ions into a mass spectrometer through an ion acquisition system, separating the positive ions according to mass-to-charge ratios, and measuring the content of corresponding elements in the sample according to the peak intensity of an element mass spectrum.
Preferably, before the step (S2), the method further comprises a gas path purging, specifically comprising the following steps:
before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, opening the ball valve, and purging the sampling gas circuit with the gas circuit replacement flushing gas.
Before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, the ball valve is opened to purge the sampling gas path with filtered nitrogen. High-purity nitrogen can be selected as the gas path replacement flushing gas, and a 0.01um filter is added in the purging gas path to remove particles in the nitrogen.
Preferably, in step (S2), the quantitative analysis method is a standard curve method.
The gas to be detected enters a mass spectrometer through an ion acquisition system, the mass spectrometer is separated according to the mass-to-charge ratio, and the content of corresponding elements in the sample gas is measured according to the peak intensity of the mass spectrum of the elements.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method for measuring the trace impurity content in the nitrous oxide provided by the invention can be used for directly measuring the content of corresponding elements in a sample by using a mass spectrometer through absorbing and enriching an absorption liquid in a gas washing bottle by using a solution absorption method, thereby improving the detection precision and reducing the detection cost.
(2) The flow rate of the sample gas is controlled to be 0.5-2.5L/min, and the absorption efficiency of the absorption liquid on the sample gas is improved.
(3) The invention controls the absorption time of the absorption liquid to the sample gas to be 1-4 h, and improves the absorption efficiency of the absorption liquid to the sample gas.
(4) Based on theoretical and experimental researches, the team of the invention discovers that the experimental results are not different when 5% nitric acid and EW-I grade ultrapure water are used as the absorption liquid, so that the EW-I grade ultrapure water is better selected as the absorption liquid by comprehensively considering.
Detailed Description
The invention is further described below with reference to examples.
General examples
The method for measuring the trace impurity content in nitrous oxide is characterized by comprising the following steps of:
(S1) sequentially passing the sample gas through one or more absorption containers filled with absorption liquid to enrich the sample gas;
(S2) quantitatively analyzing the sample gas by using a mass spectrometer.
Preferably, in the step (S1), the flow rate of the sample gas is 0.5 to 2.5L/min.
More preferably, in the step (S1), the flow rate of the sample gas is 1.5 to 2.5L/min.
Preferably, in the step (S1), the absorption time of the sample gas by the absorption liquid is 1 to 4 hours.
More preferably, in the step (S1), the absorption time of the sample gas by the absorption liquid is 3 to 4 hours.
Preferably, in step (S1), the absorption liquid is a nitric acid solution or ultrapure water.
More preferably, in step (S1), the absorption liquid is ultrapure water.
Preferably, in step (S1), the sample gas is passed through an empty absorption vessel as a buffer bottle before passing through the absorption vessel containing the absorption liquid.
Preferably, in step (S2), the mass spectrometer is an inductively coupled plasma mass spectrometer,
wherein, the collection parameters are: the peak type is 3 points, the repetition number is 3, the scanning/repetition number is 100, and the rapid scanning integration time is 0.3S;
the inductively coupled plasma mass spectrometer operating conditions were as follows:
RF power: 500 to 1500W of the material to be processed,
plasma gas: 15.0L/min of the total weight of the product,
atomizing gas: 1.0L/min of the total weight of the product,
auxiliary gas: 1.0L/min of the total weight of the product,
make-up/dilution gas: 1.0L/min.
Preferably, before the step (S2), the method further comprises a gas path purging, specifically comprising the following steps:
before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, opening the ball valve, and purging the sampling gas circuit with the gas circuit replacement flushing gas.
Preferably, in step (S2), the quantitative analysis method is a standard curve method.
Example 1
(1) Enriching a sample: the method comprises the steps of selecting a same bottle of high-purity nitrous oxide sample, respectively absorbing with 5% nitric acid solution and EW-I grade ultrapure water as absorption liquids, and enriching sample gas by passing through an empty absorption container serving as a buffer bottle and then passing through 2 absorption containers filled with the absorption liquids before passing through the absorption container filled with the absorption liquids. The flow rate of the sample gas was set to 2L/min, and the absorption time of the absorption liquid to the sample gas was set to 3h.
(2) And (3) air path purging: before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, the ball valve is opened to purge the sampling gas path with filtered nitrogen. High-purity nitrogen is selected as the gas path replacement flushing gas, and a 0.01um filter is added in the purging gas path.
(3) And (3) measuring: introducing the processed sample into an atomization system to be atomized by taking high-purity argon as carrier gas, introducing the sample into a plasma central area in an aerosol form, desolvating, vaporizing, dissociating and ionizing the sample in high temperature and inert atmosphere to convert the sample into positive ions with positive charges, introducing the positive ions into an inductively coupled plasma through an ion acquisition system, separating the positive ions and the negative ions according to mass-to-charge ratio by a mass spectrometer, and determining corresponding elements in the sample according to the intensity of an element mass spectrum peakContent of the element. Wherein N used in the experiment 2 The types of metal ions and main technical indexes contained in the O sample are shown in table 1, main instruments and materials used in the experiment are shown in table 2, and the measuring conditions and the operating parameters of the instruments are shown in tables 3, 4 and 5.
TABLE 1N 2 The kind of metal ion contained in O sample and main technical index
TABLE 2 Main instruments and materials
Table 3 inductively coupled plasma mass spectrometer operating conditions
| Operating parameters | Setting value | Sample injection system | Specification of specification |
| RF power (W) | 500-1500 | Atomizing chamber | Quartz |
| Plasma gas (L/min)) | 15.0 | Atomizer | Quartz |
| Atomizing gas (L/min) | 1.0 | Rectangular tube | Quartz |
| Auxiliary gas (L/min) | 1.0 | Cone with conical surface | Pt |
| Compensation/dilution gas (L/min) | 1.0 |
Table 4 parameters of acquisition
| Parameters (parameters) | Setting up |
| Peak type | 3 points |
| Number of repetitions | 3 |
| Number of scans/repetitions | 100 |
| Fast scan integration time | 0.3S |
TABLE 5 test patterns for elements
| Sequence number | Element(s) | Mass to charge ratio | Mode | Sequence number | Element(s) | Mass to charge ratio | Mode |
| 1 | Cr | 52 | Cool NH 3 | 10 | Na | 23 | Cool NH 3 |
| 2 | Mo | 95 | He | 11 | Zn | 64 | He |
| 3 | Ni | 58 | Cool NH 3 | 12 | Al | 27 | Cool NH 3 |
| 4 | Mn | 55 | Cool NH 3 | 13 | Mg | 24 | Cool NH 3 |
| 5 | Cu | 63 | Cool NH 3 | 14 | K | 39 | Cool NH 3 |
| 6 | Fe | 56 | Cool NH 3 | 15 | Li | 7 | Cool NH 3 |
| 7 | Ti | 48 | He | 16 | Ag | 107 | Cool NH 3 |
| 8 | Co | 59 | Cool NH 3 | 17 | Pb | 208 | He |
| 9 | Ca | 40 | Cool NH 3 |
(4) Results: the metal element in the sample was quantified by the standard curve method, the metal element detection results using a 5% nitric acid solution as the absorption liquid are shown in Table 6, and the metal element detection results using EW-I grade ultrapure water as the absorption liquid are shown in Table 7.
TABLE 6 detection results of metallic element in 5% nitric acid solution as absorbent
TABLE 7 metallic element detection results with EW-I grade ultra-pure water as absorption liquid
According to the experimental results of 5% nitric acid and EW-I grade ultrapure water absorption liquid, the difference between the results is not great, so that the EW-I grade ultrapure water is better selected as the absorption liquid by comprehensively considering.
Example 2
(1) Enriching a sample: selecting a high-purity nitrous oxide sample in the same bottle, enabling the flow rate of sample gas to pass through an air-washing gas bottle serving as a buffer bottle at 0.5L/min, 1.0L/min, 1.5L/min, 2.0L/min and 2.5L/min respectively, and enriching the sample gas by passing through an absorption container with 2 gas filled absorption liquid. The mass of the two bottles of absorption liquid is 100g respectively, the total absorption amount of the gas is 120L, the absorption time of the absorption liquid to the sample gas is set to 3h, and the absorption liquid is EW-I grade ultrapure water.
(2) And (3) air path purging: before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, the ball valve is opened to purge the sampling gas path with filtered nitrogen. High-purity nitrogen is selected as the gas path replacement flushing gas, and a 0.01um filter is added in the purging gas path.
(3) And (3) measuring: and introducing the treated sample into an atomization system to be atomized by taking high-purity argon as carrier gas, introducing the sample into a plasma central area in an aerosol form, desolvating, vaporizing, dissociating and ionizing the sample in high temperature and inert atmosphere to convert the sample into positive ions with positive charges, introducing the positive ions into an inductively coupled plasma through an ion acquisition system, separating the positive ions and the negative ions according to a mass-to-charge ratio by a mass spectrometer, and determining the content of corresponding elements in the sample according to the intensity of an element mass spectrum peak. Wherein N used in the experiment 2 The types of metal ions and main technical indexes contained in the O sample are shown in table 1, main instruments and materials used in the experiment are shown in table 2, and the measuring conditions and the operating parameters of the instruments are shown in tables 3, 4 and 5.
(4) Results: the metal elements in the samples were quantified by a standard curve method, and the results are shown in tables 8 to 12.
TABLE 8 detection results of sample gas flow rate of 0.5L/min
TABLE 9 detection results of sample gas flow rate of 1.0L/min
TABLE 10 detection results of sample gas flow rate of 1.5L/min
TABLE 11 detection results of sample gas flow rate of 2.0L/min
TABLE 12 detection results of sample gas flow rate of 2.5L/min
According to comparison of experimental results of the different flow rates, the absorption efficiency of 2.0L/min is found to be higher than that of the other flow rates. The team of the invention is based on theoretical and experimental researches, and discovers that when the flow rate of the sample gas is more than 2.5L/min, the absorption efficiency of the absorption liquid on the sample gas is reduced, and the reason is presumably that the incomplete absorption and absorption of metal impurities in the sample gas are caused by the excessively high flow rate of the sample gas. Based on the method, the flow rate of the sample gas is controlled to be 0.5-2.5L/min, so that the absorption efficiency of the absorption liquid on the sample gas can be improved.
Example 3
(1) Enriching a sample: selecting a same bottle of high-purity nitrous oxide sample, enabling sample gas to pass through an air washing gas bottle serving as a buffer bottle, then passing through 2 absorption containers filled with absorption liquid, and respectively setting the absorption time of the absorption liquid to the sample gas to be 1h, 2h, 3h and 4h, so as to enrich the sample gas. The mass of the two bottles of absorption liquid is 100g respectively, the total absorption amount of the gas is 120L, the flow rate of the sample gas is 2.0L/min, and the absorption liquid is EW-I grade ultrapure water.
(2) And (3) air path purging: before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, the ball valve is opened to purge the sampling gas path with filtered nitrogen. High-purity nitrogen is selected as the gas path replacement flushing gas, and a 0.01um filter is added in the purging gas path.
(3) And (3) measuring: and introducing the treated sample into an atomization system to be atomized by taking high-purity argon as carrier gas, introducing the sample into a plasma central area in an aerosol form, desolvating, vaporizing, dissociating and ionizing the sample in high temperature and inert atmosphere to convert the sample into positive ions with positive charges, introducing the positive ions into an inductively coupled plasma through an ion acquisition system, separating the positive ions and the negative ions according to a mass-to-charge ratio by a mass spectrometer, and determining the content of corresponding elements in the sample according to the intensity of an element mass spectrum peak. Wherein N used in the experiment 2 The types of metal ions and main technical indexes contained in the O sample are shown in table 1, main instruments and materials used in the experiment are shown in table 2, and the measuring conditions and the operating parameters of the instruments are shown in tables 3, 4 and 5.
(4) Results: the metal elements in the samples were quantified by a standard curve method, and the results are shown in tables 13 to 16.
TABLE 13 detection results of absorption time of absorption liquid to sample gas of 1h
TABLE 14 detection results of absorption time of absorption liquid to sample gas of 2h
TABLE 15 detection results of absorption time of absorption liquid to sample gas of 3h
TABLE 16 detection results of absorption time of absorption liquid to sample gas of 4h
According to comparison of experimental results of different absorption times, the absorption efficiency of the absorption liquid on the sample gas is found to be higher than that of other absorption liquids, wherein the absorption time of the absorption liquid on the sample gas is 3h. The team of the invention is based on theoretical and experimental researches, and found that when the absorption time of the sample gas is more than 4 hours, the absorption efficiency of the absorption liquid to the sample gas is reduced, and the reason is presumably that the absorption of the sample gas is basically complete when the absorption of the sample gas reaches a certain time. Based on the method, the absorption time of the sample gas is controlled to be 1-4 hours, and the absorption efficiency of the absorption liquid on the sample gas can be improved.
The raw materials and equipment used in the invention are common raw materials and equipment in the field unless specified otherwise; the methods used in the present invention are conventional in the art unless otherwise specified.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The method for measuring the trace impurity content in nitrous oxide is characterized by comprising the following steps of:
(S1) sequentially passing the sample gas through one or more absorption containers filled with absorption liquid to enrich the sample gas;
(S2) quantitatively analyzing the sample gas by using a mass spectrometer.
2. The method for measuring the trace impurity content in nitrous oxide according to claim 1, wherein in the step (S1), the flow rate of the sample gas is 0.5 to 2.5L/min.
3. The method for measuring the trace impurity content in nitrous oxide according to claim 2, wherein in the step (S1), the flow rate of the sample gas is 1.5 to 2.5L/min.
4. The method for measuring the trace impurity content in nitrous oxide according to claim 1, wherein in the step (S1), the absorption time of the absorption liquid to the sample gas is 1 to 4 hours.
5. The method for measuring the trace impurity content in nitrous oxide according to claim 4, wherein in the step (S1), the absorption time of the absorption liquid to the sample gas is 3 to 4 hours.
6. The method for measuring the trace impurity content in nitrous oxide according to claim 1, wherein in the step (S1), the absorption liquid is a nitric acid solution or ultrapure water.
7. The method for measuring the trace impurity content in nitrous oxide according to claim 6, wherein in the step (S1), the absorption liquid is ultrapure water.
8. The method for measuring the trace impurity content in nitrous oxide according to claim 1, wherein in the step (S1), the sample gas is passed through an empty absorption vessel as a buffer bottle before passing through the absorption vessel containing the absorption liquid.
9. The method for determining trace impurity content in nitrous oxide according to claim 1, further comprising a gas path purge prior to step (S2), specifically comprising the steps of:
before connecting the sampling pipeline with the sample gas and the subsequent absorbing device, opening the ball valve, and purging the sampling gas circuit with the gas circuit replacement flushing gas.
10. The method for measuring the trace impurity content in nitrous oxide according to claim 1, wherein in the step (S2), the quantitative analysis method is a standard curve method.
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| US6418781B1 (en) * | 1998-04-09 | 2002-07-16 | Nippon Sanso Corporation | System for analyzing trace amounts of impurities in gases |
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| US6418781B1 (en) * | 1998-04-09 | 2002-07-16 | Nippon Sanso Corporation | System for analyzing trace amounts of impurities in gases |
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