CN109580800A - The measuring method of organic sulfur compound ingredient in air - Google Patents
The measuring method of organic sulfur compound ingredient in air Download PDFInfo
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- CN109580800A CN109580800A CN201710912425.3A CN201710912425A CN109580800A CN 109580800 A CN109580800 A CN 109580800A CN 201710912425 A CN201710912425 A CN 201710912425A CN 109580800 A CN109580800 A CN 109580800A
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Abstract
The invention discloses a kind of measuring method of organic sulfur compound ingredient in air, this method carries out air sample acquisition using Soviet Union's Ma tank；Using nitrogen as spirit, with Soviet Union's Ma tank dynamic dilution instrument configuration hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, five kinds of organic sulfur calibrating gas of ethyl sulfide and for the interior standard gas of assisted quantitative, the sample introduction interface of configured gas and concentrating instrument connects and draws gas into concentrating instrument；Concentrating instrument draws standard curve by the way that concentrated gas is inputted gas chromatograph-mass spectrometer analysis after the absorption parsing of three-level cold-trap；By the sample of acquisition by inputting gas chromatograph-mass spectrometer after the absorption parsing of concentrating instrument three-level cold-trap, analyzed using inner mark method ration, through reference standard curve, respectively obtain Air Hydrogen Sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, ethyl sulfide concentration value.This method copes with the extremely strong activity of organic sulfur compound and unstable feature, and easy to operate, realization quickly and effectively detects, the batch quantity analysis of organic sulfur compound suitable for air.
Description
Technical field
The present invention relates to a kind of measuring methods of organic sulfur compound ingredient in air.
Background technique
Stench refer to irritating human body olfactory organ, cause unhappy and damage living environment gaseous matter.Its
Middle organosulfur compound is one of the main reason for causing environmental malodors to pollute, and sulfurous gas includes carbon disulfide, thioether, sulphur
The organosulfur compounds such as alcohol, hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, ethyl sulfide, since its odor threshold is lower, to human body
Physiological system causes significant discomfort, and toxicity causes to seriously endanger and extremely concerned to human health greatly.Stench is examined at present
The most commonly used is triangle odor bag methods for survey, manually smell and distinguish, error is larger, and without legal.
Organic sulfur compound there are polarity strong, poor chemical stability has the characteristics that be easy absorption and reaction, cause common
Detection method is difficult to detect.Currently, national standard (GB/T 14678-1993) has studied hydrogen sulfide, methyl mercaptan, methyl sulfide and diformazan two
The measurement of four kinds of organic sulfur compound ingredients such as sulphur.Its principle is that low temperature is concentrated and uses gas chromatography analysis, but this method needs
Special enrichment facility, is concentrated using liquid oxygen, there is certain risk, and the steaming of the water in sample is not accounted in analysis method
Gas influences, and sampling step is cumbersome, causes the stability of testing result poor, so application range is not wide at present, is difficult to carry out batch
Analysis.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of measuring method of organic sulfur compound ingredient in air, we
Method copes with the extremely strong activity of organic sulfur compound and unstable feature, while easy to operate, and realization quickly and effectively detects,
The batch quantity analysis of organic sulfur compound suitable for air.
In order to solve the above technical problems, the measuring method of organic sulfur compound ingredient includes the following steps: in air of the present invention
Step 1: being sampled using Soviet Union's Ma tank through silanization treatment, automatic clear tank instrument high pure nitrogen pair is used before sampling
Soviet Union's Ma tank is cleaned and is evacuated, repeated multiple times after being analyzed no blank residual, opens Soviet Union's Ma pot valve in sampled point
Door, closing valve takes back laboratory after adopting full sample；
Step 2: using nitrogen as spirit, with Soviet Union's Ma tank dynamic dilution instrument by hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, second sulphur
Five kinds of organic sulfur calibrating gas of ether are diluted to 10ppb, will be used for the bromochloromethane of assisted quantitative, Isosorbide-5-Nitrae-difluorobenzene, chlorobenzene-D5,
Standard gas is diluted to 100ppb, configured organic sulfur calibrating gas and interior standard gas in 4- bromofluoro benzene and the sample introduction interface of concentrating instrument connects
It connects, extracts 40~800ml gas and enter concentrating instrument；
Step 3: concentrating instrument draws standard by the way that concentrated gas is inputted gas chromatograph-mass spectrometer analysis after the absorption parsing of three-level cold-trap
Curve；
Step 4: concentrated gas is inputted makings after the sample for Ma tank acquisition of reviving is parsed by the absorption of concentrating instrument three-level cold-trap
Combined instrument is analyzed using inner mark method ration, through reference standard curve, respectively obtains Air Hydrogen Sulfide, thiophene, ethyl mercaptan, first
The concentration value of ethyl sulfide, ethyl sulfide.
Further, the condition of the concentrating instrument three-level cold-trap absorption parsing is -150 DEG C of level-one cold trap trapping temperature, baking
150 DEG C of temperature, baking time 8min；- 30 DEG C of second level cold trap trapping temperature, 180 DEG C of resolution temperature, 190 DEG C of baking temperature, baking
Time 10min；- 160 DEG C of three-level cold trap trapping temperature, sample injection time 2min, baking time 3min.
Further, the chromatographic condition of the gas chromatograph-mass spectrometer analysis is 125 DEG C of injection port, nonpolar capillary column, program liter
50 DEG C of stop 4min of temperature, 120 DEG C of stop 4min are warming up to 20 DEG C/min, are warming up to 220 DEG C of stops with 25 DEG C/min
3min, carrier gas are He gas, column flow rate is 1.2ml/min and without shunting；Mass Spectrometry Conditions are 230 DEG C of ion source temperature, quadrupole rod
150 DEG C, EI voltage 70eV, solvent delay 4 minutes, full scan mode, bromofluoro benzene tuning.
Further, the specification of the nonpolar capillary column is 60 m of length, 0.25 mm of internal diameter, 0.25 μm of film thickness；It is described complete
The mass number of scan pattern is 32~37M/Z, and mass number is 35~200M/Z from 5.5 minutes.
Further, the connecting pipeline between Soviet Union's Ma tank, concentrating instrument and gas chromatograph-mass spectrometer passes through silanization inertization.
Since the measuring method of organic sulfur compound ingredient in air of the present invention uses above-mentioned technical proposal, i.e. this method is adopted
Laboratory is taken back after carrying out air sample acquisition with Soviet Union's Ma tank through silanization treatment；Using nitrogen as spirit, with Soviet Union's Ma tank dynamic
It dilutes five kinds of instrument configuration hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, ethyl sulfide organic sulfur calibrating gas and is used for assisted quantitative
Interior standard gas, the sample introduction interface of configured organic sulfur calibrating gas and interior standard gas and concentrating instrument connects and draws gas into dense
Contracting instrument；Concentrating instrument draws standard curve by the way that concentrated gas is inputted gas chromatograph-mass spectrometer analysis after the absorption parsing of three-level cold-trap；It will
The sample of acquisition by concentrating instrument three-level cold-trap absorption parsing after inputs gas chromatograph-mass spectrometer, analyzed using inner mark method ration, through pair
Sighting target directrix curve, respectively obtain Air Hydrogen Sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, ethyl sulfide concentration value.This method energy
The enough extremely strong activity of reply organic sulfur compound and unstable feature, at the same it is easy to operate, and realization quickly and effectively detects, and is applicable in
The batch quantity analysis of organic sulfur compound in air.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and embodiments:
Fig. 1 is the chromatogram of the five kinds of organic sulfur compounds measured using this method.
Specific embodiment
The measuring method of organic sulfur compound ingredient includes the following steps: in air of the present invention
Step 1: being sampled using Soviet Union's Ma tank through silanization treatment, automatic clear tank instrument high pure nitrogen pair is used before sampling
Soviet Union's Ma tank is cleaned and is evacuated, repeated multiple times after being analyzed no blank residual, opens Soviet Union's Ma pot valve in sampled point
Door, closing valve takes back laboratory after adopting full sample；
Step 2: using nitrogen as spirit, with Soviet Union's Ma tank dynamic dilution instrument by hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, second sulphur
Five kinds of organic sulfur calibrating gas of ether are diluted to 10ppb, will be used for the bromochloromethane of assisted quantitative, Isosorbide-5-Nitrae-difluorobenzene, chlorobenzene-D5,
Standard gas is diluted to 100ppb, configured organic sulfur calibrating gas and interior standard gas in 4- bromofluoro benzene and the sample introduction interface of concentrating instrument connects
It connects, extracts 40~800ml gas and enter concentrating instrument；
Step 3: concentrating instrument draws standard by the way that concentrated gas is inputted gas chromatograph-mass spectrometer analysis after the absorption parsing of three-level cold-trap
Curve；
Step 4: concentrated gas is inputted makings after the sample for Ma tank acquisition of reviving is parsed by the absorption of concentrating instrument three-level cold-trap
Combined instrument is analyzed using inner mark method ration, through reference standard curve, respectively obtains Air Hydrogen Sulfide, thiophene, ethyl mercaptan, first
The concentration value of ethyl sulfide, ethyl sulfide.
Preferably, the condition of the concentrating instrument three-level cold-trap absorption parsing is -150 DEG C of level-one cold trap trapping temperature, baking
150 DEG C of temperature, baking time 8min；- 30 DEG C of second level cold trap trapping temperature, 180 DEG C of resolution temperature, 190 DEG C of baking temperature, baking
Time 10min；- 160 DEG C of three-level cold trap trapping temperature, sample injection time 2min, baking time 3min.
Preferably, the chromatographic condition of the gas chromatograph-mass spectrometer analysis is 125 DEG C of injection port, nonpolar capillary column, program liter
50 DEG C of stop 4min of temperature, 120 DEG C of stop 4min are warming up to 20 DEG C/min, are warming up to 220 DEG C of stops with 25 DEG C/min
3min, carrier gas are He gas, column flow rate is 1.2ml/min and without shunting；Mass Spectrometry Conditions are 230 DEG C of ion source temperature, quadrupole rod
150 DEG C, EI voltage 70eV, solvent delay 4 minutes, full scan mode, bromofluoro benzene tuning.
Preferably, the specification of the nonpolar capillary column is 60 m of length, 0.25 mm of internal diameter, 0.25 μm of film thickness；It is described complete
The mass number (mass-to-charge ratio) of scan pattern is 32~37M/Z, and mass number (mass-to-charge ratio) is 35~200M/Z from 5.5 minutes.
Preferably, the connecting pipeline between Soviet Union's Ma tank, concentrating instrument and gas chromatograph-mass spectrometer passes through silanization inertization.
This method is avoided using Soviet Union's Ma tank sampling, pre-concentration trapping and is used liquid oxygen in national standard (GB/T 14678-1993)
The security risk of concentration, while being detected using gas chromatograph-mass spectrometer and improving qualitative accuracy compared with gas Chromatographic Determination, it uses
The step of Soviet Union's Ma tank of silanization samples and analysis, simplifies entire analytic process, the detection suitable for batch air sample.
Concentration gradient configuration 5-200mg/m is established by this method3Standard curve series, 400ml sample volume enter it is pre- dense
Contracting instrument establishes standard curve, the result is shown in Figure 1 and table 1.
Table 1
Abscissa is the time in Fig. 1, and ordinate is abundance, i.e., the ionic strength that Mass Spectrometer Method arrives is being selected as seen from Figure 1
Under analysis condition, 5 kinds of organic sulfur compound good separations.And since the molecular weight of hydrogen sulfide is 34, so setting
Scanning of the mass spectrum range is 32~280 M/Z of mass-to-charge ratio, 35~280 M/Z of mass-to-charge ratio from 6 minutes from 4.5 minutes.In view of sweeping entirely
The mode of retouching has been able to meet the needs of actual sample detection, so selection uses full scan mode, obtain above-mentioned table 1 as a result,
Wherein linearly dependent coefficient is fully able to meet the requirement of quantitative analysis 0.99 or more.
Mark-on (5 mg/m are carried out in blank sample can3) experiment, repeat 6 times, with the relative standard of measurement result
3 times of deviation are used as method detection limit, and the synchronous calculating rate of recovery and precision, the results are shown in Table 2.
Table 2
As can be seen from Table 2, the detection of 5 kinds of organic sulfur compounds is limited to 0.003~0.008 mg/m3, the rate of recovery is 93.9~102.5%,
Precision is 7.5~18.5%, and accuracy and precision are fully able to meet quantitative detection requirement.
It is measured using stationary source sample of this method to certain chemical plant, as a result detects the ethyl mercaptan of high concentration,
Content is between 0.02mg/m3~0.2mg/m3Between, but ethyl mercaptan, this aspect are not detected in the surrounding air near factory
Illustrate that ethyl mercaptan has part to be discharged as the raw material of some chemical industry synthesis, in addition also illustrate that its discharge amount is totally little, spreads
It is diluted substantially after into air, furthermore the property of ethyl mercaptan itself is unstable, the aerial degradation of ethyl mercaptan is also promoted,
Show that this method is completely suitable for the measurement of organic sulfur compound ingredient in air.
Claims (5)
1. the measuring method of organic sulfur compound ingredient in a kind of air, it is characterised in that this method includes the following steps:
Step 1: being sampled using Soviet Union's Ma tank through silanization treatment, automatic clear tank instrument high pure nitrogen pair is used before sampling
Soviet Union's Ma tank is cleaned and is evacuated, repeated multiple times after being analyzed no blank residual, opens Soviet Union's Ma pot valve in sampled point
Door, closing valve takes back laboratory after adopting full sample；
Step 2: using nitrogen as spirit, with Soviet Union's Ma tank dynamic dilution instrument by hydrogen sulfide, thiophene, ethyl mercaptan, methyl ethyl sulfide, second sulphur
Five kinds of organic sulfur calibrating gas of ether are diluted to 10ppb, will be used for the bromochloromethane of assisted quantitative, Isosorbide-5-Nitrae-difluorobenzene, chlorobenzene-D5,
Standard gas is diluted to 100ppb, configured organic sulfur calibrating gas and interior standard gas in 4- bromofluoro benzene and the sample introduction interface of concentrating instrument connects
It connects, extracts 40~800ml gas and enter concentrating instrument；
Step 3: concentrating instrument draws standard by the way that concentrated gas is inputted gas chromatograph-mass spectrometer analysis after the absorption parsing of three-level cold-trap
Curve；
Step 4: concentrated gas is inputted makings after the sample for Ma tank acquisition of reviving is parsed by the absorption of concentrating instrument three-level cold-trap
Combined instrument is analyzed using inner mark method ration, through reference standard curve, respectively obtains Air Hydrogen Sulfide, thiophene, ethyl mercaptan, first
The concentration value of ethyl sulfide, ethyl sulfide.
2. the measuring method of organic sulfur compound ingredient in air according to claim 1, it is characterised in that: the concentrating instrument
The condition of three-level cold-trap absorption parsing is -150 DEG C of level-one cold trap trapping temperature, 150 DEG C of baking temperature, baking time 8min；Two
- 30 DEG C of grade cold trap trapping temperature, 180 DEG C of resolution temperature, 190 DEG C of baking temperature, baking time 10min；Three-level cold trap trapping temperature
Spend -160 DEG C, sample injection time 2min, baking time 3min.
3. the measuring method of organic sulfur compound ingredient in air according to claim 1 or 2, it is characterised in that: the gas
The chromatographic condition of matter combined instrument analysis be 125 DEG C of injection port, nonpolar capillary column, 50 DEG C of stop 4min of temperature programming, with 20 DEG C/
Min is warming up to 120 DEG C of stop 4min, 220 DEG C of stop 3min is warming up to 25 DEG C/min, carrier gas is He gas, column flow rate is
1.2ml/min and without shunting；Mass Spectrometry Conditions are 230 DEG C of ion source temperature, 150 DEG C of quadrupole rod, EI voltage 70eV, solvent delay
4 minutes, full scan mode, bromofluoro benzene tuning.
4. the measuring method of organic sulfur compound ingredient in air according to claim 3, it is characterised in that: the nonpolarity
The specification of capillary column is 60 m of length, 0.25 mm of internal diameter, 0.25 μm of film thickness；The mass number of the full scan mode be 32~
37M/Z, mass number is 35~200M/Z from 5.5 minutes.
5. the measuring method of organic sulfur compound ingredient in air according to claim 3, it is characterised in that: Soviet Union's Ma
Connecting pipeline between tank, concentrating instrument and gas chromatograph-mass spectrometer passes through silanization inertization.
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| CN113433207A (en) * | 2021-07-15 | 2021-09-24 | 广西电网有限责任公司电力科学研究院 | Method for detecting content of carbon disulfide component in sulfur hexafluoride gas |
| CN114324691A (en) * | 2021-12-30 | 2022-04-12 | 江苏省环境监测中心 | Method for improving sulfide detection precision |
| CN114935478A (en) * | 2022-05-31 | 2022-08-23 | 北京博赛德科技有限公司 | ODS component analysis method and analysis system based on same |
| CN115112441A (en) * | 2022-04-27 | 2022-09-27 | 由希华 | Analysis method for simultaneously determining ozone depletion substances and fluorine-containing greenhouse gases in ambient air |
| CN115201367A (en) * | 2022-07-11 | 2022-10-18 | 中国计量科学研究院 | Method for detecting sulfur-containing organic compounds in pollution source |
| CN115436148A (en) * | 2022-09-02 | 2022-12-06 | 北京博赛德科技有限公司 | Online automatic dilution and concentration dual-mode system and online detection method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110031587A (en) * | 2019-05-21 | 2019-07-19 | 中国测试技术研究院化学研究所 | Measure the pre-concentration-gas chromatograph and detection method of sulfide content in hydrogen |
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| CN113433207A (en) * | 2021-07-15 | 2021-09-24 | 广西电网有限责任公司电力科学研究院 | Method for detecting content of carbon disulfide component in sulfur hexafluoride gas |
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| CN115112441A (en) * | 2022-04-27 | 2022-09-27 | 由希华 | Analysis method for simultaneously determining ozone depletion substances and fluorine-containing greenhouse gases in ambient air |
| CN114935478A (en) * | 2022-05-31 | 2022-08-23 | 北京博赛德科技有限公司 | ODS component analysis method and analysis system based on same |
| CN115201367A (en) * | 2022-07-11 | 2022-10-18 | 中国计量科学研究院 | Method for detecting sulfur-containing organic compounds in pollution source |
| CN115201367B (en) * | 2022-07-11 | 2024-01-26 | 中国计量科学研究院 | Method for detecting sulfur-containing organic compounds in pollution sources |
| CN115436148A (en) * | 2022-09-02 | 2022-12-06 | 北京博赛德科技有限公司 | Online automatic dilution and concentration dual-mode system and online detection method thereof |
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