CN101539549A - Photoionization gas chromatography detection method of organic volatile compounds in air - Google Patents
Photoionization gas chromatography detection method of organic volatile compounds in air Download PDFInfo
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- CN101539549A CN101539549A CN200910094414A CN200910094414A CN101539549A CN 101539549 A CN101539549 A CN 101539549A CN 200910094414 A CN200910094414 A CN 200910094414A CN 200910094414 A CN200910094414 A CN 200910094414A CN 101539549 A CN101539549 A CN 101539549A
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- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 150000001875 compounds Chemical class 0.000 title claims abstract description 6
- 238000004817 gas chromatography Methods 0.000 title abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005070 sampling Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000010812 external standard method Methods 0.000 claims abstract description 5
- 238000010813 internal standard method Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 67
- 239000012855 volatile organic compound Substances 0.000 claims description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000000523 sample Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 4
- 239000012749 thinning agent Substances 0.000 claims description 4
- 238000012417 linear regression Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 239000012496 blank sample Substances 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 238000003795 desorption Methods 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 239000002594 sorbent Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 45
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 30
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003822 preparative gas chromatography Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 230000005477 standard model Effects 0.000 description 2
- 230000009897 systematic effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The invention relates to a photoionization (PID) gas chromatography detection method of organic volatile compounds in the air. The n-hexane internal standard method or the standard gas external standard method is used for detection. The detection method is characterized by fast response speed, high sensitivity and low detection limit (not more than 10ppb); the detection method can use a sampler for collecting gas and then directly inject a sample to a chromatograph for test and can also bring the chromatograph to the test site and complete the sampling from the environmental air, the sample injection and the test at one time. The detection method does not need to use a solid sorbent for concentration and does not need to carry out desorption by thermal desorption. Therefore, the detection method simplifies the detection procedure, reduces the system error and the random error caused during the absorption, the desorption and the extraction processes, greatly shortens the detection cycle and leads the detection result to be more accurate.
Description
Technical field
The present invention relates to a kind of organic gas detection technique field, specifically the photoionization gas chromatogram detection method of organic volatile (VOCs) in the air.
Background technology
(Gas Chromatography is to utilize material different partition factor, adsorption coefficient or perviousness in the solid and gas two-phase to realize analyzing and testing GC) to vapor-phase chromatography.Common flame ion (FID) vapor-phase chromatography need be burning gases with hydrogen during detection, temperature, firing rate when therefore needing temperature-controlled cabinet accurately to control temperature, the rate of heat addition and parsing.Whole detection system more complicated, bulky, can only in the laboratory, use.In addition owing to be subjected to the performance limitations of (FID) detecting device, detection speed, sensitivity and detect precision etc. and all be restricted.Airborne harmful gas is detected, need earlier to concentrate (gas absorption to be measured in solid adsorbent), by thermal desorption device gas desorption from adsorbent is come out to detect then with solid adsorbent.So not only increased absorption, the desorption process of sample, made sense cycle elongated, the more important thing is and in sample preparation, introduced new systematic error and stochastic error and the low problem of the desorption recovery.
Summary of the invention
The photoionization gas chromatogram detection method that the purpose of this invention is to provide organic volatile in a kind of air (VOCs).This method is applied to a kind of photoionization (PID) gas chromatographic technique to detect the concentration of organic volatile VOCs in the air.
Photoionization (PID) vapor-phase chromatography is a kind of new gas detection technology.Tested gas enters instrument, after separating by chromatographic column, is bombarded by vacuum ultraviolet photon, can make organic volatile (VOCs) wherein be ionized into negative ions.Measure the size of gas current by detecting device, just can determine the concentration of different VOCs, have fast, the highly sensitive characteristics of response speed.The present invention is, based on the characteristics of PID gas chromatographic technique, make a kind of comprehensive syringe container, create new analytical approach, form the complete detection system of a cover, be applied to the qualitative and detection by quantitative of harmful gas in the air (organic volatile that comprises benzene, toluene and dimethylbenzene).
Technical scheme of the present invention is:
1. detection system comprises: comprehensive syringe container (can be used for gathering gas and direct injecting chromatograph, also can be used for preparing calibrating gas and direct injecting chromatograph), chromatograph (comprises chromatographic column, vacuum UV lamp and PID detecting device, be respectively applied for the detection of separation, ionization and the ionization current of gas), analyzer is (respectively by internal standard method and external standard method, the chromatographic peak that the PID detecting device is detected carries out analytical calculation, draws qualitative, quantitative result).
2. detection step:
Method one: normal hexane internal standard method
(1) at first adding quality in the syringe distribution container that is filled with 1L (volume under the standard state) high pure nitrogen is the VOCs standard solution of m, the hexane solution that adds equal in quality simultaneously is as internal standard compound matter, mix, be mixed with the deposit gas that every kind of VOC concentration is m/L.With high purity nitrogen deposit gas is diluted 1000 times again during use and make concentration C
J=m/1000L is as interior gas body, and direct injected 10.0mL accurately measures the peak area (as Fig. 1) of normal hexane and VOCs calibrating gas.Calculate the relative calibration factor of VOCs with following formula:
In the formula:
f
iThe calibration factor of-VOCs;
S
iThe peak area of VOCs in-Nei gas body;
S
jThe peak area of-normal hexane;
C
jVOCs concentration in-Nei gas body.
(2) gather 1L (volume under the standard state) gas to be measured with sampling syringe container in air, adding 1mL concentration is normal hexane/nitrogen of m/L, and after mixing, direct injected 10.0mL detects the peak area of normal hexane and VOCs to be measured.
Calculate the concentration of VOCs according to following formula
In the formula:
C
iThe concentration of VOCs in the-air;
S
iThe peak area of VOCs in the-air;
S
jThe peak area of normal hexane in the-air
Method two: calibrating gas external standard method
(1) be that thinning agent extracts various VOCs standard solution 5 μ L and is mixed with the VOCs storing solution that concentration is 1 μ L/mL with methyl alcohol in the volumetric flask of 5mL.With syringe distribution container storing solution being diluted vaporization respectively when using is made into concentration and is C
1, C
2, C
3, C
4The VOCs calibrating gas, direct injected 10.0mL accurately measures the peak area S of every group of concentration VOCs
Ij(as Fig. 2).With VOC
SConcentration be horizontal ordinate, the respective peaks area is an ordinate drawing standard curve.Draw the slope of straight line by linear regression, get the calculated factor of its B reciprocal as sample determination.
(2) gather 1L (volume under the standard state) gas to be measured with sampling syringe distribution container, direct injected 10.0mL detects the peak area of VOCs to be measured.Calculate the concentration of VOCs according to following formula:
C
i＝(S
i-S)B (3)
In the formula:
C
iThe concentration of tested VOCs in the-air;
S
iThe peak area of VOCs in the-air;
The peak area of the blank sample of S-;
The calculated factor of B-sample determination.
Characteristics of the present invention:
1.PID vapor-phase chromatography is to organic volatile detection sensitivity height, response speed is fast.Use this method and detect organic volatile in the air, do not need absorption, concentrate and link such as desorption, the gas that collects, the gas of sample introduction and gas concentration to be checked are consistent, therefore, and can be with the syringe direct injected of sampling.Testing process is easy and simple to handle, quick, and the comparable hydrogen flame gas of its speed phase chromatography improves more than 10 times, and has reduced the additive error that the too many levels operation is brought into;
2. the gas sampling volume reaches 10mL or bigger, improves more than 10 times than conventional gas sampling volume, makes the also corresponding significantly raising of precision of sample introduction;
3. in internal standard method,, can effectively eliminate the most of systematic error in the test, measuring accuracy is further improved by normal hexane internal standard compound matter;
4. in the calibrating gas external standard method, adopt methanol liquid as thinning agent, following characteristics arranged:
(1) in identical container, can strengthen the preparation dosage (5 μ L) of standard model, thereby when having reduced conventional method preparation standard model, the stochastic error that dosage brings for a short time;
(2) methyl alcohol can mix with most of organism, and does not go out the peak in the PID chromatogram, therefore can be used for the organic preparation of a lot of standards and can not disturb their peak intensity and measuring accuracy.
Description of drawings
Fig. 1 is the chromatogram of internal standard compound normal hexane and VOCs calibrating gas;
Fig. 2 is. concentration is C
1, C
2, C
3, C
4VOCs calibrating gas chromatogram;
Embodiment
Embodiment 1:
The concentration determination of benzene, toluene and dimethylbenzene in the laboratory.
Detection system comprises: comprehensive syringe container, chromatograph, analyzer.
Detect step:
1, sampling: gather 1L (volume under the standard state) air at the scene with the gas sampling syringe, be sealed into gas port;
2, measure calibration factor: get normal hexane, benzene, toluene and the adding of dimethylbenzene normal fluid that quality is 0.5mg respectively and be full of in the sampler bag of 1L high pure nitrogen, be mixed with deposit gas.With high purity nitrogen deposit gas is diluted 1000 times again in another distribution syringe, the concentration that is configured to normal hexane, benzene, toluene and dimethylbenzene is the interior gas body of 0.5mg/1000L; Open the chromatograph power supply, preheating 30min transfers to 50 ℃ with working temperature, pressure 6pa; Carrier gas flux transfers to 15mL/min, and interior gas body direct injected 10.0mL starts instrument.From Fig. 1, measure the retention time and the peak area of normal hexane, benzene, toluene and dimethylbenzene, calculate the calibration factor (the results are shown in Table 1) of benzene, toluene and dimethylbenzene according to formula (1)
Table 1: the calibration factor 3 of benzene, toluene and dimethylbenzene in the calibrating gas
| Benzene (f 1) | Toluene (f 2) | Dimethylbenzene (f 3) |
| 0.142mg/m 3 | 0.125mg/m 3 | 0.20mg/m 3 |
3, quantitative test: in the syringe distribution container that is filled with 1L (volume under the standard state) high pure nitrogen, add the 0.5mg normal hexane, get after mixing in the gas sampling syringe to be measured of 1mL gas implantation step one, after mixing once more, direct injected 10.0mL, measure the peak area of normal hexane, benzene, toluene and dimethylbenzene according to the method for step 2, calculate the concentration (the results are shown in Table 2) of benzene, toluene and dimethylbenzene according to formula (2).
Table 2: the concentration of benzene, toluene and dimethylbenzene in the gas to be measured
| Benzene (C 1) | Toluene (C 2) | Dimethylbenzene (C 3) |
| 0.002mg/m 3 | 0.003mg/m 3 | 0.001mg/m 3 |
Embodiment 2:
The concentration determination of office indoor VOCs.
Detection system comprises: comprehensive syringe container, chromatograph, analyzer.
Detect step:
1, sampling: gather 1L (volume under the standard state) air at the scene with the gas sampling syringe, be sealed into gas port.
2, drawing standard curve: in the 5mL volumetric flask, be that thinning agent is mixed with the VOCs storing solution that concentration is 1 μ L/mL with methyl alcohol.With the 100mL syringe storing solution being diluted vaporization respectively again, to be made into concentration be C
1=0.10mg/m
3, C
2=0.20mg/m
3, C
3=0.30mg/m
3, C
4=0.40mg/m
3The VOCs calibrating gas.Open the chromatograph power supply, preheating 30min transfers to 50 ℃ with working temperature, pressure 6pa; Carrier gas flux transfers to 15mL/min, and calibrating gas direct injected 10.0mL starts instrument.From Fig. 2, measure the retention time and the peak area of each component VOCs calibrating gas respectively, with VOC
SConcentration be horizontal ordinate, the respective peaks area is an ordinate drawing standard curve.Draw the slope of straight line by linear regression, and obtain the calculated factor (the results are shown in Table 3) of VOCs respectively
The calculated factor of table 3:VOCs calibrating gas
| Benzene (B 1) | Toluene (B 2) | Ethylbenzene (B 3) | Dimethylbenzene (B 4) | Styrene (B 5) |
| 0.0015 | 0.0010 | 0.0030 | 0.0007 | 0.0020 |
3, quantitative test: direct injected 10.0mL gas from gas sampling syringe to be measured, measure the peak area of VOCs according to the method for step 2, calculate the concentration (the results are shown in Table 4) of benzene, toluene and dimethylbenzene according to formula (2).
Table 4: the concentration of VOCs in the gas to be measured
| Benzene (C 1) | Toluene (C 2) | Ethylbenzene (C 3) | Dimethylbenzene (C 4) | Styrene (C 5) |
| 0.002mg/m 3 | 0.01mg/m 3 | 0.00mg/m 3 | 0.03mg/m 3 | 0.00mg/m 3 |
Claims (1)
1, the photoionization gas chromatogram detection method of organic volatile in a kind of air is characterized in that carrying out according to the following steps:
Method 1: normal hexane internal standard method
1) at first adding quality in the syringe distribution container of the volume high pure nitrogen under being filled with 1L standard state is the VOCs standard solution of m, the hexane solution that adds equal in quality simultaneously is as internal standard compound matter, mix, be mixed with every kind of VOC concentration and be the deposit gas of m/L, will lay in gas during use and be diluted to concentration C
JThe interior gas body of=m/1000L, direct injected 10.0mL accurately measures the peak area of normal hexane and VOCs calibrating gas, calculates the relative calibration factor of VOCs with following formula:
In the formula:
f
iThe calibration factor of-VOCs;
S
iThe peak area of VOCs in-Nei gas body;
S
jThe peak area of-normal hexane;
C
jVOCs concentration in-Nei gas body.
2) usefulness sampling syringe container is gathered the volume gas to be measured under the 1L standard state in air, adding 1mL concentration is normal hexane/nitrogen of m/L, after mixing, and direct injected 10.0mL, detect the peak area of normal hexane and VOCs to be measured, calculate the concentration of VOCs according to following formula
In the formula:
C
iThe concentration of VOCs in the-air;
S
iThe peak area of VOCs in the-air;
S
jThe peak area of normal hexane in the-air
Method 2: calibrating gas external standard method
1) is that thinning agent extracts various VOCs standard solution 5 μ L and is mixed with the VOCs storing solution that concentration is 1 μ L/mL with methyl alcohol in the volumetric flask of 5mL, with syringe distribution container storing solution diluted vaporization respectively when using and be made into concentration and be C
1, C
2, C
3, C
4The VOCs calibrating gas, direct injected 10.0mL accurately measures the peak area S of every group of concentration VOCs
Ij, be horizontal ordinate with the concentration of VOCs, the respective peaks area is an ordinate drawing standard curve, draws the slope of straight line by linear regression, gets the calculated factor of its B reciprocal as sample determination;
2) gather volume gas to be measured under the 1L standard state with sampling syringe distribution container, direct injected 10.0mL detects the peak area of VOCs to be measured, calculates the concentration of VOCs according to following formula:
C
i＝(S
i-S)B (3)
In the formula:
C
iThe concentration of tested VOCs in the-air;
S
iThe peak area of VOCs in the-air;
The peak area of the blank sample of S-;
The calculated factor of B-sample determination.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910094414A CN101539549A (en) | 2009-04-29 | 2009-04-29 | Photoionization gas chromatography detection method of organic volatile compounds in air |
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| Publication Number | Publication Date |
|---|---|
| CN101539549A true CN101539549A (en) | 2009-09-23 |
Family
ID=41122854
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|---|---|---|---|
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|---|---|---|---|---|
| CN102539203A (en) * | 2010-12-30 | 2012-07-04 | 深圳光启高等理工研究院 | Method for preparing ethyl nitrite standard gas with any concentration |
| CN104764862A (en) * | 2015-05-05 | 2015-07-08 | 西安近代化学研究所 | Gas concentration site testing method |
| CN105136958A (en) * | 2015-09-15 | 2015-12-09 | 顾金华 | VOC (Volatile Organic Compound) concentration online monitoring device |
| CN105136992A (en) * | 2015-09-15 | 2015-12-09 | 顾金华 | VOC (Volatile Organic Compound) concentration online monitoring device and VOC concentration online monitoring method thereof |
| CN109164163A (en) * | 2018-08-30 | 2019-01-08 | 亚翔***集成科技（苏州）股份有限公司 | VOC detection method in a kind of toilet |
| CN109781896A (en) * | 2019-03-07 | 2019-05-21 | 西北大学 | A kind of analysis method of standard series and gaseous sample based on internal standard method |
| CN114252496A (en) * | 2022-03-01 | 2022-03-29 | 河北沃茵环保科技有限公司 | VOCs online automatic monitoring system |
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2009
- 2009-04-29 CN CN200910094414A patent/CN101539549A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539203A (en) * | 2010-12-30 | 2012-07-04 | 深圳光启高等理工研究院 | Method for preparing ethyl nitrite standard gas with any concentration |
| CN104764862A (en) * | 2015-05-05 | 2015-07-08 | 西安近代化学研究所 | Gas concentration site testing method |
| CN104764862B (en) * | 2015-05-05 | 2016-08-17 | 西安近代化学研究所 | A kind of gas concentration on-the-spot test method |
| CN105136958A (en) * | 2015-09-15 | 2015-12-09 | 顾金华 | VOC (Volatile Organic Compound) concentration online monitoring device |
| CN105136992A (en) * | 2015-09-15 | 2015-12-09 | 顾金华 | VOC (Volatile Organic Compound) concentration online monitoring device and VOC concentration online monitoring method thereof |
| CN105136992B (en) * | 2015-09-15 | 2017-01-25 | 顾金华 | VOC (Volatile Organic Compound) concentration online monitoring device and VOC concentration online monitoring method thereof |
| CN109164163A (en) * | 2018-08-30 | 2019-01-08 | 亚翔***集成科技（苏州）股份有限公司 | VOC detection method in a kind of toilet |
| CN109781896A (en) * | 2019-03-07 | 2019-05-21 | 西北大学 | A kind of analysis method of standard series and gaseous sample based on internal standard method |
| CN109781896B (en) * | 2019-03-07 | 2022-06-17 | 西北大学 | Standard series and gas sample analysis method based on internal standard method |
| CN114252496A (en) * | 2022-03-01 | 2022-03-29 | 河北沃茵环保科技有限公司 | VOCs online automatic monitoring system |
| CN114252496B (en) * | 2022-03-01 | 2022-05-17 | 河北沃茵环保科技有限公司 | VOCs online automatic monitoring system |
| CN114487211A (en) * | 2022-03-16 | 2022-05-13 | 河北科技大学 | GC-FID monitoring method and system for monitoring volatile organic compounds in second-level real time |
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