CN110346474A - TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample - Google Patents
TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample Download PDFInfo
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- CN110346474A CN110346474A CN201910680947.4A CN201910680947A CN110346474A CN 110346474 A CN110346474 A CN 110346474A CN 201910680947 A CN201910680947 A CN 201910680947A CN 110346474 A CN110346474 A CN 110346474A
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- filter membrane
- injection method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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Abstract
The invention discloses the sample injection method of nonpolar organic matter on a kind of TD-GCMS measurement gradation diameter aerosol sample, the sample injection method is by being acquired analysis according to sample spot to sample of the acquisition on each filter membrane after gradation diameter.This method operates clear thinking, will determine area-method and is changed into fixed-point number method, it is ensured that the accuracy of sample volume.
Description
Technical field
The present invention relates to a kind of sample injection methods of nonpolar organic matter on gradation diameter aerosol sample.
Background technique
Atmospheric particulates are the major pollutants for endangering human health and influencing atmosphere quality, in global climate
It plays an important role in terms of environmental change, these are influenced or effect is mainly related with its concentration, chemical composition and particle diameter distribution.
When studying atmospheric aerosol, usually first aerosol is collected on certain carrier using sampler, is adopted further according to different purposes
Analysis measurement is carried out to aerosol sample with different means, quartz filter is common aerosol sample carrier.Aerosol sample
Product acquisition has gradation diameter and regardless of partial size two ways: referring to regardless of partial size sample will be within certain aerodynamic diameter (Dp)
Atmospheric particulates all acquisition on a filter membrane (with PM10It is that aerosol of all Dp within 10 μm is complete for sample
Portion acquires on a filter membrane)；And gradation diameter sample, the Atmospheric particulates within certain Dp are exactly further partitioned into different grains
Diameter section is acquired respectively on different filter membranes, with Andersen sampler (Andersen 1ACFM abiotic environment particle size point
Grade sampler) for, it is exactly by PM10It is divided into 9 partial size sections (as shown in Figure 1) again, the sample of each partial size section acquires respectively
On a filter membrane.
Gu currently, the measuring method of nonpolar organic compound mainly has gas chromatography tandem mass spectrometry method, accelerates solvent-
Phase extraction-high performance liquid chromatography and thermal desorption-gas chromatography mass spectrometry etc..Thermal desorption-gas chromatography mass spectrometry (TD-GCMS)
Cardinal principle is aerosol sample to be incorporated with the absorption of solid absorbent to claim pipe, then claims pipe to be put into thermal desorption instrument absorption
In, after gas-chromatography separates, detected with mass spectrum.This method can direct injected, reduce sample loss, and overcome biography
The deficiency of system pre-treating method.
For the aerosol sample regardless of partial size, depressor (Punch) generally is worn with circle and cuts certain area from filter membrane
(determining area-method) is analyzed；And when being analyzed using TD-GCMS gradation diameter sample, determining area-method is but not suitable for, main
Want there is relatively large blank between points the reason is that gradation diameter sample is in uniform, discrete spot distribution on filter membrane
Region determines area-method and human error is easy to cause to increase when sample volume is lesser, and experiment collimation is deteriorated.
Summary of the invention
The purpose of the present invention is to solve defects existing in the prior art, and gradation diameter can be accurately controlled by providing one kind
Aerosol sample sample volume, the sample injection method for reducing human error, improving experiment collimation.
To achieve the goals above, the present invention provides nonpolarity on TD-GCMS measurement gradation diameter aerosol sample is organic
The sample injection method of object, the sample injection method is by being acquired point sample of the acquisition on each filter membrane after gradation diameter according to sample spot
Analysis.
Further, the sample injection method is by carrying out fixed-point number analysis to each filter membrane: taking a certain number of samples on filter membrane
Point, the quality of nonpolar organic matter to be measured in the sample that sample introduction is analyzed account for gross sample on filter membrane in conjunction with the sample spot quantity taken
The ratio of product points, calculates nonpolar organic matter to be measured concentration in an atmosphere.
Further, the calculation formula of nonpolar organic matter to be measured concentration c in an atmosphere are as follows:
Wherein, c is the concentration of target compound in an atmosphere, and V is atmosphere volume, m and m1Respectively target compound exists
Quality in atmosphere in quality and sample, s and s1The total points and sample introduction points of sample respectively on filter membrane.
Further, sample spot is sampled by the following method: successively being eluted using methanol, methylene chloride, n-hexane
Scissors, then the filter membrane part with quantity sample spot to be sampled is cut, it is used for sample introduction.
Further, the sample spot quantity of clip is 4-8 point on 0 and 1 grade of filter membrane, on the filter membrane of remaining rank
The sample spot quantity of clip is 22 points, and situation adjusts slightly according to specific experiments.
The present invention has the advantage that compared with prior art
(1) this method operate clear thinking, area-method will be determined and be changed into fixed-point number method, it is ensured that sample volume it is accurate
Property.
(2) this method can utilize sample to greatest extent, theoretically can completely avoid waste.
(3) this method is easy to operate, and reduces human error, enhances the collimation of experiment.
Detailed description of the invention
Fig. 1 is the schematic diagram that the small traffic sampling device of THERMO-ANDERSEN carries out cascade sampling；
Fig. 2 is the clip schematic diagram of gradation diameter sampling membrane of the present invention.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
As shown in Fig. 2, the Atmospheric particulates being collected into due to gradation diameter collector are on filter membrane in uniform, discrete dotted
Distribution, therefore when with TD-GCMS method test sample, it, can be due between each discrete point when using determining area-method progress sample clip
Increase human error there are relatively large white space, therefore, the present invention is sampled by fix point method.
TD-GCMS of the present invention measures the sample injection method specific steps of nonpolar organic matter on gradation diameter aerosol sample such as
Under:
(1) according to filter membrane grade and clean Cheng Chengdu (i.e. thereon adsorption sample number), the point sheared required for judging
Number.
The sample spot quantity of clip generally on the filter membrane of 0 and 1 grade (by taking classification of the small traffic sampling device in Anderson as an example)
For 4-8 point, the sample spot quantity of clip is 22 points on the filter membrane of remaining rank, can be according to the clean level of specific filter membrane
Slightly adjust.(classification is only in the small traffic sampling device of Anderson gradation diameter)
(2) sample accordingly counted is cut with scissors (needing successively to be eluted with methanol, methylene chloride, n-hexane before use)
(as shown in Fig. 2, carrying out clip along dotted line) is packed into absorption with tweezers and claims pipe, measured using TD-GCMS method.
(3) analysis instrument gas chromatography mass spectrometer (AgilentGC7890B/MS5977A) instrument test condition is as follows:
Chromatographic condition is high separation gas chromatographic column (long 30m, internal diameter 0.25mm, 0.25 μm of coating), chromatography heating journey
Sequence are as follows: initial temperature is 35 DEG C, 3min is kept, then with 10 DEG C of min-1120 DEG C are warming up to, then with 4 DEG C of min-1It is warming up to
146 DEG C, finally with 8 DEG C of min-1310 DEG C are warming up to, 16min is kept.Injection port initial temperature is 35 DEG C, with 12 DEG C of s-1It rises
Temperature keeps 2978s to 300 DEG C.Mass spectrum is 310 DEG C with EI mode operation, electron energy 70eV, ion source temperature, and carrier gas is height
Pure helium, flow velocity 1.0mLmin-1, input mode is 5 times of shunt modes.
(4) qualitative to target compound using retention time and characteristic ion, quantitative to target compound by external standard method:
The standard solution for preparing a series of different quality concentration (0.1,0.2,0.5,1,2,5,10,15 μ g/mL), is successively moved with micro needle
The above-mentioned concentration series solution injection absorption of 1.0 μ L is taken to claim to be measured and draw standard curve in pipe, to determine target compound
The range of linearity and for quantitative.
(5) concentration of target compound in atmosphere is calculated according to the following formula:
Wherein, c is the concentration of target compound in an atmosphere, and V is atmosphere volume, m and m1Respectively target compound exists
Quality in atmosphere in quality and sample, s and s1The total points and sample introduction points of sample respectively on filter membrane.
It is measured using the Atmospheric particulates that the method for the present invention is collected into gradation diameter collector:
The a collection of atmospheric aerosol sample of winter Linfen in 2017 is tested, table 1 is the test sample point of filter membranes at different levels
Several and sampling number:
1 test sample of table points and sampling number
* the 8 grade of point and point are intensive, cut when being equivalent to particulate matter and be laid in entire plane, therefore sampling with Punch (3mm)
Take 2 points, area 7.065mm2
By this method measure on filter membranes at different levels nonpolar organic compound (mainly include polycyclic aromatic hydrocarbon, n-alkane,
Hopance, gonane), content is as shown in table 2:
Table 2 measures content (the ng m of each nonpolar organic compound-3)
Claims (5)
1.TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample, it is characterised in that: the sample introduction
Method is by being acquired analysis according to sample spot to sample of the acquisition on each filter membrane after gradation diameter.
2. sample injection method according to claim 1, it is characterised in that: the sample injection method is by carrying out fixed-point number to each filter membrane
Analysis: taking a certain number of sample spots on filter membrane, the quality of nonpolar organic matter to be measured in the sample that sample introduction is analyzed, in conjunction with being taken
The sample spot quantity account for the ratio that gross sample on filter membrane is counted, calculate nonpolar organic matter to be measured concentration in an atmosphere.
3. sample injection method according to claim 2, it is characterised in that: the nonpolar organic matter to be measured concentration in an atmosphere
The calculation formula of c are as follows:
Wherein, c is the concentration of target compound in an atmosphere, and V is atmosphere volume, m and m1Respectively target compound is in an atmosphere
Quality in quality and sample, s and s1The total points and sample introduction points of sample respectively on filter membrane.
4. sample injection method according to claim 3, it is characterised in that: the sample spot is sampled by the following method:
Scissors is successively eluted using methanol, methylene chloride, n-hexane, then cuts the filter membrane part with quantity sample spot to be sampled, is used
In sample introduction.
5. sample injection method according to claim 4, it is characterised in that: the sample spot quantity of clip on 0 and 1 grade of filter membrane
For 4-8 point, the sample spot quantity of clip is 22 points on the filter membrane of remaining rank.
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| CN101881758A (en) * | 2010-06-25 | 2010-11-10 | 南开大学 | Method for measuring phthalic ester in atmospheric particulates |
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| CN103157381A (en) * | 2011-12-16 | 2013-06-19 | 中国石油化工股份有限公司 | Judgment method of reverse osmosis membrane microbial contamination and application |
| CN103472166A (en) * | 2013-08-02 | 2013-12-25 | 中国科学院地球环境研究所 | Method for directly measuring organic materials in aerosol at injection port by using thermal desorption-gas chromatography-mass spectrometry |
| CN105928840A (en) * | 2016-04-13 | 2016-09-07 | 南开大学 | Method using single point adsorption method to measure specific surface area of atmospheric particulates |
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2019
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| CN102081066A (en) * | 2009-11-27 | 2011-06-01 | 复旦大学 | High time resolution microsampling method of atmospheric aerosol |
| CN101881758A (en) * | 2010-06-25 | 2010-11-10 | 南开大学 | Method for measuring phthalic ester in atmospheric particulates |
| CN103157381A (en) * | 2011-12-16 | 2013-06-19 | 中国石油化工股份有限公司 | Judgment method of reverse osmosis membrane microbial contamination and application |
| CN103472166A (en) * | 2013-08-02 | 2013-12-25 | 中国科学院地球环境研究所 | Method for directly measuring organic materials in aerosol at injection port by using thermal desorption-gas chromatography-mass spectrometry |
| CN105928840A (en) * | 2016-04-13 | 2016-09-07 | 南开大学 | Method using single point adsorption method to measure specific surface area of atmospheric particulates |
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Application publication date: 20191018 |