CN107064321A - A kind of method of volatile organic content in measure industrial waste gas - Google Patents
A kind of method of volatile organic content in measure industrial waste gas Download PDFInfo
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- CN107064321A CN107064321A CN201611004521.XA CN201611004521A CN107064321A CN 107064321 A CN107064321 A CN 107064321A CN 201611004521 A CN201611004521 A CN 201611004521A CN 107064321 A CN107064321 A CN 107064321A
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Abstract
The present invention is for the deficiency for analyzing waste gas collecting the certain methods such as time-consuming, cost height existing at present, real-time monitoring to industrial waste gas Volatile Organic Components and content is realized by a kind of quick industrial waste gas sampling analysis, a kind of simplicity, fast and accurately Simple, Practical Determination Method of VOCs is set up.The assay method sample pretreatment process that the present invention is provided is simple, and whole operation automaticity is high, can realize the continuity of measure, and the sensitivity determined is high, and method and scientific basis are provided for current industrial waste gas volatile solvent content detection.
Description
Technical field
The invention belongs to detection technique field, and in particular to the side of volatile organic content in a kind of measure industrial waste gas
Method.
Background technology
VOC（Volatile organic compound, abbreviation volatile organic matter）Refer to boiling point
Compound of the scope at 50 DEG C ~ 250 DEG C, according to the definition of the World Health Organization, volatile organic matter refers to that saturation is steamed at 25 DEG C
Air pressure is present in the class volatile organic matter in air in vapour form at normal temperatures more than 133.32Pa.
VOC main source includes the incomplete of industrial waste gas, vehicle exhaust, domestic fuel and tobacco leaf
Burning and interior architecture ornament materials etc..The industrial waste gas wherein produced in chemical industry process of factory production is the volatilization in air
The main source of property Organic Pollution, and be mostly based on benzene homologues, such as in PX plant produceds, waste gas it is main into
It is benzene to divide, and remainder is almost substituted benzene toluene and dimethylbenzene.This pollutant easily passes through respiratory system and skin
It is absorbed by the body, the nervous system of harmful to human, or even carcinogenic, teratogenesis.Therefore, for this kind of noxious volatile in industrial waste gas
The detection and research of organic matter are of great interest, and various countries have formulated corresponding discharge standard.
At present, the detection method for volatile organic matter in industrial waste gas mainly has gas chromatography, spectroscopic methodology etc..Mesh
Before, state specified standards detection method is gas chromatography, because this method sensitivity is high, quantitative result is accurate.But sample
Product pretreatment process is complicated, it is necessary to which by processes such as gas collecting, enrichment, concentrations, acquisition cost is high, it is long to expend the time, simultaneously
Sample can cause damage in processing procedure.
The content of the invention
Contain it is an object of the invention to provide volatile organic matter in a kind of Static Headspace-gas Chromatographic Determination industrial waste gas
The method of amount.
To achieve the above object, the present invention is using volatile organic matter in Static Headspace-gas Chromatographic Determination industrial waste gas
The method of content, it is characterised in that waste gas sample is directly taken in Chemical Manufacture, without further sample pretreatment, directly
Heated and balanced using Static Headspace injector, reached after balance, headspace sampling (takes upper air body injection gas-chromatography in ml headspace bottle
Instrument is separated) so that effective carry out volatile organic matter to be measured to separate and accurate quantitative analysis.Wherein gas-chromatography is used
DB-WAX chromatographic columns, quantitative approach is quantified by external standard method.
The method of volatile organic content in a kind of Static Headspace-gas Chromatographic Determination industrial waste gas, it is characterised in that：
This method comprises the following steps：
The preparation of volatile organic matter mixed standard solution：The accurate pure material for weighing 9 kinds of chromatographically pure volatile organic matters, is first used
Chromatographic Pure Methanol is made into a high concentration mixed standard solution as deposit mother liquor；Again with methanol dilute step by step be configured to it is a series of
The mixed standard solution of various concentrations gradient；
The detection of volatile organic matter mixed standard solution and the drafting of standard curve：The accurate removing step 1 of difference）One obtained
Serial mixed standard solution is respectively put into head-space sampler and detected into the headspace sampling bottle for the number of finishing；With each
The chromatographic peak area X of organic matter is the standard gas concentration Y (mg/m in abscissa, its corresponding ml headspace bottle3) drawn for ordinate
The standard curve of every kind of volatile organic matter, calculates the regression equation for obtaining each standard curve；
Waste gas sample is sampled and handled：In the sampling of waste gas monitoring point, the host solvents of the volume as standard sample are rapidly added, will
The testing sample bottle of acquisition seals rapidly to be measured.
The measure of volatile organic content in waste gas sample：Waste gas testing sample bottle is put into head-space sampler and carried out
After balance, automatic headspace sampling carries out separation and quantitative detection.The chromatographic peak area of obtained various volatile organic matters is distinguished
Substitute into its corresponding regression equation, you can obtain the content of various volatile organic matters in waste gas.
Wherein, in described mixed standard solution, the concentration of various volatile organic matters is 0.1 ~ 2.0 μ g/mL；
Described headspace sampling condition is：80 DEG C of Sample equilibration temperature；95 DEG C of sample amounts circumstance temperature degree；Sample transfer line temperature
105℃；The min of Sample equilibration time 10.；The psi of sample bottle moulding pressure 15；The psi of nebulizer gas pressure 30；Pressing time 0.20
min；The min of inflationtime 0.20；The min of sample loop equilibration time 0.05；The min of sample injection time 1.
The volume of described addition mixed standard solution is 10 μ L.
Described GC conditions are：Chromatographic column is DB-WAX（30 m×0.32 mm×0.25 μm）；Injection port temperature
160 DEG C of degree；Carrier gas is high-purity N2（Purity >=99.999%）；The mL/min of flow velocity 3.0；Split ratio 2: 1；Heating schedule：Initial temperature
40 DEG C of 2 min of holding of degree, then 70 DEG C are risen to 10 DEG C/min speed, 70 DEG C retain after 6 min with 20 DEG C/min speed liter
To 180 DEG C, 1 min is kept；
The present invention is for the deficiency for analyzing waste gas collecting the certain methods such as time-consuming, cost height existing at present, by a kind of quick
Real-time monitoring of the industrial waste gas sampling analysis realization to industrial waste gas Volatile Organic Components and content, a kind of simplicity of foundation,
Fast and accurately Simple, Practical Determination Method of VOCs.The assay method sample pretreatment process that the present invention is provided is simple, whole behaviour
Make automaticity high, the continuity of measure can be realized, and the sensitivity determined is high, is that current industrial waste gas volatility is molten
Agent content detection provides method and scientific basis.
Brief description of the drawings
Fig. 1 is the chromatogram of volatile organic matter standard liquid.
Fig. 2 is the standard working curve figure of hexamethylene.
Fig. 3 is the standard working curve figure of benzene.
Fig. 4 is the standard working curve figure of toluene.
Fig. 5 is the standard working curve figure of butyl ester.
Fig. 6 is the standard working curve figure of ethylbenzene.
Fig. 7 is the standard working curve figure of paraxylene.
Fig. 8 is the standard working curve figure of meta-xylene.
Fig. 9 is the standard working curve figure of ortho-xylene.
Figure 10 is the standard working curve figure of styrene.
Figure 11 is the gas chromatogram of plant effluent pond waste gas.
Figure 12 is the gas chromatogram of waste gas in exhaust pipe.
Embodiment
The assay method of the present invention is described further below
1. standard sample and the preparation for treating test sample
A. standard liquid is prepared：Accurately weigh the g of hexamethylene 0.9984, the g of benzene 0.0724, the g of toluene 0.0876, butyl ester 0.2176
G, the g of ethylbenzene 0.1040, the g of paraxylene 0.1066, the g of meta-xylene 0.1032, the g of ortho-xylene 0.1118, styrene
0.0794 g, is placed in 100 mL volumetric flasks, dilutes constant volume with hplc grade methanol, is used as hybrid standard working solution mother liquor.It is female
Liquid continues dilution by hplc grade methanol solution and is configured to 1 ~ 6 grade of standard working solution, by standard liquid micro-samplings at different levels
Device respectively takes 10 μ L into 20 mL headspace samplings bottles, and the volatile organic matter concentration in final ml headspace bottle will be standard working solution
Concentration, the final gas concentration of titers at different levels is shown in Table 1 in ml headspace bottle.
The standard liquid gas concentration of the volatile organic matter of table 1
B) exhaust gas sampling to be measured：a）One 20 mL headspace samplings bottle is directly placed or is suspended in cotton thread in exhaust gas atmosphere flat
Weigh after 1 h, be rapidly added 10 μ L methanol, ml headspace bottle is sealed at once to be measured；b）When taking malleation waste gas in pipeline, ml headspace bottle is put
In 20 L or so hermetic bag and empty the air in bag, hermetic bag be placed at pipeline opening or pipeline shunt mouthful,
Enter hermetic bag using the waste gas in malleation pipeline, circulation is replaced rapid with hand that hermetic bag is close after the gas in 3 hermetic bags
Envelope, allows ml headspace bottle after 30 min are balanced, to be rapidly added 10 μ L methanol in hermetic bag, ml headspace bottle is sealed at once to be measured.
2. instrument and condition
A, head space condition are：80 DEG C of Sample equilibration temperature；95 DEG C of sample amounts circumstance temperature degree；105 DEG C of sample transfer line temperature；Sample
The min of equilibration time 10.；The psi of sample bottle moulding pressure 15；The psi of nebulizer gas pressure 30；The min of pressing time 0.20；During inflation
Between 0.20 min；The min of sample loop equilibration time 0.05；The min of sample injection time 1.
B, GC conditions are：Chromatographic column is DB-WAX（30m×0.32mm×0.25μm）；160 DEG C of injector temperature；
Carrier gas is high-purity N2（Purity >=99.999%）；The mL/min of flow velocity 3.0；Split ratio 2: 1；Heating schedule：40 DEG C of guarantors of initial temperature
Hold 2 min, then 70 DEG C risen to 10 DEG C/min speed, 70 DEG C retain 6 min after rise to 180 DEG C with 20 DEG C/min speed,
Keep 1 min；
3. the detection of volatile organic content in plant gas
The measure of standard working solution and the drafting of standard curve：With nitrogen as carrier gas, by the top containing volatile organic matter
Empty composition is blown into the chromatogram of isolated volatile organic matter standard working solution in gas chromatograph, as shown in Figure 1, will
The peak area arrived（X）With corresponding standard working solution concentration（Y）Mapping, draws out standard curve, and it is bent to calculate the standard that obtains
The regression equation and coefficient correlation of line, regression equation and coefficient correlation are shown in Table 2；
The measure of volatile organic content in testing sample：With nitrogen as carrier gas, by the head space containing volatile organic matter
Composition is blown into gas chromatograph with carrier gas and separated, and obtains treating the chromatogram of volatile organic matter in test sample, by every kind of volatility
The peak area of organic matter is substituted into the regression equation of its correspondence standard curve, obtains the content of volatile organic matter in waste gas.
Least concentration standard working solution is taken, 7 parallel tests calculate standard deviation, and 3 times of standard deviations are qualitative detection
Limit, 10 times of standard deviations are quantitative test limit, are specifically shown in Table 2.
The standard working curve and coefficient correlation of the volatile organic matter of table 2
4.
5. precision
Using one of them, concentration in six 10 μ L is pipetted with microsyringe respectively（4 grades）Standard working solution to six
In 20 clean mL headspace samplings bottles, seal after ml headspace bottle, be measured, the precision measured is shown in Table 3 immediately.
Testing result and precision that 3 parallel determination of table is 6 times
Note：Testing result unit is mg/m3, and RSD represents relative standard deviation（Precision）.
Same sample repeatedly determines the RSD of testing result it can be seen from the result that table 3 is counted<2%, illustrate present invention survey
Determine the reproducible of method.
It is organic to volatility in the plant gas of specific diverse location using the above-mentioned assay method further illustrated below
Thing content is measured.
Embodiment 1
In the assay method of the present embodiment：It is suspended in the exhaust gas atmosphere of plant effluent pond and is balanced after 1 h with cotton thread, is rapidly added 10
μ L methanol, seals ml headspace bottle at once, is 80 DEG C to the head space equilibrium temperature of sample and standard specimen, 10 min, and measure the results are shown in Table 4
It is shown.
The testing result of volatile organic content in the plant effluent pond waste gas of table 4
| Volatile organic matter | Testing result（mg/m3） |
| Hexamethylene | 196570 |
| Benzene | N.D. |
| Toluene | 24810 |
| Ethylbenzene | 13990 |
| Paraxylene | 19720 |
| Meta-xylene | 50820 |
| Ortho-xylene | 22086 |
| Styrene | 550 |
Note：N.D. target compound is represented not detect
Embodiment 2
In the assay method of the present embodiment：Ml headspace bottle is placed in a 20L or so hermetic bag and the air in bag is emptied, will
Hermetic bag is placed in pipeline opening or pipeline shunt mouthful place, enters hermetic bag using the waste gas in malleation pipeline, and circulation replacement 3 times is close
Hermetic bag is sealed with hand rapidly after gas in envelope, allows ml headspace bottle after 30 min are balanced, to be rapidly added 10 in hermetic bag
μ L methanol, seals ml headspace bottle at once.To the head space equilibrium temperature of sample and standard specimen it is 80 DEG C, 10 min, measure the results are shown in Table 5
It is shown.
The testing result of waste gas volatile organic content in the exhaust pipe of table 5
It the foregoing is only presently preferred embodiments of the present invention, it is impossible to be considered as the practical range for limiting the present invention.Fan Yiben
Equivalent change that patent application scope is made all should be belonged to still within protection scope of the present invention with improving etc..
Claims (5)
1. a kind of method for determining volatile organic content in industrial waste gas, it is characterised in that：Utilize Static Headspace-gas phase color
Spectrometry directly determines volatile organic content in industrial waste gas.
2. a kind of method for determining volatile organic content in industrial waste gas according to claim 1, it is characterised in that
Comprise the following steps：
1）The preparation of volatile organic matter mixed standard solution：The accurate pure material for weighing 9 kinds of chromatographically pure volatile organic matters, first
A high concentration mixed standard solution is made into Chromatographic Pure Methanol as deposit mother liquor；Again with methanol dilutes step by step to be configured to one and is
The mixed standard solution of row various concentrations gradient；
2）The detection of volatile organic matter mixed standard solution and the drafting of standard curve：The accurate removing step 1 of difference）Obtain
A series of mixed standard solutions are respectively put into head-space sampler and detected into the headspace sampling bottle for the number of finishing；With each
The chromatographic peak area X for planting organic matter is the standard gas concentration Y (mg/m in abscissa, its corresponding ml headspace bottle3) painted for ordinate
The standard curve of every kind of volatile organic matter is made, the regression equation for obtaining each standard curve is calculated；
3）Waste gas sample is sampled and handled：In the sampling of waste gas monitoring point, the host solvents of the volume as standard sample are rapidly added,
The testing sample bottle of acquisition is sealed rapidly to be measured,
4）The measure of volatile organic content in waste gas sample：By step 3）In testing sample bottle be put into head-space sampler
Carry out headspace sampling after head space balance and carry out separation and quantitative detection,
The chromatographic peak area of obtained various volatile organic matters is substituted into step 2 respectively）In in corresponding regression equation, you can
Obtain the content of various volatile organic matters in waste gas.
3. the method according to claim 2 for determining volatile organic content in industrial waste gas, it is characterised in that：Step
2）Described in ml headspace bottle in the final standard gas concentration of volatile organic matter, the concentration of various volatile organic matters for 5 ~
5000 mg/m3；
Step 2) described in headspace sampling condition be：80 DEG C of Sample equilibration temperature；95 DEG C of sample amounts circumstance temperature degree；Sample transfer
105 DEG C of line temperature；The min of Sample equilibration time 10；The psi of sample bottle moulding pressure 15；The psi of nebulizer gas pressure 30；Pressing time
0.20 min；The min of inflationtime 0.20；The min of sample loop equilibration time 0.05；The min of sample injection time 1.
4. the method for volatile organic content in industrial waste gas according to claim 2, it is characterised in that：Step 2）In
Addition mixed standard solution volume be 10 μ L.
5. the method for volatile organic content in industrial waste gas according to claim 2, it is characterised in that：Step 2）In
GC conditions are：Chromatographic column is DB-WAX（30m×0.32mm×0.25μm）；160 DEG C of injector temperature；Carrier gas is high-purity
N2（Purity >=99.999%）；The mL/min of flow velocity 3.0；Split ratio 2: 1；Heating schedule：40 DEG C of 2 min of holding of initial temperature, then
180 DEG C are risen to 20 DEG C/min speed after rising to 70 DEG C, 70 DEG C of 6 min of reservation with 10 DEG C/min speed, 1 min is kept.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108181417A (en) * | 2017-12-15 | 2018-06-19 | 舟山出入境检验检疫局综合技术服务中心 | A kind of method of dimethylbenzene in HS-GC-MS/MS detections marine product |
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| CN108181417A (en) * | 2017-12-15 | 2018-06-19 | 舟山出入境检验检疫局综合技术服务中心 | A kind of method of dimethylbenzene in HS-GC-MS/MS detections marine product |
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