CN104931612A - Method for measuring ethyl alcohol and ethylene glycol in air and exhaust gas - Google Patents
Method for measuring ethyl alcohol and ethylene glycol in air and exhaust gas Download PDFInfo
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- CN104931612A CN104931612A CN201510297404.6A CN201510297404A CN104931612A CN 104931612 A CN104931612 A CN 104931612A CN 201510297404 A CN201510297404 A CN 201510297404A CN 104931612 A CN104931612 A CN 104931612A
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Abstract
The invention relates to a method for measuring ethyl alcohol and ethylene glycol in air and exhaust gas. The method includes the following steps: (1) sample collection: sampling by using a U-shaped porous glass plate absorption tube filled with secondary ultrapure water at a certain flow rate for a certain time; (2) drawing of a standard curve: compounding a certain amount of ethyl alcohol and ethylene glycol into a certain concentration gradient by using the secondary ultrapure water, continuously measuring for three times and drawing the standard curve of chromatogram peak area to target compound; (3) sample analysis: under certain analysis conditions, filtering the samples collected and then placing in an autosampler for analysis, detecting through capillary-column chromatography separation and a fid-flame detector, and determining the final result. The method provided by the invention adopts the ultrapure water to collect ethyl alcohol and ethylene glycol in the air and exhaust gas, and a gas chromatographic method is used for direct injection analysis; the method is fast, environment-friendly, easy to operate, and high in selectivity.
Description
Technical field
The present invention relates to a kind of method measuring ethanol and ethylene glycol in air and waste gas, belong to the technical field of purification of air.
Background technology
Ethanol and ethylene glycol are all water white liquid, and normal temperature and pressure is all volatile.Both important industrial chemicals, although belong to hypotoxicity, because its vapour density is comparatively large, diffusion length is wide, and accumulative harm is large.At present, the ethylene glycol method measured in air and waste gas has Desorption Gas Chromatography Method, but uses a large amount of organic solvent carbon disulphide in the method extraction process, causes certain injury to experimenter; And the ethanol in air and waste gas is so far without clear and definite assay method, the just assay method of methyl alcohol in reference air and waste gas, result is unsatisfactory.Therefore, the present invention is proposed.
Summary of the invention
For the above-mentioned technical matters of prior art, the object of this invention is to provide a kind of method measuring ethanol and ethylene glycol in air and waste gas, because ethanol and ethylene glycol mix with arbitrary proportion with water, and dissolution velocity is fast, present invention employs the ethanol in ultrapure water absorption collection air and waste gas and ethylene glycol, vapor-phase chromatography direct injection analysis, the method fast, be easy to operation, selectivity is strong.
For achieving the above object, the present invention is achieved by the following technical solutions:
Measure a method for ethanol and ethylene glycol in air and waste gas, comprise the following steps:
(1) collection of sample: the U-shaped fritted glass disk bubbler of secondary ultrapure water will be housed, with certain flow, sampling certain hour;
(2) drafting of typical curve: a certain amount of ethanol and ethylene glycol secondary ultrapure water are mixed with certain concentration gradient, METHOD FOR CONTINUOUS DETERMINATION several times, with chromatogram peak area to target compound drawing standard curve; The typical curve equation of described ethanol is y=741.57x+1917.66, and the typical curve equation of described ethylene glycol is y=495.57x-11708.03, and described x is sample concentration, and y is the corresponding peak area of chromatogram;
(3) sample analysis: under certain analysis condition, puts into automatic sampler analysis by the sample of collection, detects finally determine analysis result through capillary chromatographic column separation and hydrogen flame detecting device.
Described step (2), if the secondary ultrapure water of middle absorption tube has volatilization, supplements certain value after sampling.
When in described step (2), ambient temperature is more than 25 DEG C, absorption tube is immersed in ice-water bath and samples, to keep higher absorption efficiency.
Beneficial effect of the present invention is as follows:
The present invention measures the method for ethanol and ethylene glycol in air and waste gas, after adopting the sampling of secondary ultrapure water, filter direct injected, under condition after optimization, be separated through capillary chromatographic column, hydrogen flame detecting device detects (FID), the method fast, be easy to operation, the interference of other alcohols is little, selectivity is good, effectively prevent the pollution of organic solvent in extraction process, alcohol compound sample in air and waste gas can be met completely, especially the detection of ethanol and ethylene glycol.
Accompanying drawing explanation
Fig. 1 is the canonical plotting of ethanol;
Fig. 2 is the canonical plotting of ethylene glycol;
Fig. 3 is the sample chromatogram figure of ethanol and ethylene glycol.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
One, the key instrument in the present embodiment and reagent
Gas chromatograph: model 2014C, Japanese Shimadzu Corporation, is with 150 automatic samplers.
Chromatographic column: model: DB-INNOWAX (30m × 0.53mm × 0.25 μm, the chromatographic column of specialty water inlet), Agilent company.
Ethanol chromatographically pure reagent, ethylene glycol chromatographically pure reagent: be all purchased from Aladdin Reagent Company.
Experimental water is the secondary ultrapure water of preparation, detects without test substance through chromatogram.
Sampling thief: model: ZC-Q, Zhejiang Province Hengda Instruments Co., Ltd.
Sampling pipe: model: U-shaped fritted glass disk bubbler, is purchased from Zhejiang Province Hengda Instruments Co., Ltd.
Two, the analysis condition in the present embodiment
1, temperature conditions:
2, other conditions:
Sample size: 1 μ L; Split ratio: 10:1; Flow velocity: 3.00mL/min; Air and waste gas flow: 400mL/min; Hydrogen flowing quantity: 40mL/min.
Three, the present embodiment measures the method for ethanol and ethylene glycol in air and waste gas, comprises the following steps:
(1) collection of sample
By being equipped with the U-shaped fritted glass disk bubbler of 5.0mL bis-ultrapure waters, with the flow of 0.5L/min, sampling 1h, if the ultrapure water of absorption tube has volatilization, should supplement value 5.0mL after sampling.During it heat, absorption tube should be immersed in ice-water bath and sample, to keep higher absorption efficiency.
(2) drafting of typical curve
A certain amount of ethanol and ethylene glycol pure water are mixed with a series of concentration gradient, depict typical curve and see Fig. 1 and Fig. 2.
Fig. 1 and Fig. 2 is respectively the typical curve of ethanol and ethylene glycol, and its concentration and area see the following form 1:
The concentration of table 1 ethanol and ethylene glycol and peak area figure
Aiutage waste gas METHOD FOR CONTINUOUS DETERMINATION 6 times in the present embodiment, the results are shown in following table 3:
Table 3 typical curve equation and sample determination result
(3) sample analysis
Condition according to the above analysis, first use organic membrane filtration sample solution of 0.45 μm, then respectively standard solution and sample solution are analyzed, each concentration replication 3 times, with peak area to ethanol and ethylene glycol drawing standard curve, coefficient R >0.9990, if the concentration of ethanol and ethylene glycol exceedes measurement range in sample, measure after available ultrapure water dilution, during calculating, be multiplied by extension rate.
With operating conditions working sample and the placebo solution of bioassay standard series, spectrogram the results are shown in Figure 3, and after the sample peak area of mensuration is deducted the peak area of blank, calculated the concentration of trying to achieve ethanol and ethylene glycol by typical curve, computation process is:
By formula (1), sampling volume is converted into standard sample volume:
In formula:
V
nd-standard sample volume, L;
V-sampling volume, L;
tthe temperature of-sampled point, DEG C;
pthe atmospheric pressure of-sampled point, kPa;
The concentration of ethanol in air and waste gas and waste gas and ethylene glycol is calculated by formula (2):
The mass concentration of target compound in ρ-air, mg/m
3;
ρ
1the mass concentration of target compound in the-sample that calculated by calibration curve, μ g/mL;
ρ
0the mass concentration of target compound in the-contrast blank sample that calculated by calibration curve, μ g/mL;
The volume of V-sample, mL;
V
nd-standard sample volume, L.
The present invention measures the method for ethanol and ethylene glycol in air and waste gas, after adopting the sampling of secondary ultrapure water, direct injected, be separated through capillary chromatographic column, hydrogen flame detecting device detects (FID), the method fast, be easy to operation, the interference of other alcohols is little, selectivity is good, can meet alcohol compound sample in air and waste gas completely, especially the detection of ethanol and ethylene glycol.
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (3)
1. measure a method for ethanol and ethylene glycol in air and waste gas, it is characterized in that comprising the following steps:
(1) collection of sample: the U-shaped fritted glass disk bubbler of secondary ultrapure water will be housed, with certain flow, sampling certain hour;
(2) drafting of typical curve: a certain amount of ethanol and ethylene glycol secondary ultrapure water are mixed with certain concentration gradient, METHOD FOR CONTINUOUS DETERMINATION several times, with chromatogram peak area to target compound drawing standard curve; The typical curve equation of described ethanol is y=741.57x+1917.66, and the typical curve equation of described ethylene glycol is y=495.57x-11708.03, and described x is sample concentration;
(3) sample analysis: under certain analysis condition, puts into automatic sampler analysis by the sample of collection, detects finally determine analysis result through capillary chromatographic column separation and hydrogen flame detecting device.
2. measure the method for ethanol and ethylene glycol in air and waste gas as claimed in claim 1, it is characterized in that: described step (2), if the secondary ultrapure water of middle absorption tube has volatilization, supplements certain value after sampling.
3. measure the method for ethanol and ethylene glycol in air and waste gas as claimed in claim 1, it is characterized in that: when ambient temperature is more than 25 DEG C in described step (2), absorption tube is immersed in ice-water bath and samples, to keep higher absorption efficiency.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510297404.6A CN104931612A (en) | 2015-06-02 | 2015-06-02 | Method for measuring ethyl alcohol and ethylene glycol in air and exhaust gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510297404.6A CN104931612A (en) | 2015-06-02 | 2015-06-02 | Method for measuring ethyl alcohol and ethylene glycol in air and exhaust gas |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105300972A (en) * | 2015-10-10 | 2016-02-03 | 煤炭科学技术研究院有限公司 | Determination method of glycol content in phenol and oil-containing complicated system |
| CN113484425A (en) * | 2021-04-21 | 2021-10-08 | 江苏泰斯特专业检测有限公司 | Method for measuring ethanol in air |
| CN114371235A (en) * | 2021-12-30 | 2022-04-19 | 河北华清旭隆智能设备有限公司 | Method for detecting ethylene glycol in solid waste |
| CN115452959A (en) * | 2021-06-08 | 2022-12-09 | 无锡中证检测技术(集团)有限公司 | Ethanol detection device for industrial waste gas and use method |
-
2015
- 2015-06-02 CN CN201510297404.6A patent/CN104931612A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105300972A (en) * | 2015-10-10 | 2016-02-03 | 煤炭科学技术研究院有限公司 | Determination method of glycol content in phenol and oil-containing complicated system |
| CN113484425A (en) * | 2021-04-21 | 2021-10-08 | 江苏泰斯特专业检测有限公司 | Method for measuring ethanol in air |
| CN115452959A (en) * | 2021-06-08 | 2022-12-09 | 无锡中证检测技术(集团)有限公司 | Ethanol detection device for industrial waste gas and use method |
| CN114371235A (en) * | 2021-12-30 | 2022-04-19 | 河北华清旭隆智能设备有限公司 | Method for detecting ethylene glycol in solid waste |
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Application publication date: 20150923 |