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Determinartionof Nine Acetate Compounds In Air By Solid Adsorption-Solvecnt Desorption Gas Chromatograph

Posted on:2020-05-02Degree:MasterType:Thesis
Country:ChinaCandidate:H PengFull Text:PDF
GTID:2381330572487557Subject:Agricultural resource utilization
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In this paper,the gas chromatographic conditions for the collection of 9 kinds of acetate compounds and the sample pretreatment method were studied.The activated carbon tube was used to enrich the acetate compound,the carbon disulfide was used for analysis,the capillary column was separated,and the hydrogen flame ionization detector was used to detecting quantitatively.Nine kinds of substances such as methyl acetate,vinyl acetate,ethyl acetate,propyl acetate,isopropyl acetate,butyl acetate,isobutyl acetate,amyl acetate and isoamyl acetate are all acetate compounds.Color transparent liquid,slightly soluble in water;it is widely used not only in solvents,plasticizers,surfactants and polymer monomers,but also in organic chemical synthesis processes,mainly as inks,adhesives,coatings?paints and Enamel?plays an important role in the active solvents and pharmaceuticals in the formulation.The dangerous characteristic of acetate compounds is flammable.The mixture of air and its vapor is flammable and explosive.It can cause burning or explosion when exposed to strong oxidants and open flames.In addition,its vapor will be low at low concentrations.The upper respiratory tract is irritating.At higher concentrations,it can cause anesthesia to the nerves when inhaled.In severe cases,it can cause headache,dizziness,vomiting and other symptoms.If it is exposed for a long time,it will cause lung and respiratory diseases.Therefore,the detection of acetate compounds is of great significance.?1?Optimization of chromatographic conditions.By optimizing the chromatographic conditions,the final determination of the DB-624?60 m×0.25 mm×1.4?m?column,hydrogen flame ionization detector,heating program:initial temperature second temperature program:initial temperature is 40??retained 3 min?,the temperature was raised to 70? at 15?·min-1?retained for 1 min?,and the temperature was raised to 100??retained for 8 min?at 4?·min-1?31min total?;split ratio:25:1;injection volume:1?L.The nine acetate compounds showed good linearity in the range of 110 mg·L-1,and the correlation coefficients were all greater than0.9990.?2?Optimization of sample collection conditions and sample pretreatment conditions.It mainly optimizes the sampling flow,sampling time,adsorbent type,desorbent type and desorption time.Finally,the activated carbon sampling tube was determined as the best adsorbent.The sampling flow of the atmospheric sampler was set to 0.6 L·min-1,and the sampling time was 30 min.After sampling,the carbon dioxide was desorbed,and the desorption time was 30 min.After the desorption was completed,the desorption was performed.Sample analysis.?3?Method recovery and precision test.The spiked recovery test was carried out at the levels of 1 mg·L-1,5 mg·L-1,and 10 mg·L-1 by the above method,and each level was repeated5 times.The results showed that the average spiked recovery was performed.The rate was82.65%99.97%,the relative standard deviation was 1.81%6.14%,the detection limits of methyl acetate,vinyl acetate,ethyl acetate,propyl acetate,isopropyl acetate,butyl acetate,isobutyl acetate,amyl acetate and isoamyl acetate were 0.5 mg·L-1,0.3 mg·L-1,0.1 mg·L-1,0.2mg·L-1,0.05 mg·L-1,0.3 mg·L-1,0.5 mg·L-1,0.2 mg·L-1,0.5 mg·L-1 and the detection limits were0.0024 mg·m-3?0.0049 mg·m-3?0.0065 mg·m-3?0.0043 mg·m-3?0.0087 mg·m-3?0.0063mg·m-3?0.0058 mg·m-3?0.0073 mg·m-3?0.0087mg·m-3,which meets the testing requirements.The method has high sensitivity and good accuracy,and meets the technical requirements for the detection of acetate compounds,and provides technical support for the detection of acetate compounds in ambient air or workplace air.
Keywords/Search Tags:Gas chromatography, Methyl acetate, Adsorption, Desorption
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