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Objective: To establish a solvent desorption-gas chromatography method for determination of dimethyl carbonate (DMC) in workplace air. Methods: The air samples were collected using activated carbon tubes, desorbed by carbon disulfide, separated by dimethylpolysiloxane capillary columns, and detected by a flame ionization detector. Results: The linear range of DMC was 2.14 to 1.07×104 mg/L, and the correlation coefficient was greater than 0.999. The detection limit was 0.14 mg/L, the lower limit of quantification was 0.47 mg/L, the minimum detection concentration was 0.10 mg/m3, and the minimum quantification concentration was 0.32 mg/m3 (based on 1.5 L workplace air). The average desorption efficiency of the method was 96.2% to 102.0%. Both the within-run and between-run relative standard deviations were 0.9% to 2.3%. The samples could be stored for at least seven days at four celsius degree. Conclusion: This method shows high desorption efficiency, high sensitivity, good precision and is simple in using. It can be used for the determination of DMC in workplace air.
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Objective: To establish a solvent desorption-gas chromatography method for the determination of 1,1,2,2-tetrachloroethane and 1,1,1,2-tetrachloroethane in workplace air. Methods: The 1,1,2,2-tetrachloroethane and 1,1,1,2-tetrachloroethane in workplace air were collected using activated carbon tubes, desorbed with carbon disulfide, and separated and detected by gas chromatography. The quantifications were based on standard curves. Results: The linear ranges of 1,1,2,2-tetrachloroethane and 1,1,1,2-tetrachloroethane were 0.98-395.50 and 0.87-395.50 mg/L, respectively, with the correlation coefficient of 0.999 95. The detection limits were 0.29 and 0.26 mg/L, respectively. The average of desorption efficiency was 92.04%-104.67%. The within- and between-run relative standard deviations were 1.42%-2.09% and 1.63%-6.09%, respectively. The sampling efficiency was more than 98.00%. The samples could be stored at room temperature for at least 14 days. Conclusion: This method can be used in detection of 1,1,2,2-tetrachloroethane and 1,1,1,2-tetrachloroethane in workplace air.
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Objective To establish a solvent desorption inductively coupled plasma-mass spectrometry (ICP-MS) method for determination of iodine in workplace air. Methods Iodine in workplace air was collected with alkaline activated carbon tube and desorbed with 10.0 mL pure water or 20 mmol/L sodium bicarbonate solution. Rhenium-185 was used as an internal standard for quantification. The sample was determined in standard mode and kinetic energy discrimination collision (KED) mode by ICP-MS. Results In standard mode, iodine showed a good linear range in the concentration of 9.0 to 1 100.0 μg/L, with a correlation coefficient of 0.999 3 and a detection limit of 2.7 μg/L. In KED mode, iodine showed a good linear range in the concentration of 24.3 to 800.0 μg/L, with a correlation coefficient of 0.999 1 and a detection limit of 7.3 μg/L. The average desorption efficiency using pure water ranged from 99.1% to 106.7%, with within-run relative standard deviation (RSD) of 3.1% to 8.0% and between-run RSD of 4.9% to 9.3%. The average desorption efficiency using sodium bicarbonate solution ranged from 96.5% to 105.3%, with within-run RSD of 4.9% to 8.6% and between-run RSD of 2.5% to 9.9%. There were no statistical significant differences in the main effects of desorption solution, ICP-MS detection mode, their interaction on average desorption efficiency and within-run RSD (all P>0.05). Samples could be stored at room temperature for at least 7 days. Conclusion This method is highly sensitive, accurate, and suitable for the determination of iodine in workplace air. The sample pretreatment is simple and rapid.
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Objective: To establish a method for the determination of butyronitrile and isobutyronitrile in the air of workplace by gas chromatography. Methods: In March 2020, butyronitrile and isobutyronitrile in the air of workplace was collected by silica gel, eluted with methanol, separated and determined by gas chromatogram with flame ionization detector, the characteristics of determination of nitrile and isobutyronitrile by gas chromatography were analyzed. Results: The limit of detection for butyronitrile and isobutyronitrile was 0.33 μg/ml. The linear range of butyronitrile determined by this method was 1.60-1600.00 μg/ml, y=2.295x-3.480, and the coefficient correlation was 0.99998, and the minimum detection concentration was 0.22 mg/m(3) (collected sample volume was 1.50 L) . The within-run precisions were 2.43%-4.12%, the between-run precisions were 1.72%-3.70%, and the desorption rates were 93.26%-98.41%. The linear range of isobutyronitrile determined by this method was 1.52-1520.00 μg/ml, y=2.208x-0.102, and the coefficient correlation was 0.99998, and the minimum detection concentration was 0.22 mg/m(3) (collected sample volume was 1.50 L) . The within-run precisions were 2.52%-3.22%, the between-run precisions were 1.20%-3.82%, and the desorption rates were 96.85%-102.50%. The sealed samples could be stored at least 10 days at room temperature without significant loss. Conclusion: The method has the advantages of good precision, high sensitivity and simple operation. It is suitable for the simultaneous determination of butyronitrile and isobutyronitrile in the air of workplace.
Subject(s)
Air Pollutants, Occupational/analysis , Chromatography, Gas/methods , Nitriles , WorkplaceABSTRACT
OBJECTIVE: To establish a method for simultaneous determination of 15 kinds of vapor state organic acids in workplace air by solvent desorption-gas chromatography.METHODS: A total 15 kinds of vapor state organic acids such as acetic acid, propanoic acid, butyric acid and pentanoic acid in the air of workplace were collected by silica gel, eluted with acetone, separated by DB-FFAP capillary chromatograph column, and detected by gas chromatography with flame ionization detection. RESULTS: There was a good linear relationship in the selected range of 15 kinds of organic acids. The coefficient correlation was 0.999 97-0.999 98. The limit of detection of this method was 0.04-0.29 mg/L, and the minimum detection concentration was 0.03-0.19 mg/m~(3 )(collected sample volume was 1.50 L). The average desorption efficiency was 92.9%-98.5%. The within-run and between-run relative standard deviation was 0.3%-1.6% and 1.5%-3.0%, respectively. The samples could be kept for at least 15 days at room temperature. CONCLUSION: The method is simple for operation, with high sensitivity, and good precision, which is suitable for simultaneous determination of 15 kinds of vapor state organic acids in the air of workplace and sites of emergency accident.
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OBJECTIVE: To establish a solvent desorption-gas chromatography method for determination of methyl pentane in workplace air. METHODS: Methyl pentane in workplace air was collected with activated carbon tube and desorbed with carbon disulfide, then separated by DB-1 capillary column, detected by flame ionization detector, and quantified by standard curve method. RESULTS: Good linearity was obtained in the range of 1.98-6 600.00 mg/L with the correlation coefficient of 0.999 9. The minimum detection limit and the minimum quantification limit were 0.06 and 0.20 mg/L, respectively. The minimum detection concentration and minimum quantification concentration was 0.04 and 0.14 mg/m~3, respectively(calculated by collecting 1.5 L of air sample). The average desorption efficiency was 97.3%-102.2%. The within-run relative standard deviation(RSD) and the between-run RSD were 0.4%-0.9% and 0.3%-3.0%, respectively. The sampling efficiency was 96.7%-100.0% and the penetration capacity was 8.68 mg. The samples can be stored at room temperature for at least 14 days. CONCLUSION: This method is suitable for methyl pentane detection in workplace air.
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OBJECTIVE: To improve the standard detection method for acetonitrile in workplace air. METHODS: Acetonitrile in the air of workplace was collected by silica gel, eluted with methanol, separated and determined by gas chromatography with flame ionization detection. RESULTS: After the improvement of the method, the linear range of acetonitrile was 1.57-1 574.00 mg/L, and the correlation coefficient was 0.999 98. The detection limit was 0.29 mg/L and the minimum detection concentration was 0.19 mg/m~(3 )(collected sample volume was 1.5 L). The average desorption efficiency was 93.1%-98.9%. The within-run and between-run precision was 2.6%-3.3% and 1.7%-3.6%, respectively. The samples could be stored at room temperature for at least 10 days. CONCLUSION: The improved method is precisied, accurate and simple to operate, which is suitable for determination of acetonitrile in workplace air.
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OBJECTIVE: To improve the standard detection method for acetaldehyde, butyraldehyde and isobutyraldehyde in the air of workplace. METHODS: Acetaldehyde, butyraldehyde and isobutyraldehyde in the air of workplace were collected using silica gel tube, desorbed with 45.0% ethanol, separated by a capillary column and detected by a flame ionization detector. RESULTS: The linear range of this method for detecting acetaldehyde, butyraldehyde and isobutyraldehyde were 1.57-1 568.00, 1.60-1 600.00 and 1.59-1 588.00 mg/L, respectively. All the correlation coefficients were greater than 0.999. The detection limits were 0.52, 0.46 and 0.54 mg/L, respectively. The desorption efficiency was 91.0%-103.0%. The within-run relative standard deviation(RSD) was 0.7%-1.7%.The between-run RSD was 2.0%-3.7%. The samples could be stored for at least 10 days at room temperature. CONCLUSION: This method can be used for simultaneous detection of acetaldehyde, butyraldehyde and isobutyraldehyde in the air of workplace.
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Objective@#To develop a solvent desorption-gas chromatography method for simultaneous determination of methyl methacrylate (MMA) , ethyl methacrylate (EMA) , n-propyl methacrylate (PMA) and butyl methacrylate (BMA) in workplace air.@*Methods@#MMA, EMA, PMA and BMA in workplace air were captured by charcoal tubes and desorbed with carbon disulfide, separated through capillary chromatographic column, and then analyzed by gas chromatography-flame ionization detector.@*Results@#The linear ranges of MMA, EMA, PMA and BMA were 0-8 305.00 mg/L, 0-9 080.50 mg/L, 0-8 899.00 mg/L and 0-8 371.00 mg/L respectively, and the related coefficients were between 0.999 96-0.999 98. The relative standard deviations (RSD) within the group were 0.56%-1.71%, 0.45%-1.65%, 0.51%-1.49% and 0.45%-1.50% respectively, and the RSD between the group were 1.14%-2.79%, 0.79%-2.13%, 0.93%-2.30% and 1.09%-2.84% respectively. The average desorption efficiencies were 95.76%-99.58%, 97.82%-102.28%, 98.55%-102.28%and 98.70%-102.40% respectively. The minimum quantification concentrations were 0.12 mg/m3, 0.10 mg/m3, 0.07 mg/m3 and 0.07 mg/m3 respectively (3.00 L sample) . The samples could be stored at room temperature for at least 7 days.@*Conclusion@#This method could be used for monitoring of MMA, EMA, PMA and BMA in workplace air.
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Objective@#To develop a solvent desorption-gas chromatography method for determination of ethyl methacrylate(EMA) in workplace air.@*Methods@#EMA in workplace air was captured by charcoal tubes and desorbed with carbon disulfide, separated through capillary chromatographic column, and then analyzed by gas chromatography-flame ionization detector.@*Results@#The linear ranges of EMA were 0.00-9108.00 mg/L, and the related coefficients were 0.999 96. The relative standard deviations(RSD) within the group were 0.55%-1.84%, and the RSD between the group were1.26%-3.30%. The average desorption efficiencies were 98.26%-100.58%. The average samplingefficiencies were 99.98%-100.00%. and the minimum detectable concentration and the minimum quantification concentration were respectively 0.03 mg/m3 and 0.10 mg/m3 per 3.00 L of air. The samples could be stored at room temperature for 7 days.@*Conclusion@#This method could be used formonitoring of EMA in workplace air.
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OBJECTIVE: To establish a method for simultaneous determination of 1,1,1-trichloroethane(TCA) and 1,1,2-TCA in the workplace air by solvent desorption-gas chromatography. METHODS: The 1,1,1-TCA and 1,1,2-TCA in the workplace air were collected by activated carbon tube and desorbed with carbon disulfide. They were separated with DB-1(100.0% dimethyl polysiloxane) capillary column and detected by flame ionization detector. RESULTS: The good linear ranges of 1,1,1-TCA and 1,1,2-TCA were 1.340-1.338×10~4 and 1.440-1.442×10~4 mg/L, respectively. The correlation coefficients were greater than 0.999, with the detection limits of 0.100 and 0.140 mg/L, respectively. The average desorption efficiencies of 1,1,1-TCA and 1,1,2-TCA were 98.6%-99.6% and 94.9%-96.2%. The within-run and between-run relative standard deviations were 0.4%-0.9% and 0.5%-1.1%, respectively. The samples could be stored at room temperature for at least 14 days. CONCLUSION: This method has high desorption efficiency and sensitivity, good precision and simple operation, which is suitable for simultaneous detection of 1,1,1-TCA and 1,1,2-TCA in the workplace air.
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OBJECTIVE: To establish a method for determination of N-methyl-2-pyrrolidone(NMP) in workplace air by solvent desorption-gas chromatography. METHODS: NMP in the workplace air was collected with activated carbon tube and desorbed with methanol ∶dichloromethane(5 ∶95, V/V). After desorption, it was separated by capillary column separation, and detected by flame ionization detector. RESULTS: The good linear concentration of NMP was 0.51-4 108.00 mg/L. The correlation coefficient was 0.999 9. The detection limit was 0.08 mg/L(calculated by 3 times of standard deviation). The average desorption efficiency was 101.68%-103.44%. The within-run and between-run relative standard deviations were 1.94%-3.97% and 0.97%-2.26%, respectively. The sample could be stored at room temperature for at least 14 days. CONCLUSION: The developed method is suitable for the determination of NMP in workplace air.
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Objective@#A solvent desorption-gas chromatography method for determination of ethylal in workplace air has been established.@*Methods@#Ethylal in workplace air was collected by activated carbon tube and desorbed with carbon disulfide, and the desorption solutions were analysed by capillary column GC with FID detector.@*Results@#The method presented a good linearity in the range of 0.87~34 800.00 mg/L of ethylal in the standard solution, with the correlation coefficient being r=0.999 7. The limit of detection and the limit of quantification of this method were respectively 0.20 mg/L and 0.80 mg/L, and the minimum detectable concentration and the minimum quantification concentration of this method were respectively 0.17 mg/m3 and 0.60 mg/m3 per 1.50 L of air.The within-run precision of the method was 2.93%-6.20%, and the between-run precision 3.67%-6.44%. The desorption efficiency between 94.22%-97.27%. Ethylal in activated carbon tube could be kept at least 7 days at room temperature without significant loss.@*Conclusion@#The method could be used for determination of ethylal in workplace air.
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OBJECTIVE: To develop a solvent desorption-gas chromatography method for detecting ethylene glycol monopropyl ether( EGME) in workplace air. METHODS: EGME in workplace air was captured by charcoal tubes and desorbed by methanol-methylene chloride(5∶ 95,V/V),separated by capillary chromatographic column,and detected by flame ionization detector. RESULTS: The good linear range of EGME was 1. 37-1 913. 80 mg/L,and the correlation coefficient was 0. 999 90. The detection limit was 0. 06 mg/L. The minimum detectable concentration was 0. 02 mg/m3.The average desorption efficiency was 97. 81%-104. 70%. The within-run relative standard deviation( RSD) was 1. 94%-2. 99%,and the between-run RSD was 3. 24%-4. 53%. The samples could be stored at room temperature for at least 14 days. CONCLUSION: This method could be used for detection of EGME in workplace air.
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OBJECTIVE: To establish a method for simultaneous detection of 2-methoxyethoxy ethanol( 2-MEE) and2-ethoxyethoxy ethanol( 2-ETE) in workplace air by solvent desorption-gas chromatography. METHODS: The 2-MEE and 2-ETE in workplace air were collected by activated carbon tubes and desorbed with methanol-methylene chloride( 5 ∶ 95,V/V),then separated on DB-FFAP capillary chromatographic column,and finally detected using flame ionization detector.RESULTS: The 2-MEE and 2-ETE showed a good linear range in 2. 12-8 464. 00 and 2. 11-8 428. 00 mg/L respectively and the correlation coefficients was 0. 999 8. The minimum quantification limits were 0. 16 and 0. 20 mg/m~3 respectively( 3 L air sample). The average desorption efficiencies were 99. 33%-103. 72% and 99. 61%-104. 07% respectively. The withinrun relative standard deviations( RSDs) were 3. 68%-4. 73% and 3. 47%-4. 39% respectively,and the between-run RSDs were 4. 72%-6. 99% and 4. 77%-6. 28% respectively. The samples could be stored at room temperature for at least14 days. CONCLUSION: This method is simple,sensitive,precise and suitable for simultaneous detection of 2-MEE and 2-ETE in workplace air.
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OBJECTIVE: To establish a method for simultaneous detection of five kinds of olefine chlorides in workplace air by solvent desorption-gas chromatography. METHODS: The olefine chlorides in workplace air were collected using activated charcoal tubes,desorbed by carbon disulfide,separated on a HP-INNOWAX capillary column and detected with flame ionization detector. RESULTS: The linear range of the five kinds of chlorinated olefins( vinyl chloride,allyl chloride,chloroprene,trans-1, 2-dichloroethylene, cis-1, 2-dichloroethene) was wide and the linear correlation coefficient was greater than 0. 999 8. The detection limit and the minimum detectable concentrations were 0. 30-0. 80 mg/L and 0. 05-0. 13 mg/m~3,respectively( air sample volume 6. 0 L). The recovery rate was 95. 90%-102. 67%. The within-run and betweenrun relative standard deviations were 0. 00%-3. 74% and 0. 21%-6. 12%,respectively. The samples could be preserved at room temperature for at least 14 days. CONCLUSION: This method has simple operation,good linear range,high sensitivity and good reproducibility,which is suitable for detecting 5 kinds of olefine chlorides in workplace air.
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OBJECTIVE: To explore the feasibility of simultaneous detection of 45 kinds of common organic compounds in workplace air by solvent desorption-gas chromatography method.METHODS: A total of 45 kinds of common organic compounds such as benzene,1,2-dichloroeyhane,n-hexane and trichloroethylene in workplace air were collected with activated carbon tube and desorbed with carbon disulfide,separated by capillary chromatographic column,and detected with flame ionization detector.RESULTS: There was good linear relationship in the selected range.The correlation coefficients was 0.999 92-0.999 99.The detection limit was 0.03-0.30 mg/L and the minimum detectable concentration range was 0.01-0.20 mg/m~3( sample volume was 3.00 L).The average desorption efficiencies was 75.4%-105.7%.The within-run and between-run relative standard deviations were 0.4%-6.7% and 1.8%-7.9%,respectively.The sampling efficiency was 91.9%-100.0%.CONCLUSION: The method is simple,high sensitivity and good precision,which can be used for simultaneous detection of 45 kinds of common coexisting organic compounds in workplace air.
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OBJECTIVE: To establish a method for simultaneous determination of 1,2-dichloropropane and 1,3-dichloropropane in workplace air by solvent desorption-gas chromatography.METHODS: The air samples were collected by activated carbon tube and desorbed with carbon disulfide,then separated by DB-1 capillary columns,and detected by gas chromatographic.RESULTS: The linear ranges of 1,2-dichloropropane and 1,3-dichloropropane were 1.16-17 400.00 mg/L and 1.19-17 850.00 mg/L of mass concentration,respectively.The correlation coefficient was 0.999 9,and the limit of detection was 0.07 mg/L.The average desorption efficiencies of 1,2-dichloropropane and 1,3-dichloropropane were 96.9%-98.2%and 95.8%-96.8%,respectively.The within-run relative standard deviation( RSD) was 0.4%-0.6%.The between-run RSD were 1.6%-3.2% and 1.2%-2.8% respectively.The samples could be stored at room temperature for at least 14 days.CONCLUSION: This method has high desorption efficiency and sensitivity with good precision and simple operation,which is suitable for simultaneous detection of 1,2-dichloropropane and 1,3-dichloropropane in the workplace air.
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OBJECTIVE: To establish a solvent desorption-gas chromatography method for simultaneous determination of 2-methoxyethyl acetate(2-MEA) and 2-ethoxyethyl acetate(2-EEA) in the workplace air. METHODS: 2-MEA and 2-EEA in workplace air were captured by charcoal tubes and desorbed with solution of 5. 00%(V/V) methanol-methylene chloride,separated through capillary chromatographic column,and then analyzed by gas chromatography-flameionization detector. RESULTS: The linear ranges of 2-MEA and 2-EEA were 1. 50-2 403. 84 and 1. 79-2 871. 20 mg/L,respectively.The correlation coefficient were 0. 999 8. The minimum quantification concentrations were 0. 20 and 0. 09 mg/m~3,respectively(3. 00 L sample). The average desorption efficiencies were 98. 08%-99. 67% and 94. 34%-99. 79%,respectively. The within-run relative standard deviations(RSD) were 1. 77%-3. 51% and 1. 72%-3. 01%,respectively.The between-run RSD were 2. 27%-4. 44% and 2. 31%-4. 19%,respectively. The samples could be stored at room temperature for at least 14 days. CONCLUSION: This method could be used for simultaneous sampling and quantitative detection of 2-MEA and 2-EEA in workplace air.
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OBJECTIVE: To establish a method for testing tetrahydrofuran( THF) in workplace air by solvent desorption gas chromatography. METHODS: The air samples were collected by activated carbon tube,desorbed with carbon disulfide solution,then separated by capillary column and detected by flame ionization detector. RESULTS: The linearity range of THF concentration was 1. 78-8 892. 00 mg / L,and the correlation coefficient was 0. 999 9. The minimum detection limit of THF was 0. 09 mg / m3. The minimum quantitative concentration was 0. 27 mg / m3( 3. 00 L air collection). The average desorption efficiency of THF was 94. 29%-96. 46% when placed overnight at the room temperature. The within-run and the between-run relative standard deviation were 0. 30%-0. 91% and 0. 66%-1. 23% respectively. THF sample could be stored at room temperature for at least 8 days. CONCLUSION: The method could be widely applied in sampling and detection of THF in workplace air.