Determination of Volatile Halogenated Hydrocarbons in Wastewater by Single-Drop Microextraction Coupled to Capillary Gas Chromatography

2013 ◽  
Vol 295-298 ◽  
pp. 487-491
Author(s):  
Jian Qi Sun

Single-drop microextraction (SDME) coupled to capillary gas chromatography (GC) was established for the determination of seven volatile halogenated hydrocarbons in wastewater, including chloroform (CF), carbon tetrachloride (CT), trichloroethylene (TCE), bromodichloromethane (BDCM), perchlorethylene (PCE), dibromochloromethane (DBCM) and bromoform (BF). The SDME parameters such as extractants, extracting time,stirring rate and immerging depth of needle point were studyed and optimized. The abovementioned halogenated hydrocarbons were quantified by external standardization method using GC coupled with a flame ionization detector (FID). The linear regression calibration curves, detection limits (S/N=3) and the linear ranges of the method for determining each halogenated hydrocarbons were determined, respectively. The concentrations of componds abovementioned in a real wastewater sample, the average of the recoveries obtained in the spiked wastewater samples and the corresponding relative standard deviations were determined, respectively. The results showed the proposed method several attributes, friendly enviroment, economic and highly efficient pretreatment, less time, simplicity, sensitivity, accuracy and wide linear range and so on.

2013 ◽  
Vol 295-298 ◽  
pp. 483-486 ◽  
Author(s):  
Jian Qi Sun

Single-drop microextraction (SDME) coupled to capillary gas chromatography (GC) was established for the determination of four phthalate esters in wastewater, including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-octyl phthalate (DnOP) and butyl benzyl phthalate (BBP). The SDME parameters such as extractants, extracting time,stirring rate and immerging depth of needle point were studyed and optimized. The abovementioned phthalate esters were quantified by external standardization method using GC coupled with a flame ionization detector (FID). The linear regression calibration curves, detection limits (S/N=3) and the linear ranges of the method for determining each phthalate were determined, respectively. The concentrations of components abovementioned in a real wastewater sample, the average of the recoveries obtained in the spiked wastewater samples and the corresponding relative standard deviations were determined, respectively. The results showed the proposed method several attributes, friendly enviroment, economic and highly efficient pretreatment, less time, simplicity, sensitivity, accuracy and wide linear range and so on.


2013 ◽  
Vol 838-841 ◽  
pp. 2566-2569
Author(s):  
Jian Qi Sun ◽  
Bo Qiao ◽  
Jun Dai

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of chlorobenzenes (m-dichlorobenzene (m-DCB),p-dichlorobenzene (p-DCB),o-dichlorobenzene (o-DCB) and 1,2,4-trichlorobenzene (1,2,4-TCB)) in wastewater. For this purpose, single-drop microextraction (SDME) was applied as a sample preparation technique. The SDME parameters such as types of extractants, volume of the microdroplet size, extraction time, stir rate and immersion depth of needle point were studyed and optimized. The method was linear in the ranges from 4.0×10-3to 40.0 μg·mL-1form-DCB,p-DCB ando-DCB, and 4.0×10-3to 30.0 μg·mL-1for 1,2,4-TCB withR2≥0.9955. The SDME procedure allowed efficient recovery of the investigated chlorobenzenes ranging between 80 % and 105 % with a relative standard deviation (RSD) ≤6.5 for actual wastewater sampes spiked with 2, 5 and 10 μg·mL-1of chlorobenzes, respectively. These results showed the potential of this technique for chlorobenzenes monitoring in wastewater samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.


2013 ◽  
Vol 838-841 ◽  
pp. 2582-2585 ◽  
Author(s):  
Jian Qi Sun ◽  
Bo Qiao ◽  
De Si Sun

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of polycyclic aromatic hydrocarbons (PAHs) in wastewater, including naphthalene, 1-naphthol, 2-naphthol and anthracene. For this purpose, single-drop microextraction (SDME) was applied as a sample preparation technique. The SDME parameters such as types of extractants, volume of the microdroplet size, extraction time, stir rate and immersion depth of needle point were investigated and optimized. The method was linear in the ranges from 2.3 ×10-3to 70.0 μg·mL-1for naphthalene, 1-naphthol and anthracene, and 2.2 ×10-3to 50.0 μg·mL-1for 2-naphthol withR2≥ 0.9990. The SDME procedure allowed efficient recovery of the investigated PAHs ranging between 94 % and 104 % with a relative standard deviation (RSD) ≤4.2 for actual wastewater sampes spiked with 5, 10 and 20 μg·mL-1of PAHs, respectively. These results showed the potential of this technique for PAHs monitoring in wastewater samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.


2014 ◽  
Vol 881-883 ◽  
pp. 627-630 ◽  
Author(s):  
Jian Qi Sun ◽  
Fang Zeng ◽  
Xiao Feng Liu

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of acrylates (methyl acrylate (MA), methyl methacrylate (MMA), butyl acrylate (BA)) in wastewater. For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were studied and optimized. The method was linear in the ranges from 4.3×10-4 to 200.0 μg·mL-1 for abovementioned acrylates with R2≥ 0.9992. The DLLME procedure allowed efficient recovery of the investigated acrylates ranging between 81 % and 109 % with a relative standard deviation (RSD) ≤ 9.1 for the blank samples spiked with 10, 50 and 100 μg·mL-1 of acrylates, respectively. These results showed the potential of this technique for acrylates monitoring in wastewater samples. Furthermore, the investigated methods are simple, reproducible, and inexpensive.


1986 ◽  
Vol 69 (6) ◽  
pp. 976-980
Author(s):  
Richard A Niemann

Abstract Surrogate spiking the sample with 1000 parts per trillion (pptr) 1,3,7,8-tetrachlorodibenzo-p-dioxin (1378-TCDD) has doubled analytical throughput in determining toxic 2378-TCDD (analyte) at the low partper- trillion level in fish, using multicolumn high resolution liquid chromatographic cleanup before quantitation by capillary gas chromatography with electron capture detection. The 1378- and 2378-TCDD were recovered equally and were well separated by the capillary column so that the earlier-eluting surrogate did not interfere with the quantitation of levels of analyte many-fold lower. Matrix interference contributed <1 % bias in surrogate quantitation. Using surrogate recovery to correct for analyte losses during analysis, accuracy averaged (n = 7) 105% in determining 18 or 45 pptr 2378-TCDD added to fish without detectable bioincurred analyte. Analyses of selected fish with bioincurred 2378-TCDD gave results comparable to earlier work where recovery correction required a second analysis of sample fortified with analyte. With surrogate fortification, repeatability of determination (n = 3 or 4) improved markedly to <5% relative standard deviation at 37-46 pptr.


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