scholarly journals Determination of N-Octyl Bicycloheptene Dicarboximide, Pyrethrins, and Butylcarbityl 6-Propylpiperonyl Ether in Technical Materials, Concentrates, and Finished Products by Capillary Gas Chromatography: Collaborative Study

1998 ◽  
Vol 81 (3) ◽  
pp. 503-512 ◽  
Author(s):  
Khanh T Nguyen ◽  
Richard Moorman ◽  
Virginia Kuykendall ◽  
◽  
L Bura ◽  
...  

abstract Nineteen collaborating laboratories (including the authors') analyzed 6 blind, duplicate pairs of various technical materials, pyrethrum extracts, concentrates, and finished products by split injection capillary gas chromatography (GC) with flame ionization detection. This procedure simultaneously quantitates with speed, ease, accuracy, and precision all 6 insecticidal compounds in pyrethrum: pyrethrin I, jasmolin I, cinerin I, pyrethrin II, jasmolin II, and cinerin II, as well as butylcarbityl 6-propylpiperonyl ether (BPE, the predominant compound in technical piperonyl butoxide, also commonly known as piperonyl butoxide) and both the endo and exo isomers of N-octyl bicycloheptene dicarboximide (MGK 264). Repeatability ranged from 4.28 to 7.22% for total pyrethrins, from 2.41 to 7.04% for BPE, and from 2.20 to 4.91 % for total MGK 264. Reproducibility ranged from 5.22 to 9.71 % for total pyrethrins, from 4.37 to 7.04% for BPE, and from 2.66 to 6.01 % for total MGK 264. The capillary GC method for these insecticidal compounds in technical materials, concentrates, and finished products has been adopted first action by AOAC INTERNATIONAL.

2000 ◽  
Vol 83 (5) ◽  
pp. 1047-1052
Author(s):  
Linda D Vargyas ◽  
Gregory E Walls ◽  
William R Bramstedt ◽  
Gary L Eilrich ◽  
O Bennett ◽  
...  

Abstract A collaborative study was conducted for the capillary gas chromatographic (GC) method for the simultaneous determination of the fungicide chlorothalonil (CTL) and the accompanying impurity, hexachlorobenzene (HCB), in technical and formulated materials. The method calls for the dissolution of technical and dry formulations of CTL and HCB from the aqueous flowable formulation. The 10 participating laboratories were asked to analyze the samples by adhering to the method as closely as their instrumentation and data systems allowed, and to note any deviations from the method. Collaborators were asked to prepare the standards and samples, set up the capillary GC systems, analyze the samples, and calculate the results. CTL produced reproducibility relative standard deviations (RSDR) of 0.4–2.5 (active ingredient concentrations ranged from approximately 52 to 98% by weight). HCB produced RSDR values of 5.2–22% (HCB concentrations were 0.02–0.04% by weight). The method was adopted First Action by AOAC INTERNATIONAL.


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.


1984 ◽  
Vol 30 (10) ◽  
pp. 1672-1674 ◽  
Author(s):  
N B Smith

Abstract In this method for detection and quantification of volatile alcohols by capillary gas chromatography, the serum sample is deproteinized, then directly injected into the gas chromatograph with 1-propanol as the internal standard. The capillary column is a 30-m bonded methylsilicone-coated, fused-silica column. With helium as the carrier gas, the injector inlet is set at a split ratio of 1/30 and the average linear velocity in the column is 25 cm/s. Injector and flame-ionization detector temperatures are 280 degrees C, oven temperature 35 degrees C. Chromatography time is less than 3 min.


2007 ◽  
Vol 56 (8) ◽  
pp. 405-415 ◽  
Author(s):  
Seiichi Shirasawa ◽  
Makoto Shiota ◽  
Hiroshi Arakawa ◽  
Yasuhiko Shigematsu ◽  
Kazuhisa Yokomizo ◽  
...  

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.


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