油菜籽油分及脂肪酸同时测定的气相色谱快速方法

本文拟定了对菜籽油分与脂肪酸组分同时测定的气谱快速方法,基于使用氢氧化四甲铵为催化剂,酯交换在汽化室以热解方式进行,可使油分定量地转换成脂肪酸甲酯。甲酯总峰面积的大小,可作为含油量的量度,与外标作比较,求得菜籽的含油率;再对各脂肪酸甲酯的峰面积作归一化法处理,便可求得各脂肪酸的含量;与油重法和IUPAC庚烷法测定结果相比较,其相对误差分别为±3％和±3—10％,符合快速分析的要求。

Measurement of Infinite Diluted Activity Coefficient of Solvents in Polymer by Inverse Gas Chromatography Method

The infinite diluted activity coefficients of solvents in polyisopropyl methylacrylate was measured using inverse gas chromatography. The solvents used were benzene, toluene, ethyl benzene, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methanol, ethanol isopropyl alcohol, butyl alcohol, 1,2-dichloroethane, and chloroform. It was observed that the infinite diluted activity coefficient of alcohols are well above those of the other solvents investigated.

Determination of constituents of essential oil from Angelica sinensis by gas chromatographymass spectrometry

Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.

Determination of the gas compositions for direct coal liquefaction by gas chromatography

Via multi-dimensional gas chromatography, configured with parallel dual-channel, double detectors, valves switching and back flushing, rapid analysis of the gas compositions consisting of C1-C5 hydrocarbons and permanent gases, such as CO2, H2S, H2, and CO, for direct coal liquefaction has been realized. With four packed chromatographic columns, which are Hayesep-Q pre-column, Hayesep-Q column, molecular sieve 5A column and one PLOT A1203 S capillary column, the gas compositions for direct coal liquefaction are analyzed qualitatively and quantitatively by the external standard method. The determination method has such advantages as excellent separation, simple operation, rapid analysis and accurate results.

Rapid Determination of Pesticide Residues in Fresh Sweet Corn

Objective] This study aimed to detect al organophosphate, organochlorine and pyrethroid pesticide residues in fresh sweet corn in one determination using a gas chromatograph. [Method] The pesticide residues in fresh sweet corn were ex-tracted and loaded to simultaneously the gas chromatograph Agilent 6890N which was equipped with two autosamplers, two columns and two detectors. [Result] Al the 26 pesticides were completely separated and eluted out within 25 min. The re-coveries of standard addition of the 26 pesticides ranged from 76% to 106%, with relative standard deviations （RSD） ranging from 0.5% to 8.9%. The linear regression equation fit wel from 0.050 to 1.500 mg/L corn extract （r2＆gt;0.996）. [Conclusion] The method is accuracy, which meets the requirements of pesticide residue analysis and can be used for the rapid detection, qualitative and quantitative analysis of pesticide residues in fresh sweet corn.

Optimization of Sample Pretreatment for Determination of Polycyclic Aromatic Hydrocarbons in Estuarine Sediments by Gas Chromatography

This study examined levels of polycyclic aromatic hydrocarbons (PAHs) in estuarine sediments in Licun (Qingdao, China) by gas chromatography under optimized conditions for sample pretreatment via ultrasonic extraction, column chromatography, and thin layer chromatography. Methanol and dichloromethane (DCM)/methanol (2:1, v/v) were used in ultrasonic extraction, and DCM was used as eluate for column chromatography. The developing system consisted of n-hexane and DCM at a ratio of 9:1 (v/v), with DCM as the extraction solvent for PAHs-containing silica gel scraped off the plate. When the spiking level is 100 ng, total recoveries of spiked matrices for four target PAHs (phenanthrene, anthracene, pyrene and chrysene) were 83.7%, 76.4%, 85.8%, and 88.7%, respectively, with relative standard deviation (RSD) between 5.0% and 6.5% (n = 4). When the spiking level is 1000 ng, associated total recoveries were 78.6%, 72.7%, 82.7% and 85.3%, respectively, with RSD between 4.4% and 5.3% (n = 4). The opti-mized method was advantageous for determination of PAHs in complex matrix due to its effective sample purification.

Determination of brominated diphenyl ethers in atmospheric particulate matter using selective pressurized liquid extraction and gas chromatography–mass spectrometry with a negative chemical ionization

This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.

Determinations of Air Tightness of Covered Slurry Storage Tanks Using Tracer Gas Technique

The objective of this investigation was to study whether it is possible to determine the air tightness of covered slurry storage tanks using tracer gas technique by injection of sulphur hexafluoride （SF6） and measurements of the decay in gas concentrations with an infrared spectrophotometer in the air space above the slurry. By measuring the decay in concentration of injected tracer gas at different occasions, the air exchange rate was determined. Three different types of coverings were studied namely; wooden roof, plastic tent and concrete roof.

Biodiesel Production by Enzymatic Catalysis Process Using Two Analytical Ways： Gas Chromatography and Total Glycerol Determination

Currently, biodiesel is presented as one of the best alternatives for gradually replacing the use of fossil fuels, but it has some factors that make it economically impractical if it does not have a government support. For this reason, research efforts focused on this area have been responsible for optimizing the process of biodiesel production by different catalytic routes to achieve greater efficiency at a lower cost. In this case, the biggest problem has been the high cost generated by an investigation, which in many occasions is the main factor to decide if an investigation could be carried out. Trying to reduce these costs, in the current study, we are using a technique of glycerol quantification by volumetric methods and comparing obtained results with the chromatographic method, which is conventionally used and comparatively much more expensive. Biodiesel employee was obtained by an enzymatic catalysis process varying one of three process variables：oil：alcohol molar ratio, temperature and proportion of catalyst. The numerical differences obtained between the two quantification methods generated relative errors lower than 10%, resulting in some occasions lower than 1%. By gas chromatography analysis the best yield was obtained at the same conditions of the volumetric method, a temperature of 45 ℃, an oil：alcohol ratio 1：4 and 8 wt.% of catalyst, but a yield of 95.5% and 97.1%, respectively. Due to the high precision of gas chromatography, this method is used to carry out a surface response analysis obtaining as ideal operating conditions a temperature of 43.5 ℃, 8.9 wt.%. of catalyst and an oil：alcohol ratio 1：4.

Determination of trace lead and mercury in airborne particles by hydride generation atomic fluorescence spectrometry

A new method for determination of trace lead and mercury by hydride generation atomic fluorescence spectrometry （HG-AFS） was established. Lead was determined in the medium of citric acid using potassium ferricyanide （K3Fe（CN）6） as oxidant. Ni enhanced the fluorescence signals in this system. Mercury was determined in the medium of nitric acid using mixture of thiourea and ascorbic acid as masking reagent, sodium dioctylsulphosuccinate （SDSS） as enhancing reagent. The working mechanism of the hydride generation of lead and mercury was discussed. Interferences of some coexisting ions were studied systematically and the determination conditions were optimized. Under the optimized conditions, the detection limits of the method were 0.31μg.L^-1 for lead and 0.023 μg·L^-1 for mercury, and the relative standard deviations based on eleven determinations of 5.00 μg·L^-1 standard of Pb and Hg, were 2.6% for Pb and 2.2 % for Hg. This method was applied to the analysis of lead and mercury in four different diameter airborne particles after microwave digestion. Results suggested heavy metal elements easily concentrated in smaller particles.

Determination of Trihalomethanes in Water Samples Using Headspace Solid-Phase Microextraction Gas Chromatography

The chlorination process is one of the water treatment method used for the disinfection of water. The disinfection by products are trihalomethanes such as chloroform, dichloromethane, dibromochloromethane and bromoform. A headspace solid-phase microextraction method has been developed for determination oftrihalomethanes in water samples. The experimental parameters such as the stirring rate, extraction time, extraction temperature and desorption time were investigated. The linearity, detection limits and percentage recovery were evaluated. The optimum conditions were stirring rate 800 rpm/min, extraction time 6 min, extraction temperature 20 ~C, desorption time 2.5 min and desorption temperature 220 ~C. The detection limits were 0.01 ~g/L and the recoveries were in the range of 86-110 %, The proposed method was successfully applied to determination of THM4 in tap water samples. The THM4 contents were varied depending on the sample sites and the season. The total THM4 contents in cool, summer and rainy season were in the range of 27.58-41.89, 32.06-60.73 and 46.26-69.87 p.g/L, respectively. Confirmation of the detected compounds in water samples were performed by gas chromatograph-mass spectrometer. The mass spectra of the target compounds in water samples is in good agreement with trihalomethanes standard spectra.

Research on Comparison of Gas Chromatography and Liquid Chromatogram Detecting Pesticide Residue

The existing methods of detecting pesticide residue include gas chromatography, high performance liquid chromatography, gas chromatograph-mass, liquid chromatograph-mass, capillary electrophoresis, radioimmunoassay, biosensor and rapid detection on the spot. The paper analyzes the comparison of gas chromatography and liquid chromatogram detecting pesticide residue, for achieving the development tendency and the future goal of analyzing pesticide residue.

Quantification of selected monohydroxy metabolites of polycyclic aromatic hydrocarbons in human urine

An analytical method was developed to quantitatively determine selected monohydroxy metabolites of polycyclic aromatic hydrocarbons(PAHs) in human urine. The procedure included enzymatic hydrolysis to cleave the conjugated metabolites, solid-phase microextraction enrichment, and gas chromatography-mass spectrometry analysis. The method proved to be sensitive enough to detect the selected PAH metabolites in human urine.