共查询到20条相似文献,搜索用时 11 毫秒
1.
An integrated analytical procedure for polychlorinated biphenyl (PCB) multiresidues in environmental samples has been developed and applied to well-characterized samples. PCB residues are characterized and quantified using wall coated open tubular column (WCOT) gas chromatography or HRGC/MS-selected ion monitoring. An automated data system based on a Spectra Physics SP-4200 computing integrator is used to select and quantitate peaks of individual congeners and homolog groups. This procedure consistently yields results with a reproducibility within 3 percent for HRGC-ECD and 3.7 percent for HRGC/MS-SIM technique respectively. 相似文献
2.
Summary GC-MS analysis of hydrocarbons, thermally mobilized from rock and coal samples (“thermodesorption”) at 320°C, provides valuable
and readily available information of organic geochemical significance. Two oil shale and three coal samples of different rank
have been selected for this study. The molecular patterns of compound classes of various saturated and aromatic hydrocarbons
are recorded here by employing mass chromatography of selected ions. The method described is of particular importance for
the detection of those volatile constituents in coals and sedimentary rocks, which are usually not recovered during elaborate
workup procedures (i.e. solvent extraction, liquid chromatography) due to evaporation losses. 相似文献
3.
Eva Matisov 《Journal of separation science》1992,15(4):213-218
The scope of the principal techniques employed for the analysis of hydrocarbon mixtures is discussed, with emphasis on the analysis of one and two ring aromatic compounds by single column capillary gas chromatography. The paper considers both the column and the selection of the temperature regime (isothermal and temperature programmed). Much space is devoted to the characterization of the compounds by means of retention data. 相似文献
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Summary A method for determining cyclo C6-C7-peroxides and hydroperoxides by high-resolution capillary GC has been developed. The compounds were synthesized in the liquid
phase and identified in chromatograms of the reaction mixture of cyclohexyl hydroperoxide and cycloheptane using GC-MS. Peroxy
compounds were determined using an FID. The effective carbon number (ECN) concept was used to calculate response factors of
the peroxy compounds analysed. The experimentally determined response factor for cyclohexyl hydroperoxide was identical (within
error limits) with that calculated. 相似文献
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Summary Group separation of malthene fractions of tar samples obtained from brown coals of different ranks at two different temperatures
(500 and 800°C) was performed by HPLC using amino-cyano bonded phase packing with two eluent systems of different polarities
and backflushing technique. Group composition of different tar samples was compared and evaluated. Amount and distribution
of volatile compounds in the malthene fractions were determined by capillary gas chromatography on a CP-Sil 5 WCOT column.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
9.
H. G. Struppe F. Franke J. Hofmann B. Ondruschka 《Journal of chromatography. A》1996,750(1-2):239-244
In contrast to usability of Curie-point pyrolysis at 700°C directly attached to gas chromatography-mass spectrometry (GC-MS) for determination of organic wood preservatives in waste wood samples the investigation method reported here consists of thermal desorption at temperatures about 260°C in connection with GC-MS for peak identification or GC with flame ionization detection for quantitative analyses. So-called “modified closeable sampling columns” are used as batch-reactor in thermal desorption experiments. Desorbed vapours can be introduced on capillary columns without sample discrimination and without a disturbing lost of resolution. In this manner a lot of individual polycyclic aromatic hydrocarbons were determinated in waste wood samples, especially in railway sleepers. 相似文献
10.
Summary Al2O3-PLOT columns are used with great advantage for the analysis of volatiles, because of the increased capacity ratio and selectivity compared to WCOT-columns. Their applicability is limited to relatively non-polar components with relatively low boiling points i. e. eluting before n-decane.In the analysis of the halocarbons in stratospheric air, the decomposition of certain compounds was observed. In this study the stability of a number of volatile organic compounds was determined in function dependence of the column temperature using a two-dimensional GC-system.A possible reaction mechanism for the decomposition is proposed and confirmed for several chlorinated ethanes. 相似文献
11.
Prieto-Blanco MC López-Mahía P Campíns-Falcó P 《Journal of chromatography. A》2011,1218(30):4834-4839
A new device for carbonyl compounds based on coupling on-line and miniaturizing both, sample pretreatment and chromatographic separation, is reported. Two capillary columns, a GC capillary column (95% methyl-5% phenyl substituted backbone, 70 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve for in-tube solid-phase microextraction (IT-SPME) and a Zorbax SB C18 (150 mm × 0.5 mm i.d., 5 μm particle diameter) LC capillary column were employed. Different combinations of IT-SPME and derivatization using 2,4-dinitrophenylhydrazine (DNPH) were examined for mixtures containing 15 carbonyl compounds (aliphatic, aromatic and unsaturated aldehydes and ketones). A screening analysis of aqueous extracts of atmospheric particulate PM(10) was carried out. Moreover, the possibility of coupling IT-SPME and conventional liquid chromatography is also tested. Derivatization solution and IT-SPME coupled to capillary liquid chromatography provided the best results for achieving the highest sensitivity for carbonyl compounds in atmospheric particulate analysis. Detection limits (LODs) using a photodiode array detector (DAD) were ranged from 30 to 198 ng L(-1), improving markedly those LODs reported by conventional SPME-LC-DAD. 相似文献
12.
L. Zenon-Roland R. Agneessens P. Nangniot H. Jacobs 《Journal of separation science》1984,7(8):480-484
13.
Two physiologically important forms of vitamin D exist: vitamin D2 and vitamin D3, which by liver based hydroxylase enzymes are converted to 25-hydroxyvitamin D2 and 25-hydroxyvitamin D3, respectively. These hydroxylated metabolites of vitamin D are measured in plasma to assess the vitamin D status of animals and humans. Therefore cheap and reliable analytical methods are very much in demand in nutritional and physiological research. After saponification and extraction of plasma or serum samples the current method uses reverse phase high performance liquid chromatography on a C30 column and with UV detection at 265 nm for quantifying vitamin D2, vitamin D3, 25-hydroxyvitamin D2, and 25-hydroxyvitamin D3. The method proved versatile with respect to plasma lipid content, sample amount, and plasma concentration of the vitamin D metabolites as it was tested using plasma from six different species: cattle, pigs, poultry, mink, horses, and humans. In cattle plasma recoveries were between 86.6 and 101.0%, within day error between 0.9 and 5.9%, and between day error between 0.2 and 1.7%. However, depending on species and sample amount error percentages varied. When running the method on standard reference material® 972 “Vitamin D in human serum” from the National Institute of Standards and Technology (NIST) (Gaithersburg, USA) the results for 25-hydroxyvitamin D2 and 25-hydroxyvitamin D3 concentrations were within the boundaries provided by NIST, reflected by Z-scores between 0.1 and 0.9. 相似文献
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The enthalpies of solution of N,N′-dimethylethyleneurea (1,3-dimethyl-2-imidazolidinone) in water, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, and t-butanol (2-methyl-2-propanol) were measured calorimetrically at 298.15 K. For comparison purposes, the previous data on enthalpic effects of 1,1,3,3-tetramethylurea dissolution (solvation) in the same solvents were analyzed. It has been concluded that the intramolecular cyclization of tetramethylurea, to form dimethylethyleneurea, results in strengthening of the solute solvation and this tendency is more pronounced in a non-aqueous (alcoholic) medium. 相似文献
16.
Jinzhang Gao Haifeng Fan Wu Yang Xiangli Sun Chongyang Li Xuefeng Mao Jie Wang Rong Wang Zhengping Jia 《Central European Journal of Chemistry》2008,6(4):617-621
A rapid, simple and reliable capillary electrophoresis method for the separation and quantitation of inorganic cations with
indirect UV detection at 214 nm was developed. The electrolyte was: 12 mM imidazole as background absorbance provider; 5 mM
malic acid and 1.0 mM 18-crown-6 ether as complexing agents; and 20% D2O (v/v) to improve ion mobility. The pH was 4.25. The applied voltage was 22 kV at 22°C. Nine ions were completely separated
and determined with correlation coefficients of 0.9979-0.9992. The relative standard deviations (RSD) were less than 0.5%
for migration time and less than 5.2% for peak area (n=8). The detection limits (S/N=3) were from 0.08 mg L−1 (for Na+) to 0.51 mg L−1 (for Cu2+). To assess the reliability atomic absorption (AA) was also used to determine the same samples. Satisfactory results were
obtained for real samples of jasmine tea drink and coconut milk.
相似文献
17.
In this study, a novel extraction and enrichment technique based on superparamagnetic high-magnetization C18-functionalized magnetic silica nanoparticles (C18-MNPs) as sorbents was successfully developed for the determination of methylprednisolone (MP) in rat plasma by high performance liquid chromatography (HPLC). The synthesized silica-coated magnetite modified with chlorodimethyl-n-octadecylsilane was about 320 nm in diameter with strong magnetism and high surface area. It provided an efficient way for extraction and concentration of MP in the samples through hydrophobic interaction by the interior C18 groups. Moreover, MP adsorbed with C18-MNPs could be simply and rapidly isolated through placing a strong magnet on the bottom of container, and then easily eluted from C18-MNPs by n-hexane solution. Extraction conditions such as amounts of C18-MNPs added, adsorption time and desorption solvent, were investigated. Method validations including linear range, detection limit, precision, and recovery were also studied. The results showed that the proposed method based on C18-MNPs was a simple, accurate and high efficient approach for the analysis of MP in the complex plasma samples. 相似文献
18.
A selective and sensitive high resolution gas chromatography assay for simultaneous determination of Ibuprofen and its major metabolites in urine is described. Biological samples were collected from healthy volunteers after a single topical administration of the drug in gel form. The chromatographic system, developed on a WCOT OV-1 glass capillary column, ensured a clear separation of Ibuprofen and its metabolites and their quantitative evaluation. 相似文献
19.
Diagnosis of lubricating oil by evaluating cyanide and carbon molecular emission lines in laser induced breakdown spectra 总被引:1,自引:0,他引:1
I.Y. Elnasharty A.K. Kassem M. Sabsabi M.A. Harith 《Spectrochimica Acta Part B: Atomic Spectroscopy》2011,66(8):588-593
To prevent engine failure it is essential to change lubricating oil regularly before it loses its protective properties. It is also necessary to monitor the physical and chemical conditions of the oil to reliably determine the optimum oil-change intervals. The present work focuses on studying evolution of the cyanide (CN) and carbon (C2) molecular spectral emission lines in the laser induced breakdown spectra of lubricating oil as a function of its consumption. The intensities of these molecular bands have been taken as indicator of engine oil degradation at certain mileage. Furthermore, the percentage of decay of CN and C2 integral intensity values at the corresponding mileage was calculated in order to relate it to the degree of consumption of the motor oil. Such percentage decay of the CN and C2 integral intensities have been found to increase gradually with increasing mileage which is accompanied with increasing depletion of engine oil. The results of using LIBS technique in the present measurements proved that it is possible to have a direct, straightforward and easy method for prediction of lubricating oil degree of consumption. This may facilitate scheduling the proper time and/or mileage intervals for changing the oil to avoid any possibility of engine failure. 相似文献
20.
The performances of three adsorbents, i.e. silica gel, neutral and basic alumina, in the separation of short chain polychlorinated n-alkanes (sPCAs) from potential interfering substances such as polychlorinated biphenyls (PCBs) and organochlorine pesticides were evaluated. To increase the cleanup efficiency, a two-step cleanup method using silica gel column and subsequent basic alumina column was developed. All the PCB and organochlorine pesticides could be removed by this cleanup method. The very satisfying cleanup efficiency of sPCAs has been achieved and the recovery in the cleanup method reached 92.7%. The method detection limit (MDL) for sPCAs in sediments was determined to be 14 ng g−1. Relative standard deviation (R.S.D.) of 5.3% was obtained for the mass fraction of sPCAs by analyzing four replicates of a spiked sediment sample. High resolution gas chromatography/electron capture negative ion–low resolution mass spectrometry (HRGC/ECNI–LRMS) was used for sPCAs quantification by monitoring [M−HCl]− ions. When applied to the sediment samples from the mouth of the Daliao River, the optimized cleanup method in conjunction with HRGC/ECNI–LRMS allowed for highly selective identifications for sPCAs. The sPCAs levels in sediment samples are reported to range from 53.6 ng g−1 to 289.3 ng g−1. C10- and C11-PCAs are the dominant residue in most of investigated sediment samples. 相似文献