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971.
溶胶-凝胶毛细管气相色谱柱热稳定性的考察 总被引:13,自引:0,他引:13
溶胶—凝胶毛细管气相色谱柱是一类新型的色谱柱。通过与静态法涂渍并用自由基引发交联使固定相固载化的色谱柱比较,溶胶—凝胶色谱柱除了具有制作工艺简单、分离效果好等特点外,还具有很好的热稳定性和溶剂稳定性。其工作温度可高于400℃。 相似文献
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975.
Pentti Passiniemi 《Journal of solution chemistry》1983,12(11):801-813
A simple and absolute closed capillary method is introduced for measuring tracer diffusion coefficients in liquids with both - and -active tracers. In this method a narrow capillary is partially filled with a labelled solution and an unlabelled solution is used to fill the rest of the capillary. The diffusion coefficient is obtained from the time dependence of the monitored activity when the length of the capillary is known. The method has been tested by remeasuring the tracer diffusion coefficients of22NaCl and Na36Cl for solutions covering a wide range of total NaCl concentration. The average precision of the measurements was about 0.3%. The results obtained for Na36Cl tracer diffusion are in good agreement with the data found in literature. The22NaCl tracer diffusion coefficients that were measured in dilute solutions agree well with those obtained using the continuous open-ended capillary method but differ from results for solutions between 0.1 and 1M obtained with the diaphragm cell method. 相似文献
976.
A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5 g of freeze-dried apple tissue with 30 mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2 g of ascorbic acid/L, for 10 min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed. 相似文献
977.
Paul V. Doskey 《Journal of separation science》1991,14(11):724-728
A comparison has been made between two cryogenic preconcentration - high resolution gas chromatography techniques for the analysis of non-methane hydrocarbons in ambient air, one involving treatment of air samples with magnesium perchlorate to remove water, the other involving analysis without treatment. Recoveries of C1-, C2-, and C3-substituted benzenes in treated samples were 80%, 50%, and 50%, respectively. Incomplete recovery of C7-C9 n-1-olefins was also observed. C2-C8 hydrocarbons and C2-C6 n-1-olefins were recovered with greater than 90% efficiency. Analyses of certified audit samples containing a mixture of C2-C8 aliphatic and aromatic hydrocarbons at the 20 ppbv level in humidified zero-grade air indicated that the accuracy of the technique for untreated air samples was approximately 90%. The use of magnesium perchlorate for water removal cannot be recommended for the analysis of non-methane hydrocarbons in ambient air. 相似文献
978.
New possibilities for using the equation that takes into account the nonlinear variation of parameters of the reference n-alkane scale for the calculation of retention indices of polar substances at different modes of temperature programming were considered. The advantages of this equation over the linear scale used traditionally were demonstrated in relation to C3—C11 alkan-1-ols. The equation appears to have considerable promise regarding the search for the equivalent isothermal index. 相似文献
979.
蜂蜜含糖量的高效毛细管电泳测定研究 总被引:6,自引:3,他引:6
利用自制的毛细管电泳-电化学安培检测装置,以铜电极为工作电极,在氢氧化钠介质中,分别对2种蜂蜜样品中的糖类化合物进行分离检测,结果满意。 相似文献
980.
A sensitive method for enantioseparation of a basic drug rivastigmine and determination of its optical impurityby capillary electrophoresis with highly sulfated β-cyclodextrin(HS-β-CD)as the chiral selector is described.Ingeneral,enantioseparation of basic chiral compounds is carried out in acidic condition(pH 2.5)to prevent analytesfrom adsorption on the capillary wall.However,in the case of rivastigmine,the detection sensitivity was too limitedto determine the optical impurity of S-rivastigmine lower than 1% when buffer pH was 2.5.It was found that thedetection sensitivity was improved 1.6 times just by raising the buffer pH value from 2.5 to 5.8.The poor columnefficiency due to the adsorption of the analytes on the capillary wall was resolved by using dynamical coating of thecapillary wall with the linear polyacrylamide solution.The experirnental parameters such as the concentration ofHS-β-CD,buffer pH and buffer ionic strength were optimized,respectively.The method was validated in terms ofrepeatability,linearity,limit of detection(LOD)and limit of quantitation(LOQ).Using the present method,the op-tical purity of nonracemic rivastigmine with the enantiomeric excess(ee)value of 99.14% was determined. 相似文献