Switaj-Zawadka A, Konieczka P, Szczygelska-Tao J, Biernat J F, Namieśnik J
Department of Analytical Chemistry, Chemical Faculty, Gdansk University of Technology 11/12 Narutowicza Street, 80-952 Gdańsk, Poland.
J Chromatogr A. 2004 Apr 9;1033(1):145-51. doi: 10.1016/j.chroma.2004.01.025.
The new type of silica gel surface modification with using the trimethylamine as a reagent is described. The samples of chemically modified silica gel have been used for generation of gaseous standard mixtures (methyl chloride as a measurand) using the technique of thermal decomposition of the surface compound. The main aim of the research was to check the suitability of the new type of silica gel surface modification for obtaining methyl chloride as a measurand of gaseous standard mixture. The gaseous standard mixture obtained with using this technique was used for calibration of a thermal desorber-gas chromatography-flame ionization detector (TD-GC-FID) system. The homogeneity of coverage of silica gel surface with the immobilized compound has been evaluated. The full uncertainty budget of determination of liberated amount of methyl chloride has been calculated. The average amount of methyl chloride liberated from the unit sample of chemically modified silica gel is 3.59 +/- 0.13 mg g(-1). The influence of the modification way on the amount of liberated analyte has also been determined.
描述了一种以三甲胺为试剂的新型硅胶表面改性方法。化学改性硅胶样品已用于采用表面化合物热分解技术生成气态标准混合物（以氯甲烷作为被测量物）。该研究的主要目的是检验这种新型硅胶表面改性方法对于获得作为气态标准混合物被测量物的氯甲烷的适用性。使用该技术获得的气态标准混合物用于热解吸 - 气相色谱 - 火焰离子化检测器（TD - GC - FID）系统的校准。评估了硅胶表面固定化化合物覆盖的均匀性。计算了氯甲烷释放量测定的完整不确定度预算。化学改性硅胶单位样品释放的氯甲烷平均量为3.59±0.13 mg g(-1)。还确定了改性方式对被分析物释放量的影响。
