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我们在进行戊烷配位氯化反应的研究过程中,为了评价催化剂的活性和选择性,以及对反应机理的探讨都需对产物进行分离和鉴定。戊烷和氯代正戊烷三种异构体的混合物的色-质分析尚未见报导,为此我们用ZhD-01S色-质仪进行了研究。色谱分离用Chromosorb WAW(60～80目):角鲨烷=100:15,长4米的不锈钢填充柱,柱温75℃、载气N_2流量29ml/分的条件下可对混合物进行分离。在质谱条件:电离电压24V;分辨600(10％谷);加速电压4KV;倍增电压2.2KV;色谱进样灵敏度优于1×10~(-10)g/s下,对质谱色谱图的各峰扫描所得质谱图清晰可见。戊烷呈现链烷烃断链的规律,从M~+,(M-15)~+,(M-29)~+和(M-43)~+峰便可确认。对于氯代正戊烷,在
In the process of pentane coordination chlorination, we need to separate and identify the products in order to evaluate the activity and selectivity of the catalyst and to explore the reaction mechanism. Color-mass analysis of a mixture of three isomers of pentane and chloropentane has not been reported, and for this reason we performed a colorimetric-mass spectrometer with ZhD-01S. Chromatography Separation of the mixture was performed on a Chromosorb WAW (60-80 mesh): squalane = 100: 15, 4-meter stainless steel packed column at 75 ° C column temperature with a N 2 flow rate of 29 ml / min. Under the conditions of mass spectrometry, the ionization voltage is 24V; the resolution is 600 (10% valley); the accelerating voltage is 4KV; the doubling voltage is 2.2KV; the sensitivity of chromatographic injection is better than 1 × 10 -10 g / Peak scan spectrum clearly visible. Pentane shows the rule of chain breaking of paraffins, which can be confirmed from M ~ +, (M-15) ~ +, (M-29) ~ + and (M-43) ~ + For chlorinated n-pentane,