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Direct Sample Analysis - Atmospheric Pressure Chemical Ionization Source Performance Study

机译:直接样品分析 - 大气压化学电离源性能研究

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The Direct Sample Analysis APCI ion source enables rapid analysis of solid, liquid or gas commercial pharmaceuticals with little or no sample preparation. The Direct Sample Analysis APCI source Reagent Ion Gun consumes 1‐1.5 L/min of nitrogen flow with the ability to add controlled concentrations of liquid or gas reagent species to enhance sample signal intensity in positive and negative ion polarity modes. The Reagent Ion Gun location was optimal at a horizontal position in line with the capillary axis or at 15 deg inclined from vertical position with an offset along the x axis of – 2mm. The nitrogen gas flow rate through the Reagent Ion Gun was found to be optimum at 1.5 to 2 L/min. The counter current gas flow rate range from 2.5 to over 6 L/min yielded consistent signal intensity. The optimum Reagent Ion Gun exit aperture diameter was found to be 6.35 mm. Temperature at the sample surface was a primary variable determining signal intensity. The optimum temperature was sample dependent. Strong sample ion signals could be achieved at higher temperatures, but with increased sample carry over. The Reagent Ion Gun gas and counter current gas temperatures and flow rates combined to heat the sample surface as it moved through the ion sampling “sweet spot”. Typically the counter current gas temperature was fixed and the Reagent Ion Gun temperature was varied to provide sufficient sample ion signal intensity with minimum carry over.
机译:直接样品分析APCI离子源能够快速分析固体,液体或气体商业药物,少或无样品制备。直接样品分析APCI源试剂离子枪消耗1-1.5升/分钟的氮气流量,其能够增加受控浓度的液体或气体试剂物质以增强正极离子极性模式的样品信号强度。试剂离子枪定位在与毛细管轴线的水平位置处的水平位置最佳,或者从垂直位置倾斜,沿X轴沿2mm的X轴倾斜。发现通过试剂离子枪的氮气流量是最佳的1.5至2L / min。计数器电流气体流速范围为2.5至超过6L / min,得到一致的信号强度。发现最佳试剂离子枪出口孔径为6.35mm。样品表面的温度是主要可变测定信号强度。最佳温度依赖于样品。在较高温度下可以实现强的样品离子信号,但随着样品越来越多地携带。试剂离子枪气体和对应电流气温和流速组合以加热样品表面,因为它通过离子采样“甜点”。通常,逆流气体温度固定,并且试剂离子枪温度变化以提供足够的样品离子信号强度,最小携带。

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