A temperature programmed fractionation inlet system for mass spectrometers
A temperature programmed fractionation inlet system for mass spectrometers
复制标题
用于质谱仪的程序升温分馏入口系统
DOI：
10.1021/ac00244a061
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发表时间：
1982
影响因子：
7.4
通讯作者：
S. Wong
中科院分区：
文献类型：
--
作者：
K. Chan;R. Tse;S. Wong
可溶样品的质谱通常采用热解质谱法（Py-MS）获得。热解通常在质谱仪外的批处理系统中进行（1,2），或者在质谱仪离子源的直接入口探针的尖端进行（3-5），这两种情况通常在高真空下进行。当使用质谱仪外的热解器时，通常只有一小部分样品被输送到离子源。当使用离子源内部的热解器时，样品通常必须溶解并涂覆在热解器上，热解器通常是灯丝。这种热解器只能接受相对清洁的样品，以免污染离子源。通常通过脉冲加热(6)或弹道加热(4)来提高温度，但通过温度编程加热可以获得更多信息。构建了一种低成本的温度程序分馏器（TPF），它可以通过传统的射流分离器与任何质谱仪的离子源连接。随着温度的升高，分馏过程包括脱附、蒸发、蒸馏，最后是热解。这是在常压或亚大气压下在氦气流中进行的，从而避免了在批处理系统中热解产物本身之间可能发生的一些复杂反应。TPFinlet系统适用于处理易混淆、未经处理和杂乱的样品，因为它可以很容易地拆卸清洗，而无需停止质谱仪。作者注意到两个使用接口的类似设备的报告，每个都用于特定目的（7,8）。
Mass spectra of involatile samples are commonly obtained by pyrolysis-mass spectrometry (Py-MS). Pyrolysis usually takes place either in a batch system outside the mass spec-trometer (1, 2) or at the tip of a direct inlet probe in the ion source of the mass spectrometer (3-5), in both cases usually under high vacuum. When a pyrolyzer outside the mass spectrometer is used, usually only a small portion of the sample is bled to the ion source. When a pyrolyzer inside the ion source is used, the sample normally has to be dissolved and coated on the pyrolyzer, which is usually a filament. Such a pyrolyzer can accept onlyrelatively clean samples, for fear of contaminating the ion source. Temperature is commonly raised by either pulse heating (6) or ballistic heating (4), but more information can be obtained by temperature programmed heating.A low cost temperature programmed fractionator (TPF) has been constructed that can be interfaced with the ion source of any mass spectrometer through a conventional jet separator. As the temperature is raised, the fractionation process includes desorption, evaporation, distillation, and finally pyrolysis. This is carried out under atmospheric or subatmospheric pressure in a stream of helium, thus avoiding some of the possible complications of reactions among the pyrolyzates themselves in a batch system. The TPFinlet system is suitable for handling involatile, untreated, and messy samples, because it can easily be dismantled for cleaning without stopping the mass spectrometer. The authors are aware of two reports of similar devices that use interfaces, each used for a specific purpose (7, 8).