Name: analysis of volatile and oxidation sensitive compounds using a cold inlet system and electron impact mass spectrometry
Uploaded: 2014-09-05T15:00:00
Description: Watch this Scientific Journal Video about Analysis of Volatile and Oxidation Sensitive Compounds Using a Cold Inlet System and Electron Impact Mass Spectrometry at JoVE.com

JS is indebted to Prof. B. Hoge of the Inorganic Chemistry department, Bielefeld University, for the idea of establishing the presented inlet system. The analyzed phosphane was a generous gift from Prof. B. Hoge. Sample preparation of the analyzed compound was performed by M. Wiesemann. Photographs of the phospane were taken by Dr. J. Bader. The mechanical workshop of the faculty of chemistry is acknowledged for the manufacturing of the interface and the glass workshop of the faculty of chemistry for the manufacturing of the lockable test tubes with flanges. Prof. B. Hoge and Prof. H. Gr&#246;ger are acknowledged for funding of this publication.

1，样品制备<ol><li>使用定制的可锁定的试管有凸缘（ 图1），用于运输和样品转移到质谱仪。之前填充样品，疏散附着到多个歧管的Schlenk线的可锁定的试管，通过加热用热枪除去残留的水。泄试管用干燥氩气，并再次抽空，同时加热。 </li><li>沉浸在上锁的试管成冷阱充满液氮（注意：用液氮时要小心）。浓缩样品到从连接到的Schlenk线的歧管的样品容器的试管中，收在试管的顶部锁...

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从在标准样品制备程序，分解的化合物收购质谱载于本协议。所提出的技术被设计为金属organyls，硅烷和膦，这是很容易受到氧化和/或水解的分析，使得它有趣特别是对于无机化学家。为了达到最佳的效果，真空或空气的条件下在整个分析加以保存。因此该协议应认真遵守。的情况下，分析物进入与空气接触泄漏或错误处理的进口系统的，因为，造成严重后果如样品容器的爆炸可根据化合物的情?...

化合物，如金属organyls，硅烷，或phosphanes通过质谱法的分析并不总是可行的。几个这些化合物是已知的时，分解迅速与空气接触。因此，测量的质谱时，最重要的步骤是样品制备中，分析物的转移到质谱仪和离子发生在不存在空气。在这个协议中，我们描述了一种策略，以满足这些要求，并提出了一个入口系统，这使得它能够得到挥发性化合物以前没有被进行质谱分析的质谱图，由于其难以处理和快速分解的环境条件下。由此，明确识别新的或现有的挥发性金属organyls，硅烷和phosphanes，易被氧化或水解的，现在可以与质谱的协助下进行的。有两个要求其具有为了分析化合物必须满足这易于氧化或水解：在惰性条件下的样品制备和离子产生。最后的前提下可使用质谱仪的离子源在真空下操作很容易地得到满足。这与大部分基质辅助激光解吸/电离（MALDI）质谱，并与所有的电子轰击离子源（EI）质谱仪1,2的情况。电喷雾电离（ESI）是不为易被氧化或水解的化合物的分析很容易兼容，如在电离过程需要在环境条件3下的地方。然而，对于一些化合物，它们与氧或水，干燥，并与该最ESI源操作雾化气体的反应不大力是通过质谱法4足够用于分析。这也是对于电离策略类似于ESI， 例如 ，低温ESI，低温大气压电离和低温液体二次离子质谱SPECTR的情况下ometry 5-7。与此相反，样品制备和转移到惰性条件下的离子源是更有挑战性。两个MALDI和ESI文书已加上手套箱中以使在惰性气氛中4,8易于氧化和/或水解的化合物的样品制备方法。质谱仪接口到手套箱中任一个传输毛细管（ESI）或直接连接到手套式操作箱（MALDI）。液体喷射场解吸/电离（LIFDI） - -与敏感化合物的分析报告9,10的手套箱中，以经由传输毛细管质谱仪的耦合也将使用另一种离子化的策略是可能的。 此外，MALDI和LIFDI不适合于高挥发性化合物的分析。 MALDI需要的共结晶的分析物与基质和LIFDI需要被分析物上的沉积中的EMITTER从一个解决方案。与两个离子化策略是非常可能的是，分析物将蒸发随着溶剂。在对比MALDI仪器，EI质谱仪通常提供了几种方法用于引入样品进入离子源：直接导入探针（少量的固体颗粒，油，或蜡沉积到其使用推杆引入铝坩埚中） ，隔片入口（液体），或耦合用气相色谱仪。再次，在至少部分样品转移发生在环境条件下是难以在惰性气氛下进行。 在20世纪60年代，进样系统，提出了使样品的引入真空成的EI仪器的离子源-全玻璃加热进气系统（AGHIS）11,12。这里，将样品位于密封件的玻璃毛细管，将其插入到AGHIS内。接着，AGHIS抽真空和与所述样品的玻璃容器破裂。该AGHIS随后，加热以蒸发其中通过的泄漏装置达到的EI质谱仪的离子源的样品。当制备在手套箱内用样品的玻璃毛细管中，样品可以被引入到质谱仪中，没有任何接触到空气。然而，AGHIS是它不是市售的，难以组装，即使是熟练的吹玻璃车间的设备。由于直接入口之间的大尺寸切换使用推杆和AGHIS不是直线前进。 在我们的质谱实验室，我们在AGHIS的风格开发出了类似的进气系统。然而，由于这是不可能的加热进口系统中，分析物具有表现出以进入质谱仪的离子源有一定的波动。分析物的挥发性必须足够，以允许化合物在真空下在液氮德转印温度 - 无论是煮沸或升华。该定制进气系统包括一个不锈钢板，其被定位在直接进样系统，不锈钢管与针型阀，和一个凸缘，以可连接含有样品可锁定试管。冷进样系统的安装无需修改质谱仪（高分辨磁质谱AutoSpec X，真空发生器，现在Waters公司，英国曼彻斯特） - 冷进气系统和直接入口之间使用，可以在几秒钟内轻松完成推杆切换。 所呈现的进口系统是特别有用的，当金属organyls，硅烷，或phosphanes，易被氧化或水解，必须进行分析。这些化合物被用核谱核磁共振（NMR）或红外（IR）光谱法常用分析。不幸的是，这些方法允许并不总是一个明确的鉴定的化合物，因为它们产生incompletE资料， 例如 ，当元件如氯或溴是该分子的一部分。另一方面气体电子衍射可以提供关于分析物的详细信息，但是，该方法是非常耗时的，样品的制备是困难的，并且只有少数群体能够进行这些分析13,14。这里，对于金属organyls，硅烷，或phosphanes，易被氧化或水解被EI质谱分析中的冷进气系统是有机化学家能够明确识别的新型化合物大量使用对（上）由与信息提供他们关于特征碎片离子的分子和质量。为质谱的一种物质对测量的唯一先决条件是在减压一定的波动性。

<table border="0" cellpadding="0" cellspacing="0" width="971">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Name of Reagent/Material</td>
			<td style="width:71px;">Company</td>
			<td style="width:155px;">Catalog Number</td>
			<td style="width:435px;">Comments</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:311px;">VG Autospec X</td>
			<td colspan="2">Micromass Co. UK Ltd (now Waters)</td>
			<td style="width:435px;">other EI mass spectrometers with direct inlet using a push rod should also be compatible with this technique</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Lockable test tubes with flange</td>
			<td style="width:71px;">-</td>
			<td style="width:155px;">-</td>
			<td style="width:435px;">costum made, teflon tap should be used for locking the test tube</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:311px;">Interface for lockable test tubes</td>
			<td style="width:71px;">-</td>
			<td style="width:155px;">-</td>
			<td style="width:435px;">costum made , interface is prepared from stainless steel. Needle valve has to be included into the interface-design!</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:311px;">Schlenk line</td>
			<td style="width:71px;">-</td>
			<td style="width:155px;">-</td>
			<td style="width:435px;">costum made, has to include vacuum pump for evacuation of thest tubes and cold trap with liquid nitrogen for trapping of the sample</td>
		</tr>
	</tbody>
</table>

analysis of volatile and oxidation sensitive compounds using a cold inlet system and electron impact mass spectrometry

这部影片提出了一个协议，用电子轰击电离挥发和氧化敏感的化合物的质量spectrometrical分析。挥发和氧化敏感的化合物通过质谱法的分析是不容易实现的，因为国家的最先进的所有质谱方法所需要的分析物（电喷雾电离），共中的至少一种的样品制备步骤， 例如 ，溶解和稀释与基质化合物（基质辅助激光解吸/电离），或所制备的样品转移到质谱仪的电离源分析物-crystallization，大气压的条件下进行。这里，使用进样系统的描述使用扇区字段质谱仪配备有电子轰击电离源挥发性金属organyls，硅烷，和phosphanes的分析。所有的样品制备步骤和样品引入的离子源质谱仪发生或者下无空气条件下或在真空条件下，使化合物的分析非常容易被氧化。所提出的技术是为无机化学家兴趣尤其，与金属organyls，硅烷，或phosphanes，它必须使用在惰性条件，如的Schlenk技术进行处理工作。操作的原理，提出在该视频。

的三（三氟甲基）膦的EI质谱示于图3中 ，化合物，其分解时迅速与空气（ 图4）接触。所呈现的界面允许质谱对这些化合物的直线前进的测量。新颖界面的操作是容易和快速的和操作的质谱仪，当与常规应用于直接入口使用推杆并没有任何障碍。 <img alt="图3" fo:content-width="5in" src="/files/ftp_upload/51858/51858fig3highres.jpg" width="500"...

Watch this Scientific Journal Video about Analysis of Volatile and Oxidation Sensitive Compounds Using a Cold Inlet System and Electron Impact Mass Spectrometry at JoVE.com

Analysis of Volatile and Oxidation Sensitive Compounds Using a Cold Inlet System and Electron Impact Mass Spectrometry

挥发和氧化敏感的化合物使用冷进气系统和电子轰击质谱分析

这部影片提出了一个协议，用电子轰击电离挥发和氧化敏感的化合物的质量spectrometrical分析。所提出的技术是为无机化学家兴趣尤其，与金属organyls，硅烷，或具有使用惰性条件下，例如在的Schlenk技术进行处理phosphanes工作。

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The ...

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