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massegb [2026/04/08 18:29] – administratormassegb [2026/04/08 19:19] (aktuell) – [Preparing samples] administrator
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 ====== Mass spectrometry ====== ====== Mass spectrometry ======
-There are multiple methods for mass spectrometry and means of ionization. However most of them are not suitable for samples from the organometallic / elementorganic field since inert application methods and soft ionization is usually necessary. In these cases the LIFDI-MS (//Liquid Injection Field Desorption Ionization Mass Spectrometry//) method has proven its strength. Samples are applied with a capillary through a septum from a sealed vial while the ionization method itself is also amongst the softest there is. For more information on LIFDI-MS I recommend reading this [[https://www.linden-cms.de/|website (external link)]].+There are multiple methods of mass spectrometry and ionization. However, most of these methods are not suitable for organometallic/elementorganic samples, since inert application methods and soft ionization are usually necessary. In these cases, the liquid injection field desorption ionization mass spectrometry (LIFDI-MS) method has proven effective. Samples are introduced through a capillary from a sealed vial with a septum, and the ionization method itself is one of the softest available. For more information on LIFDI-MS I recommend reading this [[https://www.linden-cms.de/|website (external link)]].
  
 ===== Preparing samples ===== ===== Preparing samples =====
  
-ssss+To prepare a sample in a glovebox I recommend using these small vials with a crimpable septum cap ({{ref>vials}}).
  
 <figure center|vials> <figure center|vials>
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 </subfigure> </subfigure>
 <subfigure|subfig_b_label> <subfigure|subfig_b_label>
-{{:analytik:masse:signal-2026-04-07-175444_004.jpeg?direct&200 | title}}+{{:analytik:masse:signal-2026-04-07-175444_004.jpeg?direct&250 | title}}
 <caption></caption> <caption></caption>
 </subfigure> </subfigure>
 <subfigure|subfig_b_label> <subfigure|subfig_b_label>
-{{:analytik:masse:signal-2026-04-07-175444_005.jpeg?direct&200 | title}}+{{:analytik:masse:signal-2026-04-07-175444_005.jpeg?direct&250 | title}}
 <caption></caption> <caption></caption>
 </subfigure> </subfigure>
-<caption>Vial with a crimpable septum cap.</caption>+<caption>Vial with a crimpable septum cap and the data sheets.</caption>
 </figure> </figure>
 +
 +A crimp tool is also needed for the caps ({{ref>zange}}).
 +
 +<figure center|zange>
 +{{:analytik:masse:signal-2026-04-07-175444_008.jpeg?direct&400 |title}}
 +<caption>A crimp tool.</caption>
 +</figure>
 +
 +To prepare your sample, you must first prepare a solution of the substance. In most cases, toluene has proven to be an effective solvent. It has a high boiling point, which is necessary because solvents with lower boiling points may evaporate prematurely, leading to a clogged cannula. Some substances, especially polar ones, may not dissolve easily in toluene. In these cases, adding one to a few drops of fluorobenzene has proven helpful. Since this method is very sensitive, dissolving 1 mg of substance in 1 mL of solvent is more than enough. It is also good practice to first prepare the solution in another vial and then filter it into the actual vial to prevent residual solids from clogging the cannula.
 +