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A student is given a mixture of two unknown substances, one organic and one inorganic, and is asked to identify these compounds using mass spectrometry. Can you provide a step-by-step procedure using mass spectrometry to identify the two unknown compounds?

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Step 1: Sample preparationFirst, the student must prepare the sample for mass spectrometry analysis. This involves dissolving the mixture in a suitable solvent, such as methanol or acetonitrile. The sample should be filtered to remove any particulate matter that could interfere with the analysis.Step 2: IonizationNext, the student must ionize the sample. There are several ionization techniques available, but the most common for organic and inorganic compounds are electrospray ionization  ESI  and matrix-assisted laser desorption/ionization  MALDI . In ESI, the sample is sprayed through a charged needle, creating charged droplets that evaporate to produce ions. In MALDI, the sample is mixed with a matrix and irradiated with a laser, causing the matrix to absorb the energy and ionize the sample.Step 3: Mass analysisThe ionized sample is then introduced into the mass spectrometer, where the ions are separated based on their mass-to-charge ratio  m/z . There are several types of mass analyzers, such as time-of-flight  TOF , quadrupole, and ion trap. The choice of mass analyzer depends on the specific requirements of the analysis, such as mass range, resolution, and sensitivity.Step 4: DetectionAfter the ions are separated, they are detected by a detector, such as an electron multiplier or a Faraday cup. The detector generates a signal proportional to the number of ions striking it, which is then amplified and recorded.Step 5: Data analysisThe recorded data is displayed as a mass spectrum, which is a plot of ion intensity versus m/z. The student must analyze the mass spectrum to identify the peaks corresponding to the organic and inorganic compounds. This can be done by comparing the observed m/z values to those of known compounds in a database or by using software that can predict the molecular formula and structure based on the mass spectrum.Step 6: Fragmentation  if necessary If the mass spectrum does not provide enough information to identify the compounds, the student may need to perform tandem mass spectrometry  MS/MS  to obtain additional structural information. In MS/MS, selected ions from the first mass analysis are fragmented into smaller ions, which are then analyzed in a second mass analyzer. The resulting fragment ions can provide valuable information about the structure of the parent ion, helping to confirm its identity.Step 7: IdentificationOnce the student has gathered sufficient information from the mass spectrum and any additional fragmentation data, they can confidently identify the organic and inorganic compounds in the mixture. This may involve comparing the observed data to reference spectra, consulting a database of known compounds, or using software to predict the most likely structures based on the experimental data.

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