mass spectrometry worksheet - chem 212: analytical · pdf filemassspectrometry$worksheet$...

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1 Mass Spectrometry Worksheet CHEM 212 1. What is separated and detected by mass spectrometers? 2. Below is a generalized schematic of the components of a mass spectrometer. Circle and label each of the above phases in the figure below. Ionization Methods 3. Define the following terms: Base peak Molecular ion ionization ion acceleration selection of ions detection

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Page 1: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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Mass  Spectrometry  Worksheet  CHEM  212  

 1. What  is  separated  and  detected  by  mass  spectrometers?          2. Below  is  a  generalized  schematic  of  the  components  of  a  mass  spectrometer.      

 Circle  and  label  each  of  the  above  phases  in  the  figure  below.  

                                             

Ionization  Methods  3. Define  the  following  terms:  Base  peak      Molecular  ion    

ionization   ion  acceleration  

selection  of  ions   detection  

Page 2: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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 There  are  several  (many)  ways  to  generate  ions  that  can  be  detected  for  mass  spectrometry.    These  methods  vary  in  aggressiveness  and  effectiveness.      4. The  GC-­‐MS  available  in  the  department  (and  used  in  the  CHEM  212  lab)  uses  electron  

ionization  (aka  electron  impact)  to  ionize  molecules  after  separation  by  gas  chromatography  and  prior  to  detection.      

a. Write  the  reaction  of  a  molecule  with  an  electron  to  form  the  molecular  ion.          

b. What  is  a  typical  ionization  energy  for  a  valence  electron?  If  the  electron  gives  up  12-­‐15eV  of  kinetic  energy  in  colliding  with  the  molecule,  is  that  enough  to  result  in  loss  of  a  valance  electron?    

   

     

c. Diagram  an  electron  ionization  setup.    Describe  the  function  of  each  component.  

                           5. Diagram  a  chemical  ionization  setup.    Describe  the  function  of  each  component.                        

Page 3: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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6. Rank  the  typical  reagent  gasses  in  order  from  most  to  least  aggressive  at  ionization.          7. Explain  why  the  following  MS  spectra  of  the  SAME  COMPOUND  have  different  peaks  

and  different  peak  abundances  

               8. You  collect  a  mass  spectrum  of  a  known  compound  using  electron  ionization  but  do  not  

observe  a  M+ peak.    What’s  likely  happened?    Suggest  two  methods  of  increasing  the  detected  M+ ion  abundance?  

       9. Is  chemical  or  electron  ionization  the  more  aggressive  method?    What  does  it  mean  if  an  

ionization  method  is  more  aggressive?        

     10. When  would  a  more  aggressive  method  be  best?              11. When  would  a  less  aggressive  method  be  best?      

Page 4: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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Mass  Spectrometer-­‐  Selection  of  Ions  12. Diagram  a  magnetic  sector  mass  spectrometer  and  

describe  how  it  selects  a  specific  m/z  ratio  ion  to  impact  the  detector  

                                               13. Diagram  and  describe  how  a  

quadrupole  mass  spectrometer  works.                                  

Page 5: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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14. Diagram  and  describe  how  a  TOF  works.                                        Mass  Spectrometer-­‐  Detecting  Ions  15. Diagram  an  electron  multiplier.    What  is  the  typical  amplification?                      16. What  is  a  conversion  dynode  and  when  is  it  needed?              17. Diagram  and  describe  how  a  Channeltron  converts  ions  into  a  

measureable  current.            

Page 6: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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http://www.chem.arizona.edu/massspec/  

   

Page 7: Mass Spectrometry Worksheet - CHEM 212: Analytical · PDF fileMassSpectrometry$Worksheet$ CHEM212$! 1. What!is!separated!and!detected!by!mass!spectrometers?! $ $ $ $ 2. ... Mass Spectrometry

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Creative  Project  lite-­‐  be  prepared  to  present  your  application  and  technique  in  class.  18. Find  an  application  of  mass  spectrometry  you  are  interested  in.    Describe  the  problem  

and  how  mass  spectrometry  is  used  to  address  it.                                      Learn  about  the  mass  spectrometer  used  in  this  application  and  diagram  it  below.    Be  sure  to  include  information  about  the  methods  for  ionization  and  separation  of  ions.