1 Open Access Open Access Agilent Agilent LC/MSD VL LC/MSD VL January 2009 CIC, MS Chemical Instrumentation Center Chemical Instrumentation Center - Mass Spectrometry Mass Spectrometry Instrumentation and Software Instrumentation Agilent LC 1100 Series LC/MSD VL with ESI source Software ChemStation A.10.02 EasyAccess A.02.01
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Open Access Agilent LC/MSD VL - Boston University LCMS...1 Open Access Agilent LC/MSD VL January 2009 CIC, MS Chemical Instrumentation Center -Mass Spectrometry Instrumentation and
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Open AccessOpen Access
AgilentAgilent LC/MSD VLLC/MSD VL
January 2009
CIC, MS
Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Instrumentation and Software
Instrumentation
� Agilent LC 1100 Series
� LC/MSD VL with ESI source
Software
� ChemStation A.10.02
� EasyAccess A.02.01
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Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Open Access
� Walk-up MS instrument to users 24/7
� ESI source – suitable for polar, acidic and basic molecules < 1500
m/z
� Low resolution only (1 decimal place)
� Pre-developed methods (8 and growing)
� All users are trained
� Specific methods can be developed and added
Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Method Types
�Flow injection analysis
� Running through LC without a
column
� Not much to tell on purity
� Confirmation of molecular ion
� Fast, run-time ~ 5 mins
� Running through LC with a
reverse phase column (C18,
2.1x50mm)
� Separation of components
� Additional info from UV data
� Run time ~ 15 mins
FIALCMS
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Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Open Access Methods (Positive)
0 Fragmentor100-1500100.01NoFIA_P_ACN_0Frag
30 Fragmentor100-1500100.01NoFIA_P_ACN_30Frag
120 C100-1500100.01NoFIA_P_ACN_LowT
100-1500100.01YesLCMS_P
ACN only100-1500100.005NoFIA_P_ACN
100-1500100.005NoFIA_P_HM
100-1000100.005NoFIA_P_MM
50-500100.005NoFIA_P_LM
NotesMass Range
(m/z)
Injection
Vol, (uL)
[ Conc ]
(mg/mL)
C18
ColumnMethod
Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Open Access Methods (Negative)
0 Fragmentor100-1500100.05NoFIA_N_ACN_0Frag
30 Fragmentor100-1500100.05NoFIA_N_ACN_30Frag
120 C100-1500100.05NoFIA_N_ACN_LowT
100-1500100.01YesLCMS_N
ACN only100-1500100.01NoFIA_N_ACN
100-1500100.01NoFIA_N_HM
100-1000100.01NoFIA_N_MM
50-500100.01NoFIA_N_LM
NotesMass Range
(m/z)
Injection
Vol, (uL)
[ Conc ]
(mg/mL)
C18
ColumnMethod
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Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Open Access Policy
� All users must be trained before operating this instrument.
� Suitable solvents are Methanol, Methylene Chloride, Acetonitrile or Water.
� Concentration is sample dependent, but please start at 0.005 mg/mL
(5 ppm) for FIA and 0.01 mg/mL (10 ppm) for LC/MS.
� Overloading the instrument will result in a warning and the user will also
be charged with a source-cleaning fee.
� Use 2 mL vials (insert is also approved). Fill up to at least 1/2 height.
� You do not have to, but to avoid possible carryover from previous sample,
run a blank (pure solvent). There is no charge on the blank run.
� Fail to follow these guidelines will result in removal of your permission to
operate this instrument.
� Manual direct injection users, please consult with Norman for
concentration. The highest concentration allowed is 0.5 mg/mL. Please
flush for 10 minutes after use.
Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Good Practice
� Before login, please check the standard spectrum to make sure the instrument is in good condition. CIC staff will perform maintenance weekly.
� You do not have to, but to avoid possible carryover from previous sample, run a blank (such as methanol). There is no charge on blank run.
� Don’t overload the machine with too concentrated sample, an ion counts between 104-105 are ideal.
� If there is a problem, please notify us ASAP so we can help.
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Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry
Data Analysis
M + 45 (Formic Acid)
M + 35 (Cl)
M + 18 (NH4)
M + 23 (Na)
M + 39 (K)
M + 41 (Acetonitrile)
ESI NegativeESI Positive
Adduct Ions
� Open Access is set up to process and print a report automatically.
� The automatic data processing is specific to the type of analysis carried out. For FIA, major peaks are reported. For LCMS, report is optimized for the most intense peaks.
� Isotope Pattern - determine a valid ion, spike or saturated signal.
� Halogen Patterns - visualize chlorine and bromine isotopes.
Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry