IonSense DART Ion Source 100-CE User manual

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DART Ion Source
Operation Manual
For DART CE Units
Version 20070912
Real-time science solution
s
IonSense Inc.
999 Broadway
Suite 404
Saugus, MA 01906
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DART Operation Manual
DART Operation Manual ii
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Copyright © 2005-2007 by
IonSense Inc.
All rights reserved.
The information in this document has been carefully checked and believed to be reliable.
However no responsibility is assumed for inaccuracies. Statements in the document are
not intended to create any warranty, expressed on implied. Specification and performance
characteristics of the hardware and software described in the manual may be changed at
any time without notice. IonSense Inc. reserves the right to make changes in any product
herein in order to improve reliability, design or function. IonSense Inc. does not assume
any liability arising out of application or use of any product or circuit described nor does
it convey any license under its patent rights or the rights of others.
The apparatus and application of the apparatus described in this document is protected by
US Patent Number 6,949,741 and used under license; additional patents pending.
All trademarks are property of their respective owners.
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DART Operation Manual
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DART Operation Manual
Here we will discuss the operational steps involved in a typical data acquisition run.
Installation
Hardware
Be sure the DART Source and Controller are properly installed; reference the DART
Hardware Installation manual for more details.
Software
Install the DART software on your PC if you haven’t done so already. See DART
Software Manual for installation instructions. Install the software included with your
mass spectrometer, and ready it for data acquisition.
Using DARTControl
Launch
Double click the icon on the desktop to launch the DARTControl software. If any errors
or warnings appear after launching the program then refer to the DART Software Manual
for more information.
Once the software is up and running, click the OFF/ON button on the Status Bar to turn
the software ON. Now you can either be in Standby Mode or Run Mode; the software
always defaults to Standby when first turning it ON.
Set Parameters
Gas, flow rate, and heater temperatures can be set in Standby Mode. All voltages are
controlled in Run Mode
Gas Selection
oN2 (Nitrogen) is set as the default gas in Standby Mode. N2 is
generally less sensitive as an ionization gas. It’s usually just used as a
‘flushing’ gas: keeping heat from cartridge moving, and preventing
oxidation within cartridge.
It’s also the more economic choice, since more time is
generally spent in Standby preparing an experiment vs. actually
running one.
oHelium is set as the default gas in Run Mode. Helium tends to ionize
most sample compounds better than N2 due to the metastable energy
level
NOTE: Helium may not always produce the best ionization sensitivity.
The choice of gas can be highly sample and matrix dependent.
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DART Operation Manual
DART Operation Manual 2
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oFlow Rate
Standby Mode
•Somewhere between 15-25% of the maximum flow rate
should be sufficient in Standby Mode. The default should
be set to approximately 25%
Run Mode
•Once again, this setting is application specific. Around
50% of the maximum flow rate should be a good place to
start.
•The idea is to find a balance of highest sensitivity vs.
lowest flow rate
These parameters can be adjusted in the DART Setup menu, from
Setup on the main bar.
•They can also be adjusted by simply changing the
parameters while in Standby/Run Modes. The software
will remember these settings next time you switch back and
forth.
oHeater Temperature
NOTE: Never heat the DART without gas flowing and always
allow DART to cool to at least 200ºC before turning off gas flow.
Heating without gas flow could cause serious damage to DART.
Type in your desired temperature into the ‘Set’ temperature box.
•Be sure the heater is turned On, by pushing the On/Off
button next to the Set box.
•The actual temperature will be displayed in the ‘Temp’ box
directly above
Generally, more volatile compounds can be ionized at lower
temperatures, while less volatile compounds require higher
temperatures. However, higher temperatures could cause more
fragmentation of your molecule.
It is likely that some experimentation will need to be done to
determine the best temperature for the compound you are
attempting to analyze. Between 200°C and 250ºC is usually a
good place to start.
Set temperature will not change when switching in and out of
Standby Mode unless specifically set to do so
oVoltages: Needle and Electrodes
NOTE: Never turn on the Needle voltage to the DART without
inert gas flow. Applying the Needle voltage without inert (helium
or nitrogen) gas flow could cause serious damage to DART and
produce unwanted ionization products.
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DART Operation Manual
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DART Operation Manual
Up until this point the software has been in Standby Mode. To
adjust voltages you must click the Standby/Run button in the
Status Bar to activate Run Mode.
•The needle and electrodes will automatically be energized
upon turning on Run Mode with default settings
Needle
•For positive ion analysis a voltage between 3000 and 4000
Volts generally works best. A lower voltage seems to work
well for negative ion, between 2000 and 3000 Volts.
Electrodes: Grid and Discharge
•In either positive or negative ion mode, voltages between
150 and 250 Volts generally work well
Keep in mind that these voltages may not necessarily be the best
for your specific compound, and experimentation is always
recommended.
Set voltage values will not change when switching in and out of
Standby Mode.
oSave Settings: Methods
You can save your settings to a ‘Method’, and load them again for
later use.
•See DART Software Manual for more detail regarding
Methods
-Data Acquisition
oOnce all the parameters have been set you are ready to acquire data
oStandby Mode:
While in Standby prepare your sample for introduction to the
DART gas beam, and your mass spectrometer software for an
acquisition
oRun Mode:
Turn on Run Mode and present samples to DART for ionization
oOnce you are finished ionizing your samples set the DART back to
Standby to prepare for another run, or to shut down for later use.
-Troubleshooting
oNozzle Cap Contamination
The exit nozzle of the DART can become accidentally
contaminated by touching a sample to the hot surface on the tip.
The nozzle cap is ceramic and it can be removed for cleaning. The
ceramic is fragile and care must be used when handling it. Due to
potential contamination and background from fingerprints, it is
recommended that gloves be worn when applying a clean cap.
Firstly turn off the DART source and let it cool. The cap can be
unscrewed from the nozzle and either cleaned using solvent, high
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DART Operation Manual
DART Operation Manual 4
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temperature baking, or replaced with a spare clean cap. Proper
safety procedures must be followed when using a solvent or
operating a high temperature oven. It is not recommended the cap
be baked above 1000°C.
oLow Sensitivity
Insufficient gas temperature.
•The temperature readout in the DART software is from a
thermocouple embedded in the ceramic heater, not in the
gas stream. Therefore the actual gas temperature will be
lower than this readout and is a function of the heater core
temperature, gas flow rate and heat capacity of the gas. The
heater core temperature can be adjusted through the
software within defined limits and optimized for the
application measurement.
Grid Electrode contamination.
•The grid electrode at the tip of the DART nozzle can
become contaminated with use. If the grid becomes
contaminated the sensitivity of the DART will decrease,
particularly in negative ionization mode. If so, the grid
should be replaced.
•This replacement can be easily performed by any user.
Contact IonSense regarding a document detailing the
procedure if you wish to replace the grid.
Mass Spec Inlet orifice blockage.
•Due to the wide variety of samples that can be analyzed
and the open nature of the atmospheric pressure inlet to the
mass spectrometer, it is possible for contamination to build
up on the inlet. This contamination can cause a partial or
complete blockage and loss of sensitivity of the mass
spectrometer. If you suspect this has happened, turn off the
DART, let it cool and remove the DART from the mass
spectrometer to gain access to the inlet orifice. Follow the
manufacturer’s instructions for cleaning the atmospheric
inlet orifice and reattach the DART.
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