Department of Chemistry, Tufts University
Leeman Labs PS-1000 ICP Brief Directions (Windows Software)
There are three main Windows in the WinICP application. Runner is the window that controls the operation of the
spectrometer. Database is where results and method parameters reside. Rack Editor coordinates the sample,
location, and sequence information when using the autosampler. Changes made to protocol and dataset in one
window are not automatically changed in the others! Use
and
buttons to communicate changes
made in one window to the other. A small window near the top of the Runner window will indicate BUSY (in red)
when the spectrometer is carrying out a command, IDLE otherwise. You can print the Runner or Database window
by selecting the printer icon near the upper left corner (for best results, set dithering to Fine in Printer properties)
Turn on Procedure
Turn on Argon. Pressure should be ~80 psi.
Turn on water circulator (cools down the coil).
Turn on vent switch (near adjacent door).
Turn on the instrument (Black/Red switch on left end, AND green button near torch). There should be no
red lights on the instrument panel.
Turn on computer.
Turn the printer on and monitor.
Select the WinICP icon to start the ICP Runner software. If “hardware Inoperable” error appears, exit
program, power down instrument, power up, then restart program.
Select the DB button from the toolbar to start the Database software
Put sample and drain lines in slots and pull so tubing is taut.
Lock lines in place. Push knob down. Don't turn the knobs.
Select Method and Dataset
Select Protocol from drop down menu, or create new protocol as described below.
Select existing Dataset from dropdown menu, or select File/New Dataset from main menu. If this
window remains blank, no data will be saved to disk!
Creating a new protocol
Protocols are created and edited from the Database Window. Select File/New Protocol from menu.
Enter name and title.
Protocol tab
The default Plasma, Pump, and data parameters should work in most cases. Modify them if
desired. Choose a Radial Position line (usually Mn 257.610). Select Apply
Line Select tab
Select element, then select line, usually the one labeled best. Select Insert button. Always
include Mn (257.61) for peaking. Note that elements can be displayed in periodic or alphabetic
order.
Line Info tab
If standards for all elements have the same concentrations, select Set all Lines. If elements have
different concentrations, select a line, then Set Selected. Enter concentration for standards and
check samples. Default integration times are 1 sec. Low concentration of weak lines may require
longer integration times. For Mn, select Position box, then Apply to one line button.
Saving Protocol
Changes are saves automatically. Select Utility/Protect Protocol to make the protocol read
only.
Starting the plasma
Runner window, Control tab
Revised 06/02/06
D. Wilbur
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Department of Chemistry, Tufts University
Select Cold Autostart button. Gas will flow for 60sec before plasma ignites. Watch countdown
in action window. If you can’t hear the gas flowing, exit software, turn power off, then on, then
restart software.
If there is trouble with the plasma (orange plasma) hit the red button on the instrument panel.
This will shut down the plasma.
Always have something aspirating in the plasma. Use DI water when not running samples or acid rinse.
Optimize Optics
The spectrometer and its optics are subject to expansion and contraction with temperature changes.
Runner window, Main tab
Check that real time printing is enabled.
Runner window, Scan tab
Select the Peak Optics button. A Peak Optics window will appear. Select Quick
Hg lamp will be used. After 30 sec lamp warm-up scans will appear. When it is finished scanning
the instrument will go into Idle State. The Peak Optics procedure will repeat automatically about
every 20 minutes.
Optimize plasma position
This procedure makes sure the detector is looking at the most intense portion of the plasma. The display
will be a histogram of intensities across the width and height of the plasma. Ideally, the center of the scan is
broad, symmetrical and flat, so that small shifts from the center will not change the intensity significantly.
Put the sample line in the position line solution (usually 10ppm Mn)
Runner window, Scan tab
Select the Position Plasma button. A Position Plasma window will appear.
Select Run Manual.
When finished, select Accept
The peak should be gaussian with intensity about 60,000 for 10ppm Mn (>40,000 ok). If the cursor is not in
the center of the peak, repeat the procedure. When run is done, put the sample back in the rinse.
Optimize power and flow (not usually needed for established protocols)
If desired, the gas flow and power settings can be adjusted to maximize the Mn intensity.
Runner window, Control tab
Select Chart Recorder. Chart Recorder window will appear
Select Mn line
Select Run. Adjust flow parameters for maximum intensity, minimum RSD.
Select Stop. Close chart recorder window
Standard Settings
Power
1.0 kW
Coolant
13 LPM
Nebulizer
43 psi
Aux.
0.3 LPM
Peaking (Peak Wavelength)
Wavelength peaking ensures that the spectrometer is looking at the most intense portion of the emission
line for each element analyzed. You will need a solution (or several solutions) containing all elements to
be analyzed. The solutions labeled Peak 1 and Peak 2 contain most element of interest for environmental
analysis. Additional solutions will be needed for additional elements.
Revised 06/02/06
D. Wilbur
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Department of Chemistry, Tufts University
Runner window, Sample tab
Select the metals that are in the solution
Put the sample line into the solution
Runner window, Scan tab
Select Scan
A scan of each line will appear in the Monitor window. Scans can be reviewed in the Playback
window. Lines are scanned in order of increasing wavelength.
Runner window, Profiles tab
Provides an alternate view to view all scans at once.
Intensities will vary widely for different elements, but sampling position, indicated by vertical line in Scan
tab, must be at peak maximum. When done the computer goes into IDLE mode. If any elements of interest
are not at peak, then do the next step.
Runner window, Sample tab
Select lines that are not at maximum
Select quick in the Align wavelengths area if the line is near maximum, full if far from maximum
(or no peak is seen)
Select Manual. An Align Wavelengths window will appear. You can watch the progress in
the Scan or Profile tabs.
When finished select Accept All Lines
After the scan put sample line back into DI water or Dilute nitric rinse for 60 secs
Calibration with standard samples
Database Window, Line info tab
Check that only elements present in standard are turned on, and that calibration and check
standards are correct.
To change concentration, select a line, then Set Selected. Enter concentrations for standards
and check samples.
Runner Window, Standard tab
Select New Cal Reset button
Insert tip in standard
Select desired standard button, S1, S2 …
Select desired replicates
Select Stnd Manual button
Repeat for remaining standards
Database Window, Cal Curve tab
Select each line
View the curve, select Accept this line or Accept ALL lines button
You can print the calibration plot by selecting the printer icon near the upper left corner
Run Check Standard (optional)
Runner Window, Standard tab
Insert tip in check standard
Select desired standard button, C1, C2 …
Select ChkStd Manual button
Results can be seen in Viewer tab
Repeat for remaining standards
Run Unknown Sample
Runner Window, Sample tab
Insert tip in unknown sample
Verify that desired lines are checked
Enter sample ID information
Revised 06/02/06
D. Wilbur
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Department of Chemistry, Tufts University
Select Run Manual
Results can be seen in Viewer tab
Repeat for additional samples. Make sure that after every sample the sample line is placed in 10% nitric
for 1 min.
Printing Report
There are three ways to print data.
1. You can print ANY Runner or Database window by selecting the printer icon near the upper left corner
(for best results, set dithering to Fine in Printer properties). Print quality is not very good. For better print
quality, copy to clipboard (ALT-PrintScreen), then paste to MS Word.
2. The Report Tab in the Runner window will record each measurement as it is taken. If real time
printing is enabled on the Main tab, the report can be printed using File/Page Eject from the menu.
3. Database Window, Report tab
In the Runner window select DB button to transfer all data to Database window.
Select batches and records to print with All/None boxes, or by checking individual records in the
In column.
Select Edit to edit report spec. Check or uncheck boxes to determine what information appears in
report. Select OK when finished.
Database Window, Viewer tab. Select Clear to clear existing report
Database Window, Report tab. Select Generate Report. Generate report window appears.
Select format (report for printer, PRN file or WKS file for text or spreadsheet files on
disk)
Select Destination (usually viewer only or printer).
Select Generate.
Shut down Procedure
Runner window, Control tab
Put sample line in DI water
Select Extinguish after Rinse button
The macro will rinse with DI water for 10 min., then shutoff plasma.
Press Red Button on the Instrument Panel
Turn off Argon at tank and turn water cooler off
Release pump pressure locks
Shut down computer and turn off monitor
Turn the vent off
Appendix: Data File structure
*.PRO Named protocols in C:\ICP\Protocol
*.DAT Datasets in C:\ICP\Data
*.REP Report Specs in C:\ICP\RptSpec
Revised 06/02/06
D. Wilbur
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