Copyright Resonance Ltd., December 2011
143 Ferndale Drive North, Barrie, ON L4N 9V9 Tel: 705-733-3633 Fax: 705-733-1388 Email:sales@resonance.on.ca
TR-SES-200 High Resolution VUV/UV
Transmission and Reflection Evaluation System
Manual Page 2
Manually Obtaining a Reference Spectrum
1. Make sure that all doors to the chamber are closed and that there are no sources of light leakage into the chamber.
2. Go to the “Spectrometer” tab and set the wavelength to 230nm.
3. Place the PMT at zero degrees (directly opposite the collimating assembly)
4. Set the PMT gain to a reasonable level (~2V). At thi point a signal should be detected.
5. Rotate through 360 degrees on sample wheel to identify the locations of the open sector.
6. Scan to middle of the plateau of a vacant location. Record this angle for future use.
7. Return to the PMT Rotation tab and scan across the peak from -10 to +10
8. Scan up to the middle of the peak to optimize the signal.
9. Perform a scan across the wavelength range to be used in the tes sequence and save as you reference.
Subroutines
PMT Signal Optimization for Maximum Signal
1. Go to the “Spectrometer” tab and set the wavelength to 230nm.
2. Go to the “Sample Rotation” tab and set the sample wheel to a vavant spot for the reference measurement, or to the
desired sample location.
3. Scan the PMT from -10 to +10 degrees from the expected angle at a maximum of 0.1 degree increments.
Figure 21: Manual scan for PMT alignment
4. Take note of the angle where the center of the peak is located.
5. Do another scan with the same step increment, this time ending at the peak of the curve.
Figure 22: Optimizing the PMT Signal for maximum signal
Sample Rotation Optimization
1. Go to the “Spectrometer” tab and set the wavelength to 230nm.
2. Go to the “Sample Angle” tab and set the desired angle to 45 degrees.
3. Go to the “PMT Rotation” tab and perform the “PMT Signal Optimization” subroutine at zero degrees.
4. Go to the “Sample Rotation” tab and scan across the full 360 degrees at an increment of 0.5 degrees.
5. Take note of the locations of the centers of any signal plateaus.
6. Starting just before the first plateau, scan at 0.1 degree increments to the recorded center of the plateau.
7. Record this as the optimized of the vacant slots for future use.
8. Return to the PMT Rotation tab and perofrm the PMT Signal Optimization subroutine at 90 degrees.
9. Repeat steps 4-7 recording them as the center of the samples for future use.
Sample Tilt Optimization for Maximum Signal
1. Go to the “Spectrometer” tab and set the wavelength to 230nm.
2. Go to the “Sample Rotation” tab and set the sample wheel to the desired sample location.
3. Set the PMT to the desired angle.
4. Scan the Sample Tilt from -10 to +10 degrees from the expected angle at a maximum of 0.1 degree increments.
Figure 23: Manual scan for PMT alignment
5. Take not of the angle where the center of the peak is located.
6. Do another scan with the same step increment, this time ending at the peak of the curve.
Obtaining an Optimized Referenece Spectrum without Automated Scanning
1. Perform “PMT Signal Optimization” subroutince.
2. Perform “Sample Rotation Optimization” subroutine.
Calibration
Calibrating the PMT Stage
1. Go to the “Spectrometer tab and set the wavelength to 230nm.
2. Go to the “Sample Rotation” tab and set the sample wheel to a vacant spot (such as a reference sample location).
3. Scan the PMT from -10 to +10 degrees at a maximum of 0.1 dgree increments.
4. Take note of the angle where the center of the peak is located.
5. Go into the “Settings” tab and in the section labelled “Conversions”, select “PMT Rot” in the drop-down box.
6. In the Angle textbox, type in the recorded peak angle from Step 4 and press the “Convert” button at the bottom of the
section.
7. Copy the calculated Step Position in the grey box over to the “PMT Rotation Offset” textbox in the “PMT Rotation
Constants” section.
8. Press the “Save Settings” button near the bottom of the screen. The green indicator light should turn on if the file has
been properly saved.
Calibrating the Sample Rotation
1. Go to the “Spectrometer” tab and set the wavelength to 230nm.
2. Scan from across the diameter of the desired sample location at a maximum increment of 0.1 degrees.
3. Take note of the angle where the center of the plateau is located.
4. Go into the “Settings” tab and in the section labelled “Conversions”, select “Sample Rot” in the drop-down box.
5. In the Angle textbox, type in the recorded peak angle from Step 3 and press the “Convert” button at the bottom of the
section.
6. Copy the calculated Step Position in the grey box over to the “Sample Rotation Offset” textbox in the “Sample Rotation
Constants” section.
7. Click the “Save Settings” button near the bottom of the screen. The green indicator light should turn on if the file has been
properly saved.
Calibrating the Sample Tilt
1. Place a UV reflective mirror on the sample wheel and note its location.
2. Go to the “Sample Rotation” tab and set it so that the mirror is in the beam path.
3. Go to the “Spectrometer” tab and set the wavelength to 230nm.
4. Go to the “PMT Rotation” tab and set the angle to 45 degrees.
5. Scan the angle tilt from 80-100 at a maximum of 0.1 degree increments.
6. Take note of the angle where the center of the peak is located.
7. Go into the “Settings” tab and in the section labelled “Conversions”, select “Sample Tilt” in the drop-down box.’’
8. In the Angle textbox, type in the recorded peak angle from Step 3 and click the “Convert” button at the bottom of the
section and record the calculated step position.
9. Repeat steps 2-6 on the negative side (PMT at -45 and Angle tilt scan from -80 to -100 degrees).
10. Calculate the average of the two recorded step positions. This is the location of ther zero angle (sample wheel
perpendicular to the beam path).
11. Insert the calculated zero angle into the “Sample Tilt Offset” textbox in the “Sample Tilt Constants” section.
12. Click the “Save Settings” button near the bottom of the screen. The green indicator light should turn on if the file has
been properly saved.
Calibrating the Spectrometer
To properly calibrate the spectrometer, at least 3 well defined spectral peaks are required. Hydrogen has well known lines at
121.4nm. For the second and third line, the second and third order diffraction of the 121.4nm line, at 242.8nm and 363.2nm
lines will work.
1. Set the PMT to zero degrees.
2. Set the sample wheel to vacant spot (such as a reference location).
3. Turn on the hydrogen lamp and allow 20 minutes to warm up.
4. Pump down the system to the 10-3 mbar range.
5. Perform a full range scan, from 100 to 400nm.
6. Identify the three peaks of interest and take note of their diplayed wavelength position.
7. Go to the settings tab and in the “Conversions” section, determine their corresponding step positions.
8. In the “Spectrometer Wavelength Calibration” section, insert what the actual wavelength for the peaks should ben in the
“λ1’, ‘λ2’ and ‘λ3” textboxes, and the calculated step positions in the corresponding textboxes.
9. Click the “Calculate” button to obtain a new set of constants.
10. Once satisfied with the constants, click on the “Apply” button.
11. Click the “Save Settings” button near the bottom of the screen. The green indicator light should turn on if the file has
been properly saved.
Transmission/Reflection Vs. Wavelength using Automated Scanning
1. Ensure all the stages are properly calibrated.
2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples.
3. Go to the “Setup” tab.
4. Ensure all the stages have been zeroed.
5. In the “Automated Scanning” box, select the sample wheel that is being used.
6. Click on the box next to the Sample# for all the samples to be measured.
7. Set the “Sample Tilt Angle” for the reference and the samples.
8. Set the “PMT Angle” for the reference and the samples to be measured.
9. Set the “Sample Roatation Angle” to identify the location of the reference and samples.
10. In the “Spectrometer Settings” box, set the scan parameters for the measurements; Start and end Wavelength; Wavelength
step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages)
and the slit width (for reference only, does not actually set the slit width).
11. Set the PMT Gain to an acceptable level (2.0 is adequate for the majority of situations).
12. In the “Signal Selector” box, set the input type (PMT Input for standard transmission and reflection measurements, Aux Input
for diode sensitivity measurements) and the gain (note: the +/- value indicates the signal limits with that particular gain
setting).
13. When all parameters are set, click the “Save Parameters” button.
14. Click the “Measure” button to start the scans. The system will go through the scans in the following order:
- Reference - Sample 1 - Reference - Reference - Sample 2 - Reference ...
Depending on the settings, this could take from 5 minutes to over an hour.
15. Once the scans are complete for each sample the calculated transmission/reflection graph will be displayed (shown as
Measure 1, 2 etc. with the scan plots on the right pane along with reference and sample scans).
16. To save, right click the view window and select a desired File Save Path and File Name. You have the option to save all
scanned plots or only the current viewed plots. Ensure you select the appropriate option before clearing data or exiting the
program. Click “Save” and your data will be saved to you selected save path.
Transmission/Reflection Vs. Wavelength using Automated Scanning
1. Ensure all the stages properly calibrated.
2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples.
3. Set the Sample Rotation to the vacant spot for the referenece scan.
4. Set the sample tilt to the desired angle.
5. Perform the PMT Optimization subroutine.
6. Go to the “Spectrometer” tab and set the scan parameters for the measurement: Start and end Wavelength; Wavelength step
increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages); and
the PMT gain.
7. Select the type of scan to be performed: Constant Rate of Fastest Speed. Fastest speed will go through the scan as quickly
as it can under the set parameters, however the time interval between steps may be inconsistent due to software
hand-shaking. Constant rate introduces a delay between steps so that the time interval between steps is consistent through-
out the scan.
8. When all parameters are set, click the “Start Scan” button.
9. When the scan is complete, record the Scan # for future calculation.
10. Repeat steps 3-9 for each sample to be measured. It is also remcommended to take additional reference scans either after
each sample or , at the least, after completing all the sample scans to compensate for any potential lamp drift.
11. When ready, set the scan # for the sample transmission/reflection you want to measure as Plot 2 and set two reference
scans (either the ones taken at the start and end of the scan sequence or the ones taken immediately before and after the
scan for desired sample) as plots 3 and 4.
12. Setup the function setting to calculate the transmission/reflection of the sample using the average of the two reference scans
selected.
13. When you’re satisfied with the formula setup, click on the “Calculate Result” button. The displayed graph will automatically
change to the calculated transmission/reflection curve.
14. If the curve is very noisy, you can take average of multiple data points by setting the number of data points to be used in the
text box to the right of the “Calculate Result” button and pressing the “Apply Running Averate” button above it.
15. Set the File Name and the File Save path.
16. In the drop box beside the “Save” button select “Result” then click the Save button. This will save the transmission data as
well as all the spectral data used in the calculation. The green indicator light will turn on to indicate that the file has been
saved successfully.
17. If external manifpulation of the data is desired, set Post 1, 2, 3 and 4 to the desired scan #’s and repeat the save process but
setting the Save drop box to the Plot number. This will save each scan in its own individual file.
