calibration of the photodiode - horiba of the fluorolog-3 photodiode, v. 1.1 (23 sep 2004) 1...

Calibration of the Fluorolog-3 Photodiode, v. 1.1 (23 Sep 2004)

Photodiode-Calibration Kit

Operation Manual http://www.jobinyvon.com

USA: HORIBA Jobin Yvon Inc., 3880 Park Avenue, Edison, NJ 08820-3012, Toll-Free: +1-866-jobinyvon

Tel: +1-732-494-8660, Fax: +1-732-549-5125, E-mail: [email protected], www.jobinyvon.com

France: HORIBA Jobin Yvon S.A.S., 16-18, rue du Canal, 91165 Longjumeau Cedex, Tel: +33 (0) 1 64 54 13 00, Fax: +33 (0) 1 69 09 93 19, www.jobinyvon.fr Japan: HORIBA Ltd., JY Optical Sales Dept, Higashi-Kanda, Daiji Building, 1-7-8 Higashi-Kanda Chiyoda-ku, Tokyo 101-0031, Tel: +81 (0) 3 3861 8231, www.jyhoriba.jp Germany: +49 (0) 89 462317-0 Italy: +39 0 2 57603050 UK: +44 (0) 20 8204 8142 China: +86 (0) 10 6849 2216 (All HORIBA Jobin Yvon companies were formerly known as Jobin Yvon)


Copyright © 2004 by Jobin Yvon Inc. All rights reserved. No part of this work may be reproduced, stored, in a re-trieval system, or transmitted in any form by any means, including electronic or mechanical, photocopying and recording, without prior written permission from Jobin Yvon Inc. Requests for permission should be requested in writing. Information in this manual is subject to change without notice, and does not rep-resent a commitment on the part of the vendor. February 2004

Part Number


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Calibration of the Fluorolog®-3 Photodiode

Introduction Jobin Yvon suggests that users who require extended excitation-correction above 600 nm employ a calibrated photodiode. Less advisable methods involve other quantum-counting methods, such as with the laser-dye HITC, which are not highly reproducible, and are valid over a relatively narrow range of wavelengths. The calibration procedure uses a photodiode specially mounted to sit at the position of the sample in the sample chamber, and is scanned with the same parameters as the ref-erence detector. The photodiode is connected to the extra signal channel A. Both pho-todiode and reference detector are scanned simultaneously, using only the excitation monochromator. After scanning, the data and dark offsets are entered into a special program, Cali-brate Photodiode.exe, that calculates the spectral responsivity. Two files are created: PowCorr.spc Helps determine the power in µW at the sample. Xcorr.spc Determines quantum corrections for the excitation spectrum. Essen-

tially, Xcorr.spc corrects for the number of photons arriving at the sample. Xcorr.spc = wavelength × PowCorr.spc


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Parts required for calibration Photodiode assembly DM303-P module (including

cables) Extra, blank, format-ted 3½" floppy disk


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Procedure 1 Turn on system. 2 Warm up xenon lamp for 30 min. 3 Turn off SpectrAcq. 4 Remove the boot disk from the SpectrAcq. 5 Back up the SpectrAcq boot disk.

a Right-click on disk A:.

b Copy disk A: to a back-up disk.

c In the back-up disk A:, open hardware.ini in a text processor such as Wordpad.


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6 Modify the copied boot disk to use signal chan-nel A. a Near the end of hardware.ini, change the line x ; input module 3 (i.e., whatever the initial integer x is.

Here x = 2) to 1 ; input module 3 (i.e., change the initial integer to 1)

b Save hardware.ini.


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7 Connect the DM303 module to channel A on the back of the SpectrAcq.

8 Boot up SpectrAcq using the new, modified boot disk.

9 Put the photodiode assembly in the sample compart-ment.

10 Place the lid on the sample compartment.

11 Connect the BNC ca-ble.

12 Place calibrated-photodiode isa files in the host PC. a Open A: drive.

b Open the isa_ini folder.

Connect to “INPUT A”.


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Note: Your Visual Instrument Setup may be different, depending on options and accessories.

c Select and copy all files into C:\datamax\isa_ini

d Paste the files.

e If ACQ4.ini already exists, do not override it. Instead, temporarily rename ACQ4.ini as ACQ44.ini. If ACQ4_HV4.ini already ex-ists, rename it to ACQ_HV44.ini.

f Copy ACQ4.ini into C:.

13 Open DataMax. The Layout Selection window appears.

14 Choose the PhotoDiode Calibrate lay-out.

15 Click OK. The Layout Selection window closes.

16 When the sample-selector ERROR window appears, click OK, then Disable for the next win-dow.

17 Choose the correct units for the photodiode calibration. a Open Visual

Instrument Setup.

The Visual Instrument Setup appears.


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b Click on a photodiode symbol.

The Acquisition Channel window opens.

c Set the Data Units field to Microam-peres.

d Set the Gain Level to Auto.

e Click Apply.

f Click OK. The Acquisition Channel window closes.

g Repeat steps b through f for the other photodiode symbol.

18 Close Visual Instrument Setup. 19 Run a lamp spectrum.

a Find experiment file lamp.exp on the A: drive.

b Run from 240–1000 nm.

20 Check the calibration of the peak.


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Be sure the peak is at 467 nm.

21 Pick the most intense peak of the plot, and move the excitation monochromator to that peak.

22 Using the Real Time Display, monitor the signal from the channel A. The signal should be 5–10 µA; closer to 10 µA is better. If the signal is not in this range, close or open the excitation-monochromator slits.


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23 In the acquisition window, select calib.exp in the A: (3½" floppy) drive.

24 Note the slit settings. Here the excitation monochromator’s slit is 7 nm bandpass.

25 Do another lamp scan, using the calib.exp file, with slits at the above widths. This creates a lamp scan of channels A and R simultaneously.


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Note: Peaks may be blurred because the slits may be wider.

26 Save the data as “calib.spc”. CalibA.spc is the R channel; CalibB.spc is the A channel.

27 Open the Real Time Display. 28 Close the shutter. 29 Set the

integration time to 0.5 s.

30 Write down channel R’s dark offset and channel A’s dark offset. These are the offset values.

31 On drive A:, run the program Calibrate Pho-toDiode.exe. This program calculates two new correction files. The Calibrate PhotoDiode window opens.


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32 Enter the signal offsets that you previously wrote down. a Enter signal offsets for R

and A.

b Click Load.

c The software asks for CalibA (click Open) and CalibB (click Open)

33 Save the power-correction file PowCorr.spc. Put it in DataMax, where data and xcorrect are stored, for example, in \DATA. If there is no computer, save onto the INI disk’s data-directory.

34 Save the quantum-correction file Xcorr.spc. Use the same directory as PowCorr.spc.

35 Click Cancel. The Calibrate PhotoDiode window closes.

36 View the files. On the next page is an example of PowerCorr.spc:


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This is an example of Xcorr.spc:

37 Revert to the old files in C:\datamax\isi_ini as necessary. a If ACQ4.ini and ACQ_HV4.ini were originally in the folder before

this procedure began, do not delete them or change their names.

b If ACQ4.ini and ACQ_HV4.ini were NOT originally in the folder, delete them.

c If ACQ44.ini and ACQ_HV44.ini exist now, rename them to ACQ4.ini and ACQ_HV4.ini, respectively.

d Delete the Diode.lay file.

38 Use the correction files.


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a Xcorr.spc provides the excitation correction for the excitation spec-trum. See the Fluorolog®-3 and FluoroMax®-3 operation manuals for how to use this file.

b PowCorr.spc helps to determine the power-levels at the sample. To determine the power-level at the sample, run a lamp scan at the setting of interest (excitation monochromator), and use PowCorr.spc to cor-rect the data from the reference (R) detector. The data will be reported in µW.


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References T.C. Larason, S.S. Bruce, and A.C. Parr, “Spectroradiometric Detector Measurements: Part I—Ultraviolet Detectors” and “Part II—Visible to Near-Infrared Detectors”, NIST Publ. 250-41 (1998). D.G. Taylor and J.N. Dermas, “Light Intensity Measurements I: Large Area Bolometers with Microwatt Sensitivities and Absolute Calibration of the Rhodamine B Quantum Counter”, Anal. Chem. 51 (6), 1979, pp. 712–722.


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calibration of the photodiode - horiba of the fluorolog-3 photodiode, v. 1.1 (23 sep 2004) 1...

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