Correction Factor Kit v. 1.1 (14 March 2008)

Transcription

1

2 Correction Factor Kit v. 1.1 (14 March 2008)

3 F-3026 Correction Factor Kit Operation Manual v (All HORIBA Jobin Yvon companies were formerly known as Jobin Yvon) USA: HORIBA Jobin Yvon Inc., 3880 Park Avenue, Edison, NJ , Toll-Free: jobinyvon Tel: , Fax: , France: HORIBA Jobin Yvon S.A.S., 16-18, rue du Canal, Longjumeau Cedex, Tel: +33 (0) , Fax: +33 (0) , Japan: HORIBA Ltd., JY Optical Sales Dept, Higashi-Kanda, Daiji Building, Higashi-Kanda Chiyoda-ku, Tokyo , Tel: +81 (0) , Germany: +49 (0) Italy: UK: +44 (0) China: +86 (0) i

4 Copyright 2008 by HORIBA Jobin Yvon. All rights reserved. No part of this work may be reproduced, stored, in a retrieval system, or transmitted in any form by any means, including electronic or mechanical, photocopying and recording, without prior written permission from HORIBA Jobin Yvon. Requests for permission should be requested in writing. Origin is a registered trademark of OriginLab Corporation. Spectralon is a registered trademark of Labsphere, Inc. Windows is a registered trademark of the Microsoft Corporation. Information in this manual is subject to change without notice, and does not represent a commitment on the part of the vendor. March 2008 Part Number ii

5 Table of Contents 0: Introduction About the Correction Factor Kit Chapter overview Disclaimer Safety summary Additional risks of tungsten-halogen lamps : Unpacking & Installation Electrical requirements Unpacking : System Description Introduction Components : Operation Set up the accessory Run the scan Analyze the data Remove the accessory : Maintenance : Troubleshooting Introduction Basic troubleshooting steps Further assistance : Technical Specifications Introduction Specifications : Correction-Factor-Kit Record of Use Form : Index iii

6 iv

7 0: Introduction About the Correction Factor Kit Introduction The F-3026 Correction Factor Kit is an NIST-traceable accessory for the FluoroMax and Fluorolog spectrofluorometers for calibrating the relative spectral response of the spectrofluorometer, and includes a Spectralon integrating sphere as a sampling optic. Each Correction Factor Kit includes a regulated 12 VDC power supply, a calibration certificate, and a CD with data files for use with FluorEssence software. The Correction Factor Kit provides 50 hours of operation before recalibration is necessary. Note: Keep this and the other reference manuals near the system. 0-1

8 Chapter overview 1: Unpacking & Installation How to unpack and install the accessory. 2: System Description Components of the Correction Factor Kit. 3: Operation How to set up and use the Correction Factor Kit. 4: Maintenance How to keep the Correction Factor Kit running properly for years to come. 5: Troubleshooting Potential sources of problems, their most probable causes, and possible solutions. Introduction 6: Technical Specifications Instrument specifications and computer requirements. 7: Correction-Factor-Kit Record of Use Form 8: Index A log to keep track of time that the accessory is used before recalibration is required. 0-2

9 Disclaimer By setting up or starting to use any HORIBA Jobin Yvon product, you are accepting the following terms: Introduction You are responsible for understanding the information contained in this document. You should not rely on this information as absolute or all-encompassing; there may be local issues (in your environment) not addressed in this document that you may need to address, and there may be issues or procedures discussed that may not apply to your situation. If you do not follow the instructions or procedures contained in this document, you are responsible for yourself and your actions and all resulting consequences. If you rely on the information contained in this document, you are responsible for: Adhering to safety procedures Following all precautions Referring to additional safety documentation, such as Material Safety Data Sheets (MSDS), when advised As a condition of purchase, you agree to use safe operating procedures in the use of all products supplied by HORIBA Jobin Yvon, including those specified in the MSDS provided with any chemicals and all warning and cautionary notices, and to use all safety devices and guards when operating equipment. You agree to indemnify and hold HORIBA Jobin Yvon harmless from any liability or obligation arising from your use or misuse of any such products, including, without limitation, to persons injured directly or indirectly in connection with your use or operation of the products. The foregoing indemnification shall in no event be deemed to have expanded HORIBA Jobin Yvon s liability for the products. HORIBA Jobin Yvon products are not intended for any general cosmetic, drug, food, or household application, but may be used for analytical measurements or research in these fields. A condition of HORIBA Jobin Yvon s acceptance of a purchase order is that only qualified individuals, trained and familiar with procedures suitable for the products ordered, will handle them. Training and maintenance procedures may be purchased from HORIBA Jobin Yvon at an additional cost. HORIBA Jobin Yvon cannot be held responsible for actions your employer or contractor may take without proper training. Due to HORIBA Jobin Yvon s efforts to continuously improve our products, all specifications, dimensions, internal workings, and operating procedures are subject to change without notice. All specifications and measurements are approximate, based on a standard configuration; results may vary with the application and environment. Any software manufactured by HORIBA Jobin Yvon is also under constant development and subject to change without notice. Any warranties and remedies with respect to our products are limited to those provided in writing as to a particular product. In no event shall HORIBA Jobin Yvon be held li- 0-3

10 Introduction able for any special, incidental, indirect or consequential damages of any kind, or any damages whatsoever resulting from loss of use, loss of data, or loss of profits, arising out of or in connection with our products or the use or possession thereof. HORIBA Jobin Yvon is also in no event liable for damages on any theory of liability arising out of, or in connection with, the use or performance of our hardware or software, regardless of whether you have been advised of the possibility of damage. 0-4

11 Safety summary Introduction The following general safety precautions must be observed during all phases of operation of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture and intended use of instrument. HORIBA Jobin Yvon assumes no liability for the customer s failure to comply with these requirements. Certain symbols are used throughout the text for special conditions when operating the instruments: Warning: A hazardous condition exists, or danger exists that could damage the equipment. HORIBA Jobin Yvon is not responsible for damage arising out of improper use of the equipment. Caution: Intense ultraviolet, visible, or infrared light! Wear light-protective goggles, full-face shield, skin-protection clothing, and light-blocking gloves. Do not stare into light. Warning: Hot! This symbol warns the user that hot equipment may be present, and could create a risk of fire or burns. Note: General information is given concerning operation of the equipment. Read this manual before using or servicing the instrument. Wear appropriate safety goggles to protect the eyes. 0-5

12 Introduction Additional risks of tungsten-halogen lamps Among the dangers associated with tungsten-halogen lamps are: Burns caused by contact with a hot bulb or its casing. Fire ignited by hot bulb. Interaction of other nearby chemicals with intense ultraviolet, visible, or infrared radiation. Damage caused to apparatus placed close to the lamp. Explosion or mechanical failure of the lamp. Visible radiation Any very bright visible light source will cause a human aversion response: we either blink or turn our head away. Although we may see a retinal afterimage (which can last for several minutes), the aversion response time (about 0.25 seconds) normally protects our vision. This aversion response should be trusted and obeyed. NEVER STARE AT ANY BRIGHT LIGHT-SOURCE FOR AN EXTENDED PERIOD. Overriding the aversion response by forcing yourself to look at a bright light-source may result in permanent injury to the retina. This type of injury can occur during a single prolonged exposure. Excessive exposure to visible light can result in skin and eye damage. Visible light sources that are not bright enough to cause retinal burns are not necessarily safe to view for an extended period. In fact, any sufficiently bright visible light source viewed for an extended period will eventually cause degradation of both night and color vision. Appropriate protective filters are needed for any light source that causes viewing discomfort when viewed for an extended period of time. For these reasons, prolonged viewing of bright light sources should be limited by the use of appropriate filters. The blue-light wavelengths ( nm) present a unique hazard to the retina by causing photochemical effects similar to those found in UV-radiation exposure. Infrared radiation Warning: Tungsten-halogen lamps can be dangerous. Please read the following precautions. Infrared (or heat) radiation is defined as having a wavelength between 780 nm and 1 mm. Specific biological effectiveness bands have been defined by the CIE (Commission International de l Eclairage or International Commission on Illumination) as follows: IR-A (near IR) ( nm) IR-B (mid IR) ( nm) IR-C (far IR) (3000 nm 1 mm) 0-6

13 Introduction The skin and eyes absorb infrared radiation (IR) as heat. Workers normally notice excessive exposure through heat sensation and pain. Infrared radiation in the IR-A that enters the human eye will reach (and can be focused upon) the sensitive cells of the retina. For high irradiance sources in the IR-A, the retina is the part of the eye that is at risk. For sources in the IR-B and IR-C, both the skin and the cornea may be at risk from flash burns. In addition, the heat deposited in the cornea may be conducted to the lens of the eye. This heating of the lens is believed to be the cause of so called glassblowers cataracts because the heat transfer may cause clouding of the lens. Retinal IR Hazards (780 to 1400 nm): possible retinal lesions from acute high irradiance exposures to small dimension sources. Lens IR Hazards (1400 to 1900 nm): possible cataract induction from chronic lower irradiance exposures. Corneal IR Hazards (1900 nm to 1 mm): possible flashburns from acute high irradiance exposures. Who is likely to be injured? The user and anyone exposed to the radiation or tungstenhalogen lamp shards as a result of faulty procedures. Injuries may be slight to severe. 0-7

14 Introduction 0-8

15 1: Unpacking & Installation Electrical requirements Unpacking & Installation In addition to those required for the instrument, at least one extra outlet must be available for the Correction Factor Kit. Voltage Factory preset at 110 V ± 5% at 60 Hz or 220 V ± 5% at 50 Hz Three-conductor power cord connected to the system frame (earth) ground. This ground provides a return path for fault current from equipment malfunction or external faults. Warning: For all instruments, ground continuity is required for safe operation. Any discontinuity in the ground line can make the instrument unsafe for use. Do not operate this system from an ungrounded source. HORIBA Jobin Yvon is not liable for damage from line surges and voltage fluctuations. A surge protector is strongly recommended for minor power fluctuations. For more severe voltage fluctuations, a generator or an uninterruptible power supply is suggested. Improper line voltages can damage the equipment severely. 1-1

16 Unpacking When the Correction Factor Kit arrives The accessory is delivered disassembled. The shipment should include: Power cords Power supply Source/integrating sphere module Special gap-bed Sample-compartment cover Manual CD with irradiance data Thumbscrews Calibration datasheet Unpacking & Installation Note: The source/integrating sphere module may arrive premounted atop the special gapbed. General checklist for the Correction Factor Kit Quantity Item Part Number 1 Source/integrating sphere module VDC power supply 1 12 VDC power cord 1 Mains power cord 1 Special gap-bed 1 Extended lid CD with irradiance data 1 Calibration datasheet 1 F-3026 Correction Factor Kit Operation Manual Brass thumbscrew Examine the shipping boxes carefully. If damage is evident, do not continue with the installation. Notify HORIBA Jobin Yvon and the shipper at once. Note: Many public carriers do not recognize claims for concealed damage reported later than 15 days after delivery. For a shipping damage claim, inspection by the carrier agent is required. Therefore, the original packing material should be kept as evidence. While HORIBA Jobin Yvon is not responsible for damage occurring during transit, the company will extend every effort to aid and advise. To avoid damage, unpack the equipment as close as possible to the selected location of the instrument. HORIBA Jobin Yvon suggests that you unpack the equipment in order to set the major components on the table, while also checking that all parts have arrived undamaged. Package contents The Correction Factor Kit is contained in packing cartons. If any other special accessories were included in the order, they accompany the accessory, unless specified by 1-2

17 Unpacking & Installation HORIBA Jobin Yvon. See the Performance Test Report or the sales order for a list of all items shipped or back-ordered. Unpacking instructions 1 Open the shipping carton. 2 Remove the foam-injected top piece and any other shipping restraints in the carton. 3 With at least one helper, carefully lift the components from the carton and Warning: Watch your fingers! put them on the table on which the system will rest. 4 Unpack all other boxes containing power supplies, detectors, cables, and manu- Note: Do not dispose of shipping cartons until after installation. als. Store all these items together in a safe location. 5 Inspect for previously hidden damage. Notify the carrier and HORIBA Jobin Yvon if any damage is found. 6 Check the packing list and sales order to verify that all components are present. 1-3

18 Unpacking & Installation 1-4

19 2: System Description System Description Introduction The Correction Factor Kit consists of the following major components: Module with light-source and integrating sphere mounted on a special gap-bed Special sample-compartment cover Power supply for module Irradiance data Components Module with light-source and integrating sphere The light-source (tungsten-halogen lamp) and integrating sphere are combined in a single module, mounted on a special gap-bed. This special gap-bed replaces the normal gap-bed that was included with your instrument. The 12 VDC power cord for the light source is threaded through the front of the sample compartment in a light-tight manner. Every 50 hours the accessory ought to be recalibrated. Special sample-compartment cover Because the light-source and integrating sphere module is taller than the standard sample compartment, a special sample-compartment cover is included to make the interior of the sample compartment light-tight. Power supply for module An external regulated 12 VDC power supply supplies electricity to the light source. This power supply is connected to your standard AC wall outlet (mains). Irradiance data For relative calibration of the module, irradiance data from the near-uv through IR are included on a CD with the Kit. These data can be loaded into FluorEssence to provide relative irradiance data from the module. A separate datasheet is also included. 2-1

20 System Description 2-2

21 3: Operation Set up the accessory. 1 Attach the correctionfactor light-source to its gap-bed with the brass thumbscrews. Use this orientation. Be sure the power cable doesn t block optical apertures. Operation Note: The source/integrating sphere module may arrive premounted atop the special gap-bed. 2 Plug the power cable into the front of the gap-bed. 3 Remove the standard sample-compartment gap-bed, and insert the correction-factor kit gapbed into the sample compartment. Fix the gap-bed firmly to the sample compartment with screws through the front panel. 3-1

22 Run the scan. 1 Start FluorEssence and initialize the instrument. Turn the xenon lamp OFF, and the lamp for the correction-factor kit ON. ON Operation Warning: Wear appropriate eye-protection against UV, visible, and IR when the tungsten-halogen lamp is on and the sample-compartment is uncovered. Note: We recommend keeping a log of the amount of time the source is on. Calibration is necessary after every 50 h of use. 2 Put the raised lid on the sample compartment. Make sure it fits securely, and there is no light leak into the sample compartment. Caution: Do not operate the accessory without the lid completely covering the sample compartment. 3 Collect an emission scan using the following scan parameters: Range: nm; increment: 5 nm; integration time: 1 s 3-2

23 Analyze the data. 1 Import the standard irradiance file for the calibrated lamp in the correction-factor kit: a In the File menu, click Import, and choose SPC Data. Operation The Open window appears. b Browse for and choose the irradiance file on the CD-ROM (included with this kit). Note: Choose the correct irradiance file associated with the desired detector. c Click the Open button. The irradiance file opens. 2 Identify the datalabel names for the two graphs. Right-click on the curve; the data name appears at the bottom. 3-3

24 3 From the File menu, choose New... The New window appears. Operation 4 Choose Graph, then the OK button. A new plot appears on the FluorEssence main window. 5 In the Analysis menu, choose Simple Math... The Simple Math Tool window opens. 3-4

25 Operation a Choose the data corresponding to the irradiance file. b Choose divide as the math function c For Operand, select the data corresponding to the emission spectrum obtained using the correction-factor kit. d Select the Add New radio button, and click the Apply button. 6 The new graph now displays the correction factor. Normalize the graph as follows: a Right-click on the correction-factor curve and click Go to Data. b Highlight the B(Y) column, right click and select Normalize. c Note down the Min. number. d Open a new graph from the file menu. e Again, choose Simple Math... from the Analysis menu and choose the data name corresponding to the correction-factor data file. f Select the divide function. g For Operand, select constant and enter the Min. number noted previously. h Select the Add New radio button and click the Apply button. 3-5

26 7 Export the normalized correction-factor graph. In the File menu, click Export, and select SPC Data. Operation 8 Apply the correction factor into your system configuration by following the instructions in your instrument manual. Remove the accessory. 1 Remove the sample-compartment cover. Warning: Always wear appropriate eye-protection against bright UV, visible, and IR light when the tungsten-halogen lamp is on and the sample-compartment is uncovered. 2 Turn OFF the accessory. OFF Warning: The accessory may be HOT. Let the accessory cool before removal! 3-6

27 Operation Note: We recommend keeping a log of the amount of time the source is on. Calibration is necessary after every 50 h of use. 3 Remove the accessory s sample-compartment gap-bed, and return the standard gap-bed to the sample compartment. 3-7

28 Operation 3-8

29 4: Maintenance Maintenance Every 50 hours, the Correction Factor Kit must be recalibrated. Call the Spex Fluorescence Service Department at (732) , or fax us at (732) , for instructions on how to ship the Kit to us for recalibration. 4-1

30 Maintenance 4-2

31 5: Troubleshooting Introduction Troubleshooting Because your spectrofluorometer has many user settings and adjustable parameters, many apparent system failures are simply problems with the experimental setup, sample geometry, or choice of sample. If the symptoms indicate that a problem may be a system failure, contact the Spex Fluorescence Service Department, or your local distributor. Refer to the spectrofluorometer s Operation Manual and the FluorEssence User s Guide for help with troubleshooting problems in steady-state operation. This chapter is intended to isolate and solve problems regarding operation of the Correction Factor Kit with the system only. 5-1

32 Basic troubleshooting steps Troubleshooting When an apparent problem is first observed, follow the basic steps and suggestions outlined below to troubleshoot the initial problem. In many cases, shutting down the system, carefully restarting, and redoing an experiment helps to remove an unseen or outside issue that was causing the apparent problem. If the suggestions that follow do not help to remove the problem, note the steps that led up to the problem, and proceed to the next section. 1 Reboot. If this is the first time the problem has occurred, try restarting the system. Turn off all components and accessories. After a cool-down period, turn the system on and see if the failure persists. Many apparent software and hardware problems are actually conflicts with other software or peripheral devices currently active on the system. 2 Check the connections. With the power to all components and accessories turned off, make sure all accessories and cables are attached and configured properly. Verify that line cords provide the proper input AC voltage, and that all appropriate accessories and power supplies are powered ON during use of the system. 3 Verify system performance. Verify that the system is properly calibrated in steady-state mode. Print out each spectrum, and note the peak intensities and wavelength positions. 4 Duplicate the error. Try to duplicate the problem, and write down the steps required to do so. Our service engineers will attempt the same with a test system. Depending on the nature of the problem, a service visit may not be required. 5-2

33 Further assistance... Troubleshooting Read all software and accessory manuals before contacting the Spex Fluorescence Service Department. Often the manuals show the problem s cause and a method of solution. Technical support is available for both hardware and software troubleshooting. Before contacting the service department, however, complete the following steps. 1 If this is the first time the problem has occurred, try turning off the system and accessories. After a cool-down period, turn everything back on. 2 Make sure all accessories are properly configured, and turned on as needed. 3 Following the instructions in Operation, run a xenon-lamp scan and a water-raman scan to make sure the system is properly calibrated. Print the spectrum for each and note the peak intensities. 4 Check this chapter to see if the problem is discussed. 5 Visit our web site at See if the question is addressed in the Systems or FAQs sections of the site. 6 Try to duplicate the problem and write down the steps required to do so. The service engineers will try to do the same with a test system. Depending on the problem, a service visit may not be required. 7 If an error message appears in FluorEssence, write down the exact error displayed. 8 Determine FluorEssence s version number. a Choose the Help menu. b Choose About FluorEssence

34 The About FluorEssence window opens. Near the bottom are the FluorEssence and Origin version numbers. Troubleshooting c Click the OK button to close the window. 9 Write down the software s version numbers, along with the purchase dates, model numbers, system configuration, and serial numbers of the instrument and its accessories. 10 Call the Spex Fluorescence Service Department at (732) Be prepared to describe the malfunction and the attempts, if any, to correct it. Have serial and version numbers of all software and equipment handy, along with all relevant spectra (sample, polarization ratio, xenon-lamp scan, emission calibration, etc.). If the problem persists or is unlisted, call the Spex Fluorescence Service Department at (732) , or fax us at (732)

35 6: Technical Specifications Introduction Each F-3026 Correction Factor Kit consists of: An excitation source and integrating sphere in one module A special gap-bad for the sample compartment A special cover for the sample compartment 12 VDC output power supply A CD with irradiance file Specifications Excitation source Tungsten-halogen lamp Time between calibrations 50 h Calibrated range nm Calibration method As per NIST Handbook 150-2E Output data Absolute values in µw/nm Integrating sphere size 1.5 (3.8 cm) diameter Integrating sphere material Spectralon Electrical power input V AC, Hz, 0.7 A Technical Specifications 6-1

36 Technical Specifications 6-2

37 Correction-Factor-Kit Record of Use Form 7: Correction-Factor-Kit Record of Use Form Because the spectral output of a tungsten-halogen bulb can vary slightly over time, we recommend recalibration of the correction factor kit every 50 hours. Use the record-ofuse form on the next page to keep a log of usage for the correction factor kit. Contact the Spex Fluorescence Service Department for instructions on recalibration, at (732) , or fax us at (732) , when the 50 hours of usage is reached. 7-1

38 Correction-Factor-Kit Record of Use Form Correction-Factor-Kit Record of Use Page of In Service Date Operator Current Date Time On Time Off Total Time (Hours/Min.) Total Hours / 7-2

39 8: Index Key to the entries: Times New Roman font...subject or keyword Arial font...command, menu choice, or data-entry field Arial Condensed Bold font...dialog box Courier New font...file name or extension A About FluorEssence window About FluorEssence Add New radio button Analysis menu Apply button B B(Y) column C Index calibration certificate D damage danger divide E emission scan Export F File menu , 3-6 FluorEssence 0-1, 2-1, 3-2, 3-4, 5-1, Fluorolog FluoroMax G gap-bed...1-2, 2-1, 3-1, 3-7 Go to Data Graph H hazardous condition Help menu hot equipment I Import infrared radiation integrating sphere...0-1, 1-2, 2-1, 6-1 intense light irradiance data...1-2,

40 irradiance file...3-3, 3-5, 6-1 S Index M Material Safety Data Sheets Min , 7-2 MSDS N New window New NIST , 6-1 normalization Normalize O OK button , 5-4 Open button Open window Operand P power supply , 1-2, 2-1, 6-1 R read this manual notice recalibration...0-1, 4-1, 7-1 record-of-use form safety goggles notice safety precautions sample-compartment cover , 2-1, 3-6 Service Department...4-1, 5-1, 5-3 4, 7-1 Simple Math Tool window Simple Math SPC Data...3-3, 3-6 Spectralon...0-1, 6-1 symbols T thumbscrews...1-2, 3-1 troubleshooting tungsten-halogen lamp , 3-2, 6-1, 7-1 tungsten-halogen lamp risks V visible radiation W water-raman scan X xenon lamp xenon-lamp scan

41 HORIBA JOBIN YVON INC Park Ave., Edison, New Jersey , U.S.A. [Design Concept] The HORIBA Group application images are collaged in the overall design. Beginning from a nano size element, the scale of the story develops all the way to the Earth with a gentle flow of the water.

42