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TCSPC on FluoroMax v. 1.0 (28 Oct 2005)

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FM-2013

TCSPC on FluoroMax®

Operation Manual v. 1.0 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)


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Copyright © 2005 by HORIBA Jobin Yvon. 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 HORIBA Jobin Yvon. Requests for permission should be requested in writing. Ludox® is a regulated trademark of Grace Davison. Origin® is a registered trademark of OriginLab Corporation. Information in this manual is subject to change without notice, and does not rep-resent a commitment on the part of the vendor. October 2005

Part Number 81091


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Table of Contents 0: Introduction ........................................................................................... 0-1

About the TCSPC on FluoroMax®.................................................................................................... 0-1 Chapter overview ............................................................................................................................. 0-2 Symbols used in this manual ........................................................................................................... 0-3 Laser safety information................................................................................................................... 0-4

1: Unpacking & Installation ............................................................................ 1-1 Electrical requirements..................................................................................................................... 1-1 Unpacking ........................................................................................................................................ 1-2 Installation ........................................................................................................................................ 1-5 Adjusting optics ................................................................................................................................ 1-8 Attaching the temperature bath to the FL-1065 ............................................................................. 1-11

2: System Description .................................................................................. 2-1 Components ..................................................................................................................................... 2-1 Software ........................................................................................................................................... 2-2 System diagram ............................................................................................................................... 2-2

3: Operation .............................................................................................. 3-1 Using the CW or optional pulsed xenon lamps................................................................................ 3-1 Using the TCSPC accessory............................................................................................................ 3-2 Changing NanoLED sources............................................................................................................ 3-3 Heating/cooling (FL-1065 only) ........................................................................................................ 3-4

4: Maintenance .......................................................................................... 4-1 FL-1065 heater/cooler...................................................................................................................... 4-1

5: Accessories ........................................................................................... 5-1 Phosphorimeter ................................................................................................................................ 5-2 NanoLED.......................................................................................................................................... 5-3 SpectraLED...................................................................................................................................... 5-5 FL-1065 Thermostatted Sampling Module and FL-1066 Upgrade .................................................. 5-6 F-1000/1 Temperature Bath............................................................................................................. 5-7

6: Troubleshooting ...................................................................................... 6-1 Introduction....................................................................................................................................... 6-1 Basic troubleshooting steps ............................................................................................................. 6-2 Further assistance............................................................................................................................ 6-3

7: Technical Specifications ............................................................................ 7-1 Spectrofluorometer system .............................................................................................................. 7-1 Phosphorimeter (FluoroMax®-P only) .............................................................................................. 7-3 Host computer .................................................................................................................................. 7-4 Software ........................................................................................................................................... 7-4

8: Declaration of Conformity....................................................................... 8-1 9: Index ................................................................................................... 9-1


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TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Introduction

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Note: Keep this and the other reference manuals near the system.

0: Introduction About TCSPC on FluoroMax®

The TCSPC on FluoroMax® is an accessory for the FluoroMax®-3 and FluoroMax®-P spectrofluorometers that adds lifetime-capability in the time domain. The optical port mounted on the sample compartment adds the lifetime-capability. The source (NanoLED or SpectraLED) quickly mounts on the sample compartment, and includes focusing lens. The FM-2013 uses DataStation software for time-domain lifetime meas-urements, and FluorEssence™ software for steady-state and optional phosphorescence measurements. A special sample compartment (FL-1057 or FL-1065) is required, and must be ordered separately. Discussion concerning environmental re-quirements, theory, and setup of steady-state and phosphorescence experiments are found in the FluoroMax®-3/P Operation Manual. Differences and extensions to the standard FluoroMax®-3 and FluoroMax®-P are found herein.


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Chapter overview 1: Unpacking & Installation How to unpack and install the accessories. 2: System Description Components of the TCSPC on FluoroMax® accessory. 3: Operation How to switch from steady-state to lifetime modes.

How to change from one NanoLED source to another. 4: Maintenance How to keep the TCSPC accessory running properly

for years to come. 5: Accessories Additional light-sources and accessories to expand

your experimental capabilities. 6: Troubleshooting Potential sources of problems, their most probable

causes, and possible solutions. 7: Technical Specifications Instrument specifications and computer requirements. 8: Declaration of Conformance Shows that the accessory conforms to safety

requirements for the CE. 9: Index


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Warning:

Note:

Warning:

Caution:

Caution:

Symbols used in this manual Certain symbols are used throughout the text for special conditions when operating the instruments:

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.

A hazardous high-voltage condition exists that could injure or kill a person. HORIBA Jobin Yvon is not responsible for damage arising out of improper use of the equipment.

Laser radiation exists that could damage the eye. Take appropriate safety precautions, and never look directly at the laser beam.

Laser radiation exists that could damage the eye. Take appropriate safety precautions, and never look directly at the laser beam.

General information is given concerning operation of the equipment.


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Warning: Do not attempt to operate the NanoLED or Spec-traLED excitation system without first reading all manuals. Do not attempt to open the NanoLED or SpectraLED exci-tation sources. There are no user-serviceable compo-nents inside. Opening the NanoLED or SpectraLED exci-tation sources is dangerous, and will invalidate your war-ranty. If in doubt, contact HORIBA Jobin Yvon for advice.

Be sure to follow all warnings, cautions, and directions given by manufacturers of third-party lasers that you may attach to this system.

Caution: NanoLED or SpectraLED sources can be either LEDs or La-sers emitting in the UV, visible or near-IR. Some NanoLED excita-tion sources generate laser light radiation. Do not look directly at the beam, and always observe ap-propriate safety procedures.

Using controls or adjustments or performing procedures other than those specified herein may result in hazardous radiation exposure. Ifin doubt, contact HORIBA Jobin Yvon or your laser safety officer for advice.

Laser safety information Cautionary notices

Important NanoLED, SpectraLED, and other third-party excitation sources are intended for spectroscopic applications, and as such, should be mounted onto an enclosed light-tight optical system for normal operation. NanoLED sources are designed to be mounted to a metallic surface to remove excess heat. Do not allow the sources to become hot during operation. The better the heat-sinking ability, the higher the stability of the NanoLED and SpectraLED output.


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Laser certification, identification, and warning labels Sample-compartment cover All TCSPC accessories for the FluoroMax® have a warning label on the cover of the instrument’s sample compartment:

Sampling module A laser safety warning and identification label are located on the front cover of the sampling module.

October 2004

FL-1057

001


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Laser-beam path The path of the laser beam when the NanoLED, SpectraLED, or other laser is mounted directly on the Fluorolog® system’s sample compartment is as shown.

Laser or LED specifications Any Class 1 or 2 (IEC) or Class I or II (FDA) lasers or LEDs emitting visible or invisi-ble radiation, with appropriate pulse-lengths for use in steady-state, TCSPC, or phos-phorescence modes are capable of being used with these laser products.

Recommended laser or LED sources HORIBA Jobin Yvon recommends the following laser or LED sources for use in the system:

Picosecond laser sources UV laser 375 nm NanoLED-11 Violet laser 405 nm NanoLED-07 Blue laser 440 nm NanoLED-10 Cyan laser 473 nm NanoLED-14 Red laser 635 nm NanoLED-02B Red laser 650 nm NanoLED-02 Red laser 670 nm NanoLED-02C Near-IR laser 785 nm NanoLED-12A Near-IR laser 830 nm NanoLED-12B Near-IR laser 1310 nm NanoLED-17

LED sources UV 280 nm NanoLED-15 UV 340 nm NanoLED-16 UV 370 nm NanoLED-03 Blue 455 nm NanoLED-05A Blue 465 nm NanoLED-05B Aqua 485 nm NanoLED-01 Green 560 nm NanoLED-09 Amber 590 nm NanoLED-04 Orange 605 nm NanoLED-08 Red 625 nm NanoLED-06

For SpectraLED wavelengths, please contact HORIBA Jobin Yvon or your local repre-sentative.

sample com-partment

laser port LASER-BEAM PATH


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Warning: For all instruments, ground continuity is required for safe operation. Any discontinuity in the ground line can make the in-strument 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 fluctua-tions, a generator or an uninterruptible power supply is sug-gested. Improper line voltages can damage the equipment se-verely.

1: Unpacking & Installation Electrical requirements

In addition to those required for the FluoroMax®-3, at least one extra outlet must be available for the DataStation Hub.

Voltage • Factory preset at 110 V ± 5%/60 Hz or 220 V ± 5%/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.


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Warning: The TCSPC accessories are delicate instruments with sensitive components. Mishandling may seriously damage the systems.

Note: A TCSPC on FluoroMax® acces-sory automatically includes a new host computer. If you have ordered an up-grade to an existing FluoroMax®, HO-RIBA Jobin Yvon recommends using only the new host computer. It is possi-ble to continue using the existing one for steady-state or optional phosphores-cence experiments, but you will have to swap cables.

Unpacking When the TCSPC for the FluoroMax® arrives

The accessory is delivered disassembled. The shipment should include: • Cables • Software • DataStation Hub • Host computer • Monitor • Manuals • TCSPC sticker • Optional one or more

NanoLED sources

General checklist for the TCSPC on FluoroMax® Quantity Item Part Number

1 NanoLED sample compartment, if ordered (or with optional heating and cooling system)

FL-1057 or FL-1065

1 DataStation Hub FL-1061 1 Host computer 973130 1 Monitor 973133 1 or more NanoLED light source(s), if ordered 1 NanoLED polarizer, if ordered Many Power cords (110 V)

(220 V) 98015 98020

1 TCSPC BNC signal cable, 1 m long 1 TCSPC sticker 570126 1 Optical blanking filter-plate (beam-block) 4 Mounting screws for sampling module, if sample compartment is ordered 61552 1 Optional enhancement kit for 100 ps lifetime ability (if ordered) 354186 1 FluorEssence™ Software Kit FluorEssence 1 TCSPC on FluoroMax® Operation Manual 81091 1 IBH Software Operation Manual 1 NanoLED Operation Manual (if NanoLED is ordered)


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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 HO-RIBA Jobin Yvon is not responsible for damage occurring during tran-sit, the company will extend every effort to aid and advise.

Warning: Watch your fingers!

Examine the shipping boxes carefully. If damage is evident, do not continue with the installation. Notify HORIBA Jobin Yvon and the shipper at once.

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 TCSPC accessory is contained in packing cartons. If any other special accessories were included in the order, they accompany the instrument, unless specified by HO-RIBA 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 put them on the table on which the system will rest.

4 Unpack all other boxes containing power supplies, detectors, cables, and manuals. 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.

Note: Do not dispose of shipping cartons until after installation.


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6 Check the packing list and sales order to verify that all components are present.

7 Remove the foam packing support from inside the host computer. Follow the directions with the host computer on how to open the computer case.


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Installation 1 If the accessory is ordered as an upgrade, at-

tach the enclosed laser warning label to the FluoroMax® sample-compartment lid.

2 Attach the NanoLED to the sample compart-ment. a Remove existing

sampling module.

b Slide new sampling module into sample compartment.


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c Screw in four screws to hold the new sampling module.

You may use the new mounting screws supplied, or the old, existing ones.

d Slide the NanoLED into the holder.

e Tighten the thumb-screw.

f Attach the driver cable.

g Attach the other end of the driver cable to the Drive connector in the NanoLED area, on the rear of the DataStation Hub.


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Note: When running steady-state (or optional phos-phorimetry) experiments, switch the side-panel switch ON.

3 Attach the BNC cable to the FluoroMax®. The BNC connector attaches to the TO HUB jack on the side panel.

4 Attach the other end of the BNC cable to the DataStation Hub. The BNC connector attaches to the TAC Start jack on the rear panel.

5 Switch the xenon lamp(s) off. Switch the side-panel switch to OFF.


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Note: The lenses inside the sample compartment suffer from chromatic aberration. Focusing the lenses improves the signal. NanoLEDs emitting blue or UV require extra focusing, be-cause the chromatic aberration changes more rapidly as the wavelength decreases.

Warning: Do not stare into laser beam when focusing.

Adjusting optics 1 Focus the lens.

a Insert a sample of Ludox® or similar scatterer in a cuvette.

b Loosen machine screw to free the lens.

c Follow the IBH manual to monitor the signal.

d Optimize the signal by sliding the lens in and out.

e With maximized sig-nal, lock the lens by tightening the machine screw.

2 Filter the NanoLED beam.


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Note: HORIBA Jobin Yvon does not recom-mend relying on the in-trinsic polarization of the laser-diode alone.

Note: The polarizers are not located midway along their mounts. To maximize throughput, orient the holders so that the polarizers are nearest the detector or light source, as appropri-ate.

HORIBA Jobin Yvon recommends optional 2" (50 mm) short-pass or band-pass filters in front of the NanoLED. Mount them in front of the lens. This arrange-ment gives better stray-light rejection than mounting them on the sample holder. In addition, the sample’s temperature can be controlled, and some filters’ char-acteristics change with temperature.

3 Polarize the beam.

An optional polarizer accessory is available to change the polarization of the NanoLED excitation beam. To change the polarization, rotate the knob.

Inserting the polarizers

a Remove the empty polarizer holders from their seats, by removing the polarizer idling-plugs with the appropriate Allen key.

The holders contain rubber O-rings at each end to exclude light, and should fit quite tightly. The polarizers are already mounted, ready for insertion.

b Insert the polarizers. The mounts have V-grooves on the top and bottom. These grooves help to align the polarizers automatically in the vertical position, with the small, pointed set screw in the holder.

c Tighten the set screw using the supplied key.

d Replace the holders in the polarizer seat.

Note: Contact your HORIBA Jobin Yvon representative for prices and availability of appropriate filters and polarizers for the NanoLED.


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The LED sources are unpolarized, while the laser-diode sources are linearly po-larized. HORIBA Jobin Yvon recommends setting the excitation polarizer to vertical, and the laser-diode rotated to maximize the count-rate. For better accuracy, set the excitation polarizer to horizontal, rotate the laser-diode to minimize the count-rate (i.e., extinction), and then rotate the excitation polarizer back by 90°.


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Warning: Failure to clamp these hoses securely may result in flooding and damage to the op-tics and electronics of the instrument.

Attach the temperature bath (FL-1065 only)

1 Attach the ¼" tubing from the temperature bath to the inlets on the front panel of the FL-1065.


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TCSPC on FluoroMax v. 1.0 (28 Oct 2005) System Description

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2: System Description Components

The TCSPC on FluoroMax® accessory consists of the following major components: • Sampling module with

NanoLED mounting and optional heating/cooling

• One or more optional NanoLED solid-state pulsed light sources

• DataStation Hub • Host computer

Sampling module with NanoLED mounting The sampling module holds a standard cuvette, and contains a custom mounting for a NanoLED source, along with an adjustable lens to account for chromatic aberration of the lens from different wavelengths of the different NanoLED sources. The FL-1065 sampling module includes ability to heat and cool the sample, and an adjustable-speed magnetic stirrer. The sampling module replaces the standard FluoroMax® sampling module, sliding in and out of the sample compartment.

NanoLED source The NanoLED is a novel light-source system that uses a variety of light-emitting diode (LED) and laser-diode devices to generate nanosecond and picosecond optical pulses over a wide spectral range. The LEDs generate nanosecond pulses in the UV and visible, while the laser-diodes generate picosecond pulses in the UV (375 nm), violet, blue, red, and near-IR. The NanoLEDs are fixed-wavelength light-sources, but are easily interchanged. For more details, see the NanoLED instruction manual. The electronic driver for the NanoLED sources is a NanoLED controller.

DataStation Hub The DataStation Hub counts and times the arrival of the photons that make up the fluorescence-decay curve. DataStation software controls the DataStation Hub.

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) System Description

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Warning: Always place the beam-block in the filter-holder in front of the NanoLED when operating the 150 W xenon lamp. Radiation from the xenon lamp can damage the NanoLED.

Software

Steady-state and optional phosphorescence mode For steady-state experiments and optional pulsed source for phosphorimetry, the FluoroMax® uses FluorEssence™ software, supplied with the accessory.

TCSPC time-domain lifetime mode In the time domain, the FluoroMax® with DataStation Hub uses DataStation software, supplied with the accessory.

System diagram Below is a sketch of the TCSPC accessory when mounted on the sample com-partment of a basic FluoroMax®-3 spectrofluorometer.

FluoroMax®

Nano-LED

DataStation Hub

Hos

t com

pute

r

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Operation

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Warning: Always place the beam-block in the filter-holder in front of the NanoLED when operating the 450 W CW xenon lamp or pulsed xenon lamp. Radiation from the xenon lamp can damage the NanoLED.

Note: If the TCSPC accessory switch is left off, increased dark counts or spurious data can result.

3: Operation Using the CW or optional pulsed xenon lamps

1 Place the beam-block in the filter-holder in front of the NanoLED for protection.

2 Switch the side-panel switch to ON.

3 Use FluorEssence™ software.


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Using the TCSPC accessory 1 Remove the beam-

block from the NanoLED filter-holder.

2 Switch the side-panel switch to OFF.

3 Use DataStation software.


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Changing NanoLED sources 1 Turn off the NanoLED source via the software. 2 Loosen the

thumbscrew on the NanoLED holder.

3 Disconnect the driver cable.

4 Remove the old NanoLED from the holder.

5 Connect the driver cable to the new NanoLED.

6 Insert the new NanoLED into the holder.

7 Tighten the thumbscrew on the NanoLED holder. If the new NanoLED’s wavelength is < 500 nm, refocus the beam as explained in Chapter 1.


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Note: Selecting too high a speed may create a vortex, which could affect the reproducibility of the measurement.

Heating/cooling (FL-1065 only) 1 Place the sample in a 10 mm × 10 mm cuvette

and insert a magnetic stirring bar. (The stirring bar is available from Bel-Art Products, Pequannock, NJ)

2 Place a cuvette in each holder. 3 Allow the samples to reach the desired tempera-

ture. 4 Turn on the magnetic stirrer. 5 Select the appropriate mixing speed.

6 Run your experiment as usual. The speed at which the sample should be mixed depends on the viscosity of the sample.

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Maintenance

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4: Maintenance The FluoroMax®-3 Operation Manual explains maintenance of the basic spectro-fluorometer itself. For information on maintenance of the NanoLEDs and SpectraLEDs, see the IBH instruction manuals provided with those light-sources. Upkeep for the DataStation Hub is mentioned in its instruction manual.

FL-1065 heater/cooler Examine the sampling module regularly for leaks. Tighten the hose-clamps as needed.

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Maintenance

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TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Accessories

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5: Accessories The laser-port on the sample compartment can accommodate one light source from among the following: • Solid-state NanoLED fixed-wavelength, pulsed light-source • SpectraLED fixed-wavelength, pulsed light-source • Other third-party pulsed laser In this section, various light-source accessories for the sample-compartment accessories are listed, so that you can expand your system to the highest experimental capability.


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Phosphorimeter accessory The phosphorimeter adds a programmable, pulsed excitation source and selectable sig-nal gating from the signal photomultiplier tube. This provides time-discrimination ca-pability to sort out the lifetimes of simultaneous, competing luminescence emissions. Because the duration of each exciting pulse from the phosphorimeter is very short (~3 μs), lamp interference during acquisition of decay curves is minimized. This allows the researcher to follow the decay of samples an order-of-magnitude faster than can be achieved with conventional systems that depend on mechanical choppers. To run phosphorescence experiments, the FluoroMax®-P phosphorescence upgrade, which adds a controller and electronics, is required. The phosphorimeter accessory is activated via the software. This action rotates a mirror inside, directing light from the flash tube to the sample:

Internal mirror rotates to phosphorimeter mode.

Pulsed lamp

CW lamp

Mirror


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NanoLED Introduction

A NanoLED is one of a variety of interchangeable light-sources, either light-emitting diode (LED) or laser-diode devices, to generate nanosecond and picosecond optical pulses over a wide spectral range. LED-based sources generate nanosecond pulses in the UV (280 nm) and visible, while laser-diode-based sources generate picosecond or nanosecond pulses in the UV (from 370 nm), visible, and near-IR. NanoLEDs are ideal sources for fluorescence-lifetime and biomedical applications. They are compact, easy to use, and extremely reliable: most sources feature a twelve-month warranty as standard. NanoLEDs are a range of inter-changeable NanoLED sources, each designed for use over a specific wavelength-range. High-intensity laser-diode versions are now available for those who require the most energy per pulse. These typically produce pulses of 0.9 ns duration. Each NanoLED source contains precision collection-optics and a 35 mm diameter bayonet-mounting flange for easy incorporation into your TCSPC accessory. Dedicated drive electronics in each NanoLED source means that swapping NanoLEDs involves removing a self-latching connector from the rear of one NanoLED source and plugging it into the next.

Features • Interchangeable NanoLED heads: “plug-and-play” operation even between LEDs

and diode lasers • Superior pulse-profiles • Each source contains built-in multi-element or aspheric collection-optics and bayo-

net mounting-flange • Gold-plated casings for minimized electromagnetic emission • “Sync delay” control allows quick adjustment of sync output relative to optical

pulse (up to 200 ns) • Twelve-month warranty on most NanoLED components as standard • Optional dichroic polarizers are available • Optional filters are available


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Selection chart

Picosecond laser sources: UV laser 375 nm NanoLED-11 Violet laser 405 nm NanoLED-07 Blue laser 440 nm NanoLED-10 Cyan laser 473 nm NanoLED-14 Red laser 635 nm NanoLED-02B Red laser 650 nm NanoLED-02 Red laser 670 nm NanoLED-02C NIR lasers 785 nm NanoLED-12A NIR lasers 830 nm NanoLED-12B NIR laser 1310 nm NanoLED-17

LED sources: UV 280 nm NanoLED-15 UV 340 nm NanoLED-16 UV 370 nm NanoLED-03 Blue 455 nm NanoLED-05A Blue 465 nm NanoLED-05B Aqua 485 nm NanoLED-01 Green 560 nm NanoLED-09 Amber 590 nm NanoLED-04 Orange 605 nm NanoLED-08 Red 625 nm NanoLED-06

For more information on the latest NanoLEDs available, see http://www.ibh.co.uk/products/lightsources/nanoled/nanoledsources.htm


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SpectraLED Introduction

SpectraLEDs are diode sources for phosphorescence and steady-state research. These slower-pulsed sources now extend the benefits of di-ode excitation to longer lifetime applications (e.g., phosphorescence and lanthanide de-cays) where they can be used as low-cost alternatives to xenon flashlamps and nitrogen lasers. SpectraLEDs are easy to use, requiring only +5 V power and TTL-compatible trigger pulses. Simply connect them directly to the Hub’s expansion port A. A PCI-bus controller card is also available.

Summary of features • Wavelengths from 372 nm to 625 nm • Standard minimum pulse-width with the DataStation Hub is 100 µs. • Mechanically and optically interchangeable with NanoLED sources • Each source contains built-in adjustable aspheric collection optics and bayonet

mounting flange • Connects directly to the DataStation Hub expansion port for plug-and-play opera-

tion


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FL-1065 Thermostatted Sampling Module and FL-1066 Upgrade

Specially designed for use under TCSPC conditions, the FL-1065 Thermostatted Sam-pling Module keeps a sample at a constant temperature from –20°C to +80°C. The tem-perature is maintained by an ethylene-glycol–water mixture pumped through from an external circulating temperature bath (not included). The holder also includes a magnetic stirrer, for mixing turbid or viscous samples.

HORIBA Jobin Yvon recommends the F-1000/1001 Temperature Bath for use with the FL-1065. If you already have the standard laser/NanoLED port on the sample compartment, con-sider the FL-1066 upgrade, which adds a thermostat temperature control and magnetic stirrer to the port.


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F-1000/1 Temperature Bath For studies of samples whose properties are temperature-dependent, use the F-1000/1 Temperature Bath with the FL-1065 Thermostatted Sampling Module. The controller circulates fluids externally, with tubes leading to the sample chamber. The temperature range is from –25°C to +150°C. Sensor and all cables are included with the F-1000/1. The Temperature Bath is available in a 110-V (F-1000) and 220-V (F-1001) version.

F-1000/1 Temperature Bath.


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TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Troubleshooting

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6: Troubleshooting Introduction

Because the FluoroMax®-3 with TCSPC has many user settings and adjustable parame-ters, 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 dis-tributor. Refer to the FluoroMax®-3 Operation Manual and the FluorEssence™ User’s Guide for help with troubleshooting problems in steady-state operation. For obvious trouble with the NanoLEDs or SpectraLEDs themselves, see their respective instruction manu-als. This chapter is intended to isolate and solve problems regarding operation of the TCSPC accessory with the system only.


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Basic troubleshooting steps When an apparent problem is first observed, follow the basic steps and suggestions out-lined below to troubleshoot the initial problem. In many cases, shutting down the sys-tem, carefully restarting, and redoing an experiment helps to remove an unseen or out-side 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 prob-lems 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 ac-cessories 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.


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Further assistance... 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 so-lution. 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 config-ured, and turned on as needed.

3 Following the instructions in System Operation, run a xenon-lamp scan and a water-Raman scan to make sure the system is properly cali-brated. Print the spectrum for each and note the peak intensities.

4 Check this chapter to see if the problem is dis-cussed.

5 Visit our web site at www.jobinyvon.com/fluor/fluor.htm. 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 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....


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The About FluorEssence window opens. Near the bottom are the FluorEssence™ and Origin® version numbers.

c Click OK 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) 494-8660 × 160.

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 De-partment at (732) 494-8660 × 160, fax us at (732) 549-5157, or e-mail Dr. David McLoskey at [email protected].

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Technical Specifications

7-1

7: Technical Specifications The TCSPC on FluoroMax® accessory consists of a sampling module with mounting for a light source, a host computer and monitor, a DataStation Hub controller for run-ning TCSPC lifetime mode, and DataStation software for TCSPC data-acquisition. Light sources are optional.

Spectrofluorometer system Specifications given herein are for the FluoroMax®-3 spectrofluorometer plus addi-tional components included in the TCSPC accessory and phosphorimeter upgrade. The steady-state system is controlled by FluorEssence™ software, while the lifetime por-tion of the system is controlled by DataStation software. Excitation sources

Xenon-lamp housing, containing:

• 150-W xenon, continuous output, ozone-free lamp.

• Optional phosphorimeter with UV xenon flash tube, and flash rate 0.05–25 Hz. Flash duration is 3 µs at FWHM. Low-intensity tail extends > 30 µs. Delay after flash is 50 ms to 10 s, in increments of 1 µs. Time interval between pulses should be ≥ 1 µs longer than interval between pulses. Flashes per data-point are 1–999. The sample window is 10 µs to 10 s, in increments of 1 µs.

Sample-compartment mount for:

One or more optional NanoLED sources:

• Interchangeable pulsed solid-state LEDs or laser-diodes, with fixed wavelengths from UV to near-IR. Flash duration < 200 ps (< 100 ps typical) for laser-diodes, ~ 1–1.5 ns for LEDs. Repetition rate up to 1 MHz.

One or more optional SpectraLED sources:

• Interchangeable pulsed solid-state LEDs, with fixed wave-lengths from UV to near-IR. Flash duration 100 µs to CW with DataStation Hub.

Optional third-party laser:

• Any Class 1 or 2 (IEC) or Class I or II (FDA) lasers or LEDs emitting visible or invisible radiation, with appropriate pulse-lengths for use in steady-state, TCSPC, or phosphorescence modes. Contact HORIBA Jobin Yvon about custom mounting in the system.

Dispersion 4.25 nm mm–1

Monochromators Single-grating excitation and emission spectrometers (standard).


7-2

Monochromators are f/3.5 Czerny-Turner design with classically-ruled gratings and all-reflective optics, using 1200-grooves/mm gratings:

Resolution 0.3 nm Maximum scan speed 200 nm s–1 Accuracy ±0.5 nm Step Size 0.0625–100 nm

Range 0–950 nm (physical) Gratings Excitation 330-nm blaze (220–600 nm optical range) Emission 500-nm blaze (290–850 nm optical range)

Sample module Sample module with excitation reference detector. The sample compartment also has a removable gap-bed assembly for sam-pling-accessory replacement. A special mount is available for il-luminating the sample with a NanoLED, SpectraLED, or third-party laser.

Optional front-face collection assembly available.

Heating and cooling (–20°C to +80°C) and variable-speed mag-netic stirrer available on the FL-1065. Uses an ethylene-glycol–water mixture. The recommended temperature bath with the FL-1065 is the F-1000/1.

Detectors • Calibrated photodiode for excitation reference correction from 200–980 nm.

• Emission detector is an R928P for high sensitivity in photon-counting mode (180–850 nm). High voltage = 950 V, linearity to 2 × 106 counts s–1, < 1000 dark counts s–1.

Steady-state sen-sitivity

Double-distilled, de-ionized, ICP-grade water-Raman scan 2500:1 S/N at 397 nm, 5-nm bandpass, 1-s integration time, background noise first standard deviation at 450 nm. 300 000 counts s–1 using these conditions.

Lifetime range • Standard TCSPC accessory, > 250 ps

• With enhancement kit 354186, > 100 ps

Excitation shut-ter

Computer-controlled

Optics Spectrofluorometer has all-reflective optics for focusing at all wavelengths and precise imaging for microsamples. Laser port has UV-grade fused-silica lenses.

0–950 nm (physical); 220–600 nm (optically) Excitation wave-length range 1200-groove/mm grating optimized for 330 nm

Emission wave-length range

0–950 nm (physical); 290–850 nm (optically)


7-3

Wavelength ac-curacy

0.5 nm

Minimum step size

0.0625 nm

Wavelength re-peatability

0.3 nm

Resolution 0.3 nm

Slit width 0–30 nm bandpass, continuously adjustable via host computer Integration time 1 ms to 160 s

Step size 0.0625–100 nm

Dimensions (in-strument)

32.5" wide × 10.5" high × 19" long 82.6 cm wide × 26.7 cm high × 48.3 cm long

Dimensions (sample com-partment only)

5.5" wide × 7" high × 7" long 14.0 cm wide × 17.8 cm high × 17.8 cm long

Weight 75 lbs (34 kg) Ambient tem-perature range

15–30°C (59–86°F)

Maximum rela-tive humidity

75%

Power 5 A, 120 V, 60 Hz; or 2.5 A, 240 V, 50 Hz single-phase AC

Phosphorimeter (FluoroMax®-P only) The following components and specifications also apply to the FluoroMax®-P. Source UV xenon flash tube Flash rate 0.05–25 Hz Flash duration 3 µs at full-width half-maximum. Low-intensity tail extends >

30 µs. Delay after flash 50 µs to 10 s, in increments of 1 µs. Flashes per data point

1–999

Sample window 10 µs to 10 s, in increments of 1 µs.


7-4

Note: Additional COM ports may be required to control accessories such as the MicroMax, temperature bath, etc.

Host computer Microprocessor/clock speed

Pentium IV or higher recommended, 2.4 GHz mini-mum

Operating system and en-vironment

Windows™ XP

Floppy drive 1.4 MB, 3½" floppy-disk drive.

Hard drive At least 80 GB of free storage.

CD-ROM drive Read-write capability, at least 40× maximum speed

Memory 512 MB RAM.

Video 1200 × 1600 resolution, 32-bit color, 64 MB video memory

Keyboard A 104-key keyboard, plus USB or PS/2 mouse

One parallel port for a dot-matrix printer

Two serial ports capable of 115 kilobaud for Fluoro-Max® and DataStation Hub

Ethernet 10/100/1000 interface

Available ports

Two free PCI slots. At least one of these must be full-size. If only one serial port is present, then there must be three PCI slots.

Software FluorEssence™ software for steady-state and optional phosphorescence data-acquisition and manipulation through the Windows™ environment. DataStation soft-ware for data-acquisition and manipulation in time-correlated single-photon-counting lifetime mode.

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Declaration of Conformity

8-1

8: Declaration of Conformity Manufacturer: HORIBA Jobin Yvon

Address: 3880 Park Avenue Edison, NJ 08820 USA

Product Name: TCSPC on FluoroMax

Model Number: FM-2013 Conforms to the following Standards:

Safety: EN 61010-1:2001 IEC 60825-1:2001

Supplementary Information The product herewith complies with the requirements of the Low Voltage Directive 73/23/EEC as amended by 93/68/EEC. The CE marking has been affixed on the device according to Annex III of the Low Voltage Directive 73/23/EEC. The technical file and other documentation are on file with HORIBA Jobin Yvon. ______________________________ Ray Kaminski Vice-President, Fluorescence Division HORIBA Jobin Yvon Edison, NJ 08820 USA October 28, 2005

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Declaration of Conformity

8-2

TCSPC on FluoroMax v. 1.0 (28 Oct 2005) Index

9-1

9: Index

3

354186 ............................................... 1-2, 7-2

5

570126 .......................................................1-2

6

61552 .........................................................1-2

8

81091 .........................................................1-2

9

973130 .......................................................1-2 973133 .......................................................1-2 98015 .........................................................1-2 98020 .........................................................1-2

A

About FluorEssence window .....................6-3 About FluorEssence... ............................6-3 accessories .................................................6-4

B

bandpass.................................................7-2–3 beam-block..................................... 1-2, 3-1–2 BNC ................................................... 1-2, 1-7

C

cables ................... 1-2–3, 1-6–7, 3-3, 5-7, 6-2 CE marking ................................................8-1 conflicts......................................................6-2

controller ................................................... 5-7 cuvette ........................................ 1-8, 2-1, 3-4 Czerny-Turner ........................................... 7-2

D

damage................................................0-3, 1-3 danger ........................................................ 0-3 dark counts ................................................ 7-2 DataStation Hub .1-1–2, 1-6–7, 2-1–2, 4-1, 5-

5, 7-1, 7-4 DataStation software 0-1, 2-1–2, 3-2, 7-1, 7-4 detector ...............................................1-3, 7-2 dimensions................................................. 7-3 dispersion................................................... 7-1 Drive connector......................................... 1-6

E

electrical requirements .............................. 1-1 enhancement kit...................................1-2, 7-2 ethylene-glycol ...................................5-6, 7-2

F

F-1000 ............................................5-6–7, 7-2 F-1001 ............................................5-6–7, 7-2 failure..................................................... 6-1–2 filters...................................................1-9, 5-3 FL-1057..............................................0-1, 1-2 FL-1061..................................................... 1-2 FL-1065..0-1, 1-2, 1-11, 2-1, 3-4, 4-1, 5-6–7,

7-2 FL-1066..................................................... 5-6 flash lamp ...........................................5-2, 7-3 FluorEssence™ software0-1, 1-2, 2-2, 3-1, 6-

3, 7-1, 7-4 FluoroMax®-3....... 0-1, 1-1, 2-2, 4-1, 6-1, 7-1 FluoroMax®-P ............................ 0-1, 5-2, 7-3 front-face accessory................................... 7-2


9-2

G

grating ....................................................... 7-2 ground ....................................................... 1-1

H

hazardous condition .................................. 0-3 help............................................................ 6-3 high voltage............................................... 0-3 hose-clamps............................................... 4-1 host computer............... 1-2, 1-4, 2-1, 7-1, 7-3

I

identification label .................................... 0-5 installation................................................. 1-3 integration time ..................................... 7-2–3

L

lamp scan .................................................. 6-3 laser radiation............................................ 0-3 laser-beam path ......................................... 0-6 laser-diodes ........................................ 2-1, 7-1 LEDs .................................................. 2-1, 7-1 lens ..........................................0-1, 1-8–9, 2-1 location...................................................... 1-3 Ludox® ........................................................ 1-8

M

magnetic stirrer ................... 2-1, 3-4, 5-6, 7-2 maintenance .............................................. 4-1 monochromator ......................................... 7-2

N

NanoLEDs0-1, 0-4, 0-6, 1-2, 1-5–6, 1-8–9, 2-1–2, 3-2–3, 4-1, 5-1, 5-3–5, 6-1, 7-1–2

NanoLED area.......................................... 1-6

O

OFF.................................................... 1-7, 3-2 OK button.................................................. 6-4

ON .............................................................3-1 optical blanking filter-plate .......................1-2 optics..........................................................7-2 Origin®.......................................................6-3

P

packing list.................................................1-4 performance test report..............................1-3 phosphorimeter ...................................5-2, 7-1 photodiode .................................................7-2 polarization ................................................1-9 polarizer................................ 1-2, 1-9–10, 5-3 power supply .........................................6-1–2

R

R928P ........................................................7-2 Raman........................................................7-2 recommended laser or LED sources..........0-6 reference detector ......................................7-2 relative humidity........................................7-3 resolution ...................................................7-3

S

S/N .............................................................7-2 sales order..............................................1-3–4 sample compartment...0-1, 0-5–6, 1-2, 1-5, 2-

1–2, 5-1, 5-6–7, 7-2–3 sample geometry........................................6-1 sampling module 0-5, 1-2, 1-5–6, 2-1, 4-1, 7-

1 serial number .............................................6-4 Service Department ........................6-1, 6-3–4 shutter ........................................................7-2 slits.............................................................7-3 specifications ......................................0-6, 7-1

computer ................................................7-4 phosphorimeter ......................................7-3 software .................................................7-4 spectrofluorometer system.....................7-1

SpectraLEDs.0-1, 0-4, 0-6, 4-1, 5-1, 5-5, 6-1, 7-1–2

symbols......................................................0-3 system configuration .................................6-4


9-3

T

TAC Start jack ..........................................1-7 TCSPC sticker............................................1-2 technical support ........................................6-3 temperature bath .......................... 1-11, 5-6–7 Thermostatted Sampling Module...........5-6–7 thumbscrew........................................ 1-6, 3-3 TO HUB jack.............................................1-7

U

unpacking...................................................1-3

V

version number ...................................... 6-3–4

W

warning label ......................................0-5, 1-5 water-Raman scan ..................................... 6-3 web site...................................................... 6-3 Windows™................................................ 7-4

X

xenon lamp ................................. 1-7, 3-1, 7-1 xenon-lamp housing .................................. 7-1


9-4

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