Applied Photophysics Chirascan Integrating Sphere User manual

Applied Photophysics Limited
21 Mole Business Park
Leatherhead
Surrey
KT22 7BA
United Kingdom
Tel: [phone]
Fax: [phone]
Email: [e-mail]
Applied Photophysics, Inc.
100 Cummings Center
Suite 440-C
Beverly
MA 01915
United States
Tel: [phone]
Email: [e-mail]
www.photophysics.com
User Manual
Chirascan Integrating Sphere

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Chirascan Integrating Sphere User Manual
This document contains important safety information. Read this document and the
Chirascan V100 Spectrometer User Manual before attempting to install or use the
Chirascan Integrating Sphere. Failure to do so could result in deathor serious injury.

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Chirascan Integrating Sphere User Manual
CONTENTS
USE OF THIS DOCUMENT ...............................................................................................................................4
HAZARD AND OTHER INDICATORS ...............................................................................................................5
ESSENTIAL SAFETY INFORMATION...............................................................................................................6
CHIRASCAN INTEGRATING SPHERE INSTALLATION AND OPERATIONAL REQUIREMENTS.................7
GLOSSARY........................................................................................................................................................8
1 INTRODUCTION.............................................................................................................................................9
2 INSTALLATION .............................................................................................................................................11
2.1 Preparing the Chirascan sample chamber .........................................................................................11
2.2 Installing the Integrating Sphere.........................................................................................................13
3 OPERATION..................................................................................................................................................16
3.1 Diffuse reflectance mode....................................................................................................................16
3.1.1 Typical use......................................................................................................................................... 16
3.1.2 Sample preparation........................................................................................................................... 16
3.1.3 Mounting the sample ........................................................................................................................ 16
3.1.4 Acquiring a spectrum ........................................................................................................................ 18
3.1.5 Example: D- and L-alanine................................................................................................................. 18
3.2 Transmission mode.............................................................................................................................20
3.2.1 Typical use......................................................................................................................................... 20
3.2.2 Sample preparation........................................................................................................................... 20
3.2.3 Mounting the sample ........................................................................................................................ 20
3.2.4 Acquiring a spectrum ........................................................................................................................ 22
4 MAINTENANCE AND STORAGE .................................................................................................................23
4.1 Maintenance .......................................................................................................................................23
4.2 Storage................................................................................................................................................23

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Chirascan Integrating Sphere User Manual
USE OF THIS DOCUMENT
This document is intended to inform the operator of Applied Photophysics Integrating Sphere on its design,
installation and operation with the Chirascan V100 Spectrometer. It is assumed that the user of this document
is familiar with the operation of the Chirascan spectrometer, and with Applied Photophysics Pro-Data software.
In particular it is assumed that the user is familiar with the hazards associated with the operation of the
spectrometer, and has read the safety information contained in its User Manual.
Sample preparation for the Integrating Sphere may require the use of a hydraulic press generating a pressure
of up to 10 tons and operating under high vacuum. It is assumed that the user has read the instruction manuals
supplied with the press and vacuum pump and is aware of the hazards associated with their use.
The information in this document is subject to change without notice and should not be construed as a
commitment by Applied Photophysics, who accept no responsibility for errors that may appear herein. This
document is believed to be complete and accurate at the time of publication, and in no event shall Applied
Photophysics be held responsible for incidental or consequential damages with or arising from the use of this
document.
COPYRIGHT 2018 APPLIED PHOTOPHYSICS LIMITED. ALL RIGHTS RESERVED. THIS DOCUMENT
OR PARTS THEREOF SHALL NOT BE REPRODUCED IN ANY FORM WITHOUT THE WRITTEN
PERMISSION OF THE PUBLISHER.
THE SOFTWARE PROVIDED WITH THE CHIRASCAN AND ITS ACCESSORIES (PRO-DATA CHIRASCAN,
PRO-DATA VIEWER, ETC.) IS THE PROPERTY OF APPLIED PHOTOPHYSICS LIMITED AND IS
SUPPLIED UNDER LICENSE. APPLIED PHOTOPHYSICS IS WILLING TO LICENSE THE SOFTWARE
ONLY UPON THE CONDITION THAT THE LICENSEE ACCEPTS ALL THE TERMS CONTAINED IN THE
LICENSE AGREEMENT. THESE INCLUDE THAT THE LICENSEE MAY NOT SELL, RENT, LOAN OR
OTHERWISE ENCUMBER OR TRANSFER LICENSED SOFTWARE IN WHOLE OR IN PART TO ANY
THIRD PARTY. FOR A FULL COPY OF THE LICENSE PLEASE CONTACT APPLIED PHOTOPHYSICS OR
SEE THE SOFTWARE INSTALLATION DISK.
Chirascan is a trademark of Applied Photophysics Limited.
All other trademarks or registered trademarks are the sole property of their respective owners

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Chirascan Integrating Sphere User Manual
HAZARD AND OTHER INDICATORS
HAZARD INDICATORS USED IN THIS DOCUMENT
The sign to the left is used to indicate a hazardous situation, which, if not avoided, could result
in death or serious injury.
The sign to the left is used to indicate a hazardous situation, which, if not avoided, could result
in minor or moderate injury.
OTHER INFORMATORY INDICATORS USED IN THIS DOCUMENT
The sign to the left is used to indicate a situation which, if not avoided, could result in damage
to the instrument.
HAZARD INDICATORS USED ON THE SPECTROMETER OR ITS ACCESSORIES
Note that these hazard indicators may be either colored as below or as black and white.
The sign to the left is a general hazard indicator, indicating the presence of a hazard that is either
described by text accompanying the sign or in this User Manual.
The sign to the left is a high voltage hazard indicator.
The sign to the left is a flammable hazard indicator

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ESSENTIAL SAFETY INFORMATION
MAKE SURE THAT YOU HAVE READ AND UNDERSTOODALL THE SAFETY INFORMATION CONTAINED
IN THIS DOCUMENT BEFORE ATTEMPTING TO INSTALL OR OPERATE THE INTEGRATNG SPHERE.
IF YOU HAVE ANY QUESTIONS REGARDING THE OPERATION OF THE ACCESSORY, PLEASE
CONTACT APPLIED PHOTOPHYSICS TECHNICAL SUPPORT AT THE ADDRESS SHOWN ON THE FIRST
PAGE OF THIS USER MANUAL
OBSERVE ALL SAFETY LABELS AND NEVER ERASE OR REMOVE SAFETY LABELS.
PERFORMANCE OF INSTALLATION, OPERATION OR MAINTENANCE PROCEDURES OTHER THAN
THOSE DESCRIBED IN THIS USER MANUAL MAY RESULT IN A HAZARDOUS SITUATION AND WILL
VOID THE MANUFACTURERS WARRANTY.
The photomultiplier tube (PMT) and Large Area Photodiode (LAAPD) detectors used with the
Chirascan Spectrometer operate at high voltages and can produce a shock leading to serious
injury or death. Do not connect or disconnect the detector from the spectrometer unless the
spectrometer is powered off.
Sample preparation for the Integrating Sphere may require the use of a hydraulic press
generating a pressure of up to 10 tons and operating under high vacuum. It is assumed that
the user has read the instruction manuals supplied with the press and vacuum pump and is
aware of the hazards associated with their use.
Disconnecting electrical components without powering off the spectrometer can cause
damage to the components. Power off the spectrometer before removing any accessories or
installing the Integrating Sphere.
The internal surface of the Integrating Sphere is coated with a highly reflective material and
the performance of the sphere will deteriorate if the surface becomes contaminated. Do not
touch the surface or the white parts of the reflective plug used when the sphere is operating in
transmission mode. Do not allow them to come into contact with other materials, and do not
attempt to clean them except by blowing gently with clean, dry air or nitrogen.
Avoid subjecting the Integrating Sphere to humid environments, or to extremes of temperature.
When not in use, the sphere should be stored in a clean, dry place.

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CHIRASCAN INTEGRATING SPHERE INSTALLATION AND OPERATIONAL
REQUIREMENTS
Environmental and electrical requirements
The Integrating Sphere has no environmental requirements additional to those of the Chirascan spectrometer.
Bench space
The Integrating Sphere has no bench space requirements additional to those of the Chirascan spectrometer.
Nitrogen purge gas
The recommended Integrating Sphere purge gas rate is 3 liters per minute; this gives a total recommended
purge gas rate to the spectrometer of 7 liters per minute.
Circulating water
The Integrating Sphere has no temperature control, and no requirement for circulating water
Servicing
Servicing of the Integrating Sphere should only be undertaken by qualified personnel. If you are in any doubt
at all please contact the Applied Photophysics Technical Support at the address given on the first page of this
User Manual.

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GLOSSARY
The following abbreviations may be found in this User Manual
CD circular dichroism
IR infrared
IS Integrating Sphere
UV ultraviolet
HYPERLINKS
This document contains hyperlinks between references (for example the Contents tables, or references to
Sections or Figures in the text), and sources. To follow a link, place the cursor over the reference and use
CTRL+click. Hyperlinks in the text are indicated by underlined blue font.

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Chirascan Integrating Sphere User Manual
1 INTRODUCTION
The Chirascan Integrating Sphere, shown in Figure 1.1, is designed to be used with the Chirascan V100
spectrometer.
Figure 1.1: the Integrating Sphere
Integrating spheres were developed early in the twentieth century, and were originally used to measure the
total output of a light source, without reference to the original direction of the light. They are now commonly
used when measuring the UV/visible or IR absorption spectra of solid samples, and their use can be extended
to the UV/visible CD spectroscopy of solids.
Light enters the sphere through an inlet port, and the white internal surfaces of the sphere are reflective and
diffuse, so that the light becomes equally distributed within the sphere through multiple scattering reflections.
A detector is placed at an outlet port and the intensity of the light is measured. For CD spectroscopy, the
sample can be placed either at the inlet port, so that the light passes through it before entering the sphere, or
at a point on the sphere opposite the inlet port, so that light is diffusely reflected from the sample after entering
the sphere.
These two operating modes are called respectively transmission and diffuse reflectance. In both cases the
sample is prepared in powder form. For transmission mode it must then be dispersed in either potassium
bromide or potassium chloride and compressed into a disc. For diffuse reflectance mode, it remains as a free
powder, if necessary dispersed in a diluent such as barium sulphate or polytetrafluoroethylene (PTFE).
The ideal integrating sphere should have as high an inner surface area as possible, with the ratio of the port
area to the total inner surface as low as possible. The Applied Photophysics Integrating Sphere has a diameter
of 100 mm, with the port sizes the minimum for light inlet and the detector active surface, giving a total reflective
surface of over 300 cm2. The inner surfaces of the sphere are coated with proprietary diffuse reflectance
material, although small areas around the ports are coated with barium sulphate.
A schematic of the Integrating Sphere is shown in Figure 1.2.

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Figure 1.2: schematic of the Integrating Sphere (top view).
The light enters at the light inlet port (Port A). In transmission mode it passes through the sample situated at
the light inlet port, while the diffuse reflectance port (Port B) is occupied by a reflective plug. In diffuse
reflectance mode the light inlet port is occupied by an aperture, and the sample is situated at the diffuse
reflectance port. In both cases the detector port (Port C) is occupied by the detector. The baffles are positioned
to prevent light entering the detector directly from the light inlet port or the sample, without diffuse reflectance.
Light, 
Port C
Port B
Port A
Detector
Baffle