Professional Documents
Culture Documents
User Manual
I 24319
3rd edition 2017, publication date March 2017
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hout our prior written permission. Brand names, registered trademarks etc. used in this
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trademarks law. They are the property of their respective owner.
This manual is the original documentation for the FT-IR microscope HYPERION.
Table of Contents
Table of Contents
1 Safety..............................................................................................................5
1.1 General safety information.................................................................................... 5
1.2 Classification of the safety notes ......................................................................... 5
1.3 Overview of possible types of hazard .................................................................. 6
1.3.1 Possible hazards during installation, operation, maintenance and repair ................ 6
1.3.2 Possible hazardous sample materials...................................................................... 7
1.4 Intended use ........................................................................................................... 8
1.5 Service contact data............................................................................................... 8
2 Installation......................................................................................................9
2.1 General information ............................................................................................... 9
2.2 Inspecting the packaging ...................................................................................... 9
2.3 Transporting the microscope................................................................................ 9
2.4 Scope of delivery.................................................................................................. 10
2.5 Site requirements ................................................................................................. 11
2.6 Connecting the microscope to the power supply ............................................. 13
2.6.1 General information................................................................................................ 13
2.6.2 Safety note ............................................................................................................. 13
2.6.3 Procedure............................................................................................................... 14
2.7 Cable connections ............................................................................................... 15
2.7.1 Overview of the connection sockets....................................................................... 15
2.7.2 Connecting the motorized microscope stage ......................................................... 17
2.7.3 Connecting the joystick .......................................................................................... 18
2.7.4 Connecting the video camera................................................................................. 18
2.7.5 Connecting the MCT detector(s) ............................................................................ 19
2.7.6 Connecting the FPA detector ................................................................................. 20
2.7.7 Connecting the microscope to the spectrometer.................................................... 22
2.8 Connecting the microscope to the purge gas supply line ............................... 23
2.8.1 General information................................................................................................ 23
2.8.2 Procedure............................................................................................................... 23
3 Overview.......................................................................................................25
3.1 Microscope variants............................................................................................. 25
3.2 Complete overview - operating elements & components................................. 26
3.3 Operating panel .................................................................................................... 29
3.4 Brightness control and brightness indicator .................................................... 30
3.5 Microscope stages ............................................................................................... 31
3.5.1 Overview ................................................................................................................ 31
3.5.2 Manual stage.......................................................................................................... 32
3.5.3 Focus control elements .......................................................................................... 33
3.5.4 Motorized stage...................................................................................................... 34
3.5.5 Joystick-controlled stage movement ...................................................................... 35
3.6 Condenser............................................................................................................. 36
3.7 Apertures............................................................................................................... 37
3.7.1 Overview................................................................................................................. 37
3.7.2 Installation locations of the apertures ..................................................................... 39
3.7.3 Manual knife-edge aperture.................................................................................... 40
3.7.4 Iris aperture for setting the Koehler illumination ..................................................... 41
3.8 Light path selector lever ...................................................................................... 42
3.9 Revolving nosepiece and objectives.................................................................. 43
3.10 Binocular ............................................................................................................... 45
3.11 LCD monitor.......................................................................................................... 46
3.12 Detectors ............................................................................................................... 47
3.12.1 Installation locations ............................................................................................... 47
3.12.2 Types of detector .................................................................................................... 48
3.13 Beam path ............................................................................................................. 49
3.14 Possible instrumental setups.............................................................................. 53
4 Operation......................................................................................................55
4.1 General information ............................................................................................. 55
4.2 Switching on / off the analysis system............................................................... 56
4.3 Preparing the microscope for a spectroscopic measurement......................... 58
4.4 Cooling the detector............................................................................................. 59
4.4.1 General information ................................................................................................ 59
4.4.2 Safety notes............................................................................................................ 59
4.4.3 Funneling liquid nitrogen in the detector................................................................. 60
4.5 Resetting the motorized stage ............................................................................ 62
4.6 Checking and correcting the condenser setting ............................................... 63
4.7 Checking the IR signal intensity ......................................................................... 66
4.7.1 Procedure in transmission mode ............................................................................ 66
4.7.2 Procedure in reflection mode.................................................................................. 68
4.7.3 Procedure with ATR objective ................................................................................ 72
4.8 Checking the detector saturation ....................................................................... 75
4.9 Viewing the sample and selecting the measurement area ............................... 77
4.10 Viewing and measuring a sample in transmission ........................................... 78
4.11 Viewing and measuring a sample in reflection.................................................. 82
4.12 ATR objective - Important operating notes ........................................................ 86
4.12.1 General handling instructions ................................................................................. 86
4.12.2 Cleaning the ATR crystal ........................................................................................ 86
4.12.3 Attaching the ATR objective at the revolving nosepiece......................................... 87
4.12.4 Setting the viewing mode / measuring mode at the ATR objective ........................ 88
4.12.5 Setting contact pressure levels............................................................................... 89
4.12.6 Focussing ............................................................................................................... 89
4.13 Measuring a sample with the ATR objective (single point measurement)...... 91
4.14 Measuring a sample with the ATR objective (mapping measurement) ........... 95
7 Troubleshooting ........................................................................................147
7.1 General information ........................................................................................... 147
7.2 Problem - possible cause - solution ................................................................. 148
7.2.1 Sample viewing through the binocular: No field of view or dark field of view ....... 148
7.2.2 No video image is displayed on the LCD monitor and/or in OPUS ...................... 149
7.2.3 No IR signal is detected or the detected IR signal intensity is too low ................. 150
7.2.4 IR signal check in OPUS shows an unusual spectrum curve shape .................... 153
7.2.5 Problems regarding the motorized microscope stage .......................................... 154
7.2.6 Problems regarding the ATR objective ................................................................. 155
7.2.7 Problems regarding mapping measurements....................................................... 157
7.2.8 Problems regarding the FPA detector .................................................................. 158
A Specifications ............................................................................................161
A.1 HYPERION microscope...................................................................................... 161
A.2 Objectives ........................................................................................................... 161
A.3 Motorized microscope stage ............................................................................. 162
A.4 Manual microscope stage.................................................................................. 162
A.5 Detectors ............................................................................................................. 163
A.6 Heating / freezing sample stage THMS600 (Linkam)....................................... 164
A.7 Heatable sample holder ..................................................................................... 165
D System diagram.........................................................................................173
➣ Read carefully all instructions and safety notes in this manual before installing,
putting the microscope into operation or maintaining it. Keep this manual for future
reference available at any time.
➣ Always observe the instructions and safety notes given in this manual. Failure to
do so can lead to personal injuries and/or property damage. Non-observance of
the instructions and safety notes will violate the intended use of the microscope.
(See section 1.4.)
➣ It is the operator's duty to plan and implement all necessary safety measures and
to supervise their observance. Moreover, the operator must ensure that the micro-
scope is in proper condition and fully functioning.
➣ A safe and trouble-free operation of the microscope is ensured only if all compo-
nents of the analysis system are installed and operated as well as maintained and
repaired according to the procedures described in this manual and in compliance
with all relevant safety standards and regulation.
➣ The microscope should be operated only by authorized personnel which is trained
in operating the microscope and which is familiar with the relevant safety instruc-
tions. Never remove or deactivate any supporting safety systems during micro-
scope operation. Objects and/or material not required for the operation should be
kept outside the operating area of the microscope.
➣ The microscope complies with the IEC/EN 61010-1 safety regulations.
Depending on the degree of hazard, important safety notes are classified in this manual
by signal words as follows:
WARNING
➣ Indicates a hazardous situation which, if not avoided, could result in death or seri-
ous (possibly irreversible) injury and major property damage.
CAUTION
➣ Indicates a hazardous situation which, if not avoided, may result in minor or mod-
erate (reversible) injury.
NOTE
➣ Hazard, which could result in material damage if the appropriate safety instruc-
tions are not observed.
Hazards that can possibly occur during installing, operating and repairing the micro-
scope are indicated by the appropriate warning labels on the microscope. The following
warning labels indicate different dangerous situations which may be occur by an
improper use of the analysis system:
Warning Definition
symbol
General hazard
This warning symbol indicates a general hazard area. Consult the man-
ual and inform yourself about the concrete nature of the hazard in ques-
tion. Observe the safety instructions and follow the precautions
described in the manual to avoid personal injury and/or property dam-
age.
Electrical shock hazard
This warning symbol indicates an electrical hazard. It is located near
live parts or on housings behind which are live parts that represent an
accidental contact hazard.
Do not touch these parts. Do not remove any housing part for which you
are not authorized. Ensure that all live parts do not come into contact
with a conductive substance or liquid.
Crushing hazard due to moving parts
This warning symbol indicates a crushing hazard caused by a moving
part. It is located near or on the moving part in question. Keep your
hands and other parts of the human body away from moving parts.
Potential source of hazard: motorized microscope stage
Danger of frostbite in case of skin contact with cryogenic sub-
stances
Exposure to cryogenic substances or cooled components causes frost-
bite effects. Handle these substances with utmost care. Observe the
safety instructions for operating with cryogenic liquids. Do not touch
cold parts.
Potential source of hazard: liquid nitrogen used for cooling the MCT
detector and FPA detector; heating / freezing sample stage THMS600
(Linkam)
Hot surface
This warning symbol indicates a risk of burn injuries caused by compo-
nents and surfaces which can become very hot during operation. Do
not touch these components and surfaces. Be careful when operating
near hot components and/or surfaces.
Potential source of hazard: heatable sample holder and heating / freez-
ing sample stage THMS600 (Linkam)
Important: All warning labels on the microscope must always be kept legible. Immedi-
ately replace a worn or damaged label!
There can also be hazards caused by the sample material. The following list contains
some examples of hazardous substances:
Symbol Definition
Infectious material
Radioactive material
Corrosive substances
Depending on the type of hazardous substances you work with, you have to observe the
specific substance-relevant safety instructions and regulations and take the correspond-
ing protective measures (e.g. wearing protective clothing, masks, gloves etc.). Affix the
corresponding warning label at the appropriate place at the microscope. The label must
be well legible and permanently discernible.
Waste disposal
Dispose all waste produced (chemicals, infectious and radioactively contaminated sub-
stances etc.) according to the prevailing laboratory regulations. Detergents and cleaning
agents must be disposed according to the special waste regulations.
The microscope HYPERION is intended for the microscopic examination and FT-IR
spectroscopic analysis of micro-samples, small sample areas and inhomogeneous sam-
ples. For the FT-IR spectroscopic analysis, the microscope needs to be coupled to a FT-
IR spectrometer of the TENSOR or VERTEX series. It is suited for all kinds of solid sam-
ples which absorb infrared light (radiation energy).
It is intended for the use in a laboratory under the environmental conditions specified in
appendix A.1.
The intended use includes also the compliance with the relevant standards and
regulations, especially:
• regional or national safety regulations
• regional or national accident prevention regulations
• generally recognized technical regulations
The intended use also includes the strict observance of all instructions given in this
manual, namely:
• safety instructions
• installation instructions,
• operation instructions
• repair and maintenance instructions
Use only components and accessories supplied by Bruker. For components and acces-
sories made by other manufacturers and used in conjunction with the microscope,
Bruker Optik GmbH does not assume any liability for safe operation and proper function-
ing.
WARNING
Health hazard because of unintended use of the microscope
Non-observance of the following safety instruction could result in injury and/or micro-
scope damage.
➣ Do not take any actions that violate the intended use. The operational safety of
the microscope is ensured only if it is used as intended.
In case you have questions about safety, installation and/or operation as well as repair
and maintenance of the analysis system or you need technical assistance in case of a
hardware and/or software problem, you can contact the Bruker service as follows:
• Service Hotline Hardware: +49 (0) 72 43 504-2020
• Service Hotline Software: +49 (0) 72 43 504-2030
• Fax: +49 (0) 72 43 504-2100
• E-Mail: service.bopt.de@bruker.com
service.bopt.us@bruker.com
☞ On our website www.bruker.com/about-us/offices/offices/bruker-optics you will
find also the current contact data of all Bruker Optics service offices worldwide.
The installation of the complete analysis system (i.e. microscope plus FT IR spectrome-
ter plus data station plus possible accessories) as well as the initial start-up and the site
acceptance test are done by the Bruker service. The operating company has to provide
an installation site that meets the site requirements described in section 2.5.
☞ See also the technical document Installation Requirements for IR-Microscope
HYPERION 1000 / 2000 / 3000 provided by Bruker Optik GmbH in advance of the
instrument delivery.
The installation of the microscope includes the following actions:
• connecting the microscope to the power supply
• connecting the microscope to the purge gas supply line (Not required, but highly
recommended.)
• connecting the microscope to a computer
• connecting the microscope to the FT IR spectrometer
☞ For detailed information about how to connect the FT-IR spectrometer, the computer
and peripherals, refer to the corresponding manuals.
➣ Important note: The operator can reconnect all cables if required, for example after
having relocated the analysis system. For information about the connections, refer
to the corresponding sections in this chapter.
After having received the microscope, inspect the packaging for damages. If there are
any signs of damage contact shipping company.
CAUTION
Possible damage to the delivered microscope because of transport
damage
Non-observance of the following safety instructions could result in injury.
➣ A microscope delivered in a damaged packaging may be damaged as well.
Therefore, in this case do not put the microscope into operation. Contact Bruker
instead. For the contact data, see section 1.5.
CAUTION
Injury and/or microscope damage due to an inadequate method of
transport
Non-observance of the following safety instructions could result in injury.
➣ For a short-distance, the microscope can be carried by at least two persons.
➣ For a long-distance, put the microscope on a wheeled table, for example. To avoid
damages, transporting the microscope in original packing is recommended.
a. The HYPERION microscope is available in three different variants: HYPERION 1000, HYPERION 2000 and
HYPERION 3000. For information about the available microscope variants, see section 3.1.
The operating company has to provide an installation site that meets the following site
requirements:
Possibilities of inter- The mains power supply of the microscope can be inter-
rupting the mains rupted as follows:
power supply: • by disconnecting the safety plug
• by switching off the microscope using the ON / OFF
switch at the microscope rear side
• disconnecting the primary power receptacle
➣ Important: When preparing the installation site, take
into account that the mains power supply connections
are easily accessible at any time.
Purge gas supply • dry air or nitrogen gas (dew point < -40°C corresponds to
requirements: a degree of dryness of 128ppm humidity)
• oil-free and dust-free purge gas
• max. pressure: 2 bar (29 psi)
• controllable flow rate (In case of continuous purging, the
recommended purge gas flow rate is 200 liters/hour. The
purge gas flow rate should not exceed 500 liters/hour.)
The microscope power supply is realized by an external power supply unit. The external
power supply unit plus power cord and low-voltage cable are included in the standard
delivery scope of the microscope.
☞ For information about the power supply requirements, see section 2.5.
i Depending on the local conditions, the original power cord may need to be exchanged
for a power cord that complies with the standards of the country in question. Ensure that
the installed power cord has the approval of the local authority (e.g. UL for US, CSA for
Canada or VDE for Europe).
CAUTION
Injury and/or property damage due to non-observance of the following
safety instructions regarding the external power supply unit
To ensure a safe operation of the external power supply unit, observe the following
safety instructions:
➣ If the external power supply unit is damaged disconnect it instantly from the sup-
ply circuit. Never put a damaged external power supply unit into operation! Only
authorized technicians are allowed to repair the external power supply unit!
➣ Operate the external power supply unit only in a dry environment.
➣ Make sure that the external power supply unit is not exposed to direct sunlight.
Avoid temperatures above +50 °C. Provide for sufficient air circulation.
➣ Position the external power supply unit in such a way that it does not present a trip
hazard.
➣ Do not put heavy objects on the external power supply unit.
➣ Do not place the external power supply unit on a hot surface.
2.6.3 Procedure
In case you intend to relocate the analysis system, this section provides information
about the cable connections. For connecting the data station, monitor etc., refer to the
corresponding computer manual.
B D
E
A
F
Microscope rear side - total view Microscope rear side - detail view
G H
Microscope
A Z-IN: socket for connecting the cable which comes from the stage motor
which drives the motorized stage in z-direction
➣ This cable is factory-connected to the stage motor.
B Z-OUT: socket for connecting the cable which is used for controlling the
motorized stage movement in z-direction
➣ The cable for controlling the motorized stage movement in z-direction
comes from the PC.
D DET.A: socket for connecting the signal transmission cable of the detector
in the left detector compartment (detector A).
➣ The detector signal is transmitted to the spectrometer.
E DET.B: socket for connecting the signal transmission cable of the detector
in the right detector compartment (detector B).
➣ The detector signal is transmitted to the spectrometer.
F EXT.SYNC.: socket for connecting the signal cable which comes from the
A/D converter box (A/D converter for detector signals)
➣ If the signal cable is connected to the EXT.SYNC socket and the
parameter External synchronization is activated in OPUS then the
user can start a spectroscopic measurement by pressing the START
button (H in fig. 3.4) on the control panel of the microscope.
Spectrometer
G external detector
PC
I FPA detector
K Joystick
☞ Regarding the PC and the spectrometer, the description in this manual is restricted
to only those sockets which are of relevance for connecting the microscope compo-
nents. For detailed information about the other sockets, refer to the corresponding
manual.
By default, the motorized microscope stage is equipped with two motors which allow for
a computer-controlled or a joystick-controlled stage movement in x- and y-direction.
Optionally, the stage can be equipped with a third motor which allows for a computer-
controlled or a joystick-controlled stage movement in z-direction.
The required cables are included in the delivery scope.
➣ Attention: Before connecting the joystick cable, make sure that the PC is switched
off. If the PC is switched on, connecting the joystick can cause unintentional stage
movements!
②
③
HYPERION 1000 and HYPERION 2000 can be equipped with at most two MCT detec-
tors; HYPERION 3000 with at most one MCT detector.
A B C D
A ON / OFF switch
C LED
Note: This LED lights green when the FPA detector is switched on.
④
The power is supplied by a dedicated
external power supply unit. Connect this
external power supply unit to a mains
socket outlet.
The microscope interior can be purged with dry air or dry nitrogen.
☞ For information about the purge gas supply requirements, see section 2.5.
The purge gas inlet is at the microscope rear side.
Note: The connection opening has a lock ring which prevents the hose
from being pulled out unintentionally.
2.8.2 Procedure
i The required hose is not included in the standard delivery scope of the microscope. It is
the operating company’s duty to provide a hose (PVC, outer diameter: 6 mm) of the
required length. Make sure that the hose is rated for the indicated operating pressure.
2 Connect the other end of the hose to the local purge gas supply line.
Important note: The connecting piece of the purge gas supply line has to be dimensioned
for the connection of a hose having an outer diameter of 6 mm.
Front view
G
B
A Control panel
D LCD monitor
E Binocular
F Video camera
D
F
B G
I
A
A Brightness control
D Visible light routing control (i.e. control element for routing the light either
to the video camera or to the binocular)
G Koehler aperture control (for opening and closing the iris aperture to set
the Koehler illumination in the reflection mode
F
D
A
G
D
F
C G
B H
G Detector temperature warning indicator: lights up red when the MCT detector tem-
perature exceeds its operating temperature. In case the microscope is equipped with
two MCT detectors, a red point lights up left or right in the display depending on
which detector has exceeded its operating temperature.
Note: In this case, the detector needs to be cooled with liquid nitrogen. For informa-
tion about how to cool the detector, see section 4.4.
H Start button: to start a spectroscopic measurement directly from the microscope
using the current measurement parameter settings in OPUS.
Note: Before pressing this button, make sure that either the IR button or VIS/IR but-
ton is activated, the OPUS software program is open and appropriate measurement
parameter settings are selected. (See appendix B in this manual and the OPUS Ref-
erence Manual.)
3.5.1 Overview
Manual stage
This type of stage is standard for the HYPERION 1000
variant. It can be moved in x-, y- and z-direction only man-
ually.
☞ For information about the manual stage operation,
see section 3.5.2.
With this stage, only single point measurements with the
current stage position are possible. Mapping measure-
ments at predefined x/y-stage positions are not possible.
Motorized stage
This type of stage is standard for the variants
HYPERION 2000 and HYPERION 3000.
By default, the motorized stage can be moved in x- and y-
direction by means of a joystick and the corresponding
OPUS functions. Optionally, a joystick- and computer-con-
trolled stage movement in z-direction is also possible.
☞ For information about a joystick-controlled stage
movement, see section 3.5.5.
☞ For information about a computer-controlled stage
movement, refer to the OPUS/VIDEO Manual and the
OPUS/MAP Manual.
With a motorized stage, spectroscopic mapping measure-
ments at predefined measurement positions are possible.
Important note: By default, the motorized stage is
equipped with two motors allowing for a motorized stage
movement in x- and y-direction. A joystick- and computer-
controlled stage movement in z-direction (focussing) is
only possible if the motorized stage is equipped with a
third motor. The third stage motor is an optional feature.
By default, the max. travel range in x- and y-direction is
50 mm x 75 mm.
☞ For information about optional stages and sample holders, see section 5.3.
B
D
A Rotary knob for moving the stage in x-direction: Using this knob, the stage is
moved to the left / to the right, assuming the operator stands in front of the micro-
scope.
B Rotary knob for moving the stage in y-direction: Using this knob, the stage is
moved backward / forward, assuming the operator stands in front of the microscope.
C Manual x/y-stage
Note: The sample has to be placed over the hole.
D Rotary knob for moving the stage in z-direction: Using this knob, the stage is
moved upward / downward for focussing purposes.
☞ More information about focussing, see section 3.5.3.
A C
B’
C’
A’
Figure 3.7: Focus control elements (upper image: right side view,
lower image: left side view)
B and B’ Coarse focus knob: Using this rotary knob, the distance between sample
and objective is changed in larger increments than with the fine focus con-
trol.
C and C’ Fine focus knob: Using this rotary knob, the distance between sample
and objective is changed in smaller increments than with the coarse focus
control.
➣ The coarse and the fine focus knobs are used for focussing in case of the following
types of stage: manual stage and motorized x/y-stage.
3.6 Condenser
C
A
D’
C’
Figure 3.9: Condenser (upper image: left side view, lower image: right side view)
B Condenser
☞ For detailed information about how to adjust the condenser, see section 4.6.
3.7 Apertures
3.7.1 Overview
E F
A Pinhole aperture: is used for checking the condenser adjustment (in transmitted
light microscopy)
☞ See section 4.6.
B Iris aperture for setting the Koehler illumination in transmission: This aperture
is opened and closed by a knurled ring which is located below the condenser.
➣ Attention: This aperture is in the IR-beam path. For this reason, do not forget
to open the aperture completely before starting a spectroscopic measurement!
E Iris aperture for setting the Koehler illumination in reflection: This aperture is
opened and closed by a lever.
☞ For information about how to operate this aperture, see section 3.7.4.
F Motorized knife-edge aperture: used for narrowing down the sample area to be
analyzed, i.e. sample areas which are not intended for spectroscopic analysis are
masked off by the aperture knife edges.
Note: The motorized knife-edge aperture is an option. It is installed instead of the
manual knife-edge aperture (D in fig. 3.10). It is operated exclusively by the OPUS/
VIDEO software.
☞ For information about how to operate the motorized knife-edge aperture, refer
to the OPUS/VIDEO Manual
This type of aperture consists of four knife edges which are arranged at right angles to
each other. This arrangement of the knife edges results in a rectangular aperture open-
ing with the two opposite knife edges forming a pair each.
A Thumbwheels: These two thumbwheels are used for realizing the following functions:
• increasing or reducing the distance between two opposite knife edges (i.e. setting
the size of the rectangular aperture opening)
• rotating the complete knife-edge aperture with the previously adjusted rectangular
aperture opening (rotation angle up to 360°)
Which of these two functions is actually realized depends on the current position of the
lever. (See B and C in fig. 3.11.)
B Lever in front position: When the lever is in the front position, the aperture can be
rotated by max. 360° using the thumbwheels (A in fig. 3.11). In this case, the previ-
ously set aperture opening size is locked and the knife-edge aperture is rotated. The
rotation center is identical with the center of the viewing field.
C Lever in back position: When the lever is in the back position, the distance between
two opposite knife edges (i.e. the size of the rectangular aperture opening) can be
increased or reduced using the two thumbwheels (A in fig. 3.11). In doing so, the size
of the rectangular aperture opening is set.
In reflection mode
This aperture (E in fig. 3.10) is used for setting the Koehler illumination in reflection
mode. The illumination intensity can be set in a stepless manner.
Lever
Figure 3.12: Operating element of the aperture for setting Koehler illumination in reflection mode
In transmission mode
This aperture (B in fig. 3.10) is used for setting the Koehler illumination in transmission
mode. It is located underneath the microscope stage. This aperture is opened and
closed by rotating the knurled ring.
Figure 3.13: Operating element of the aperture for setting Koehler illumination in transmission mode
➣ Important note: This aperture is situated in the IR beam path. For this reason, do not
forget to open this aperture completely before starting a spectroscopic measurement.
A
B
A Light path selector lever: Using this lever, the visible light is routed either to the
binocular or to the video camera.
The possible lever positions and their meaning are illustrated in the legend below
the light path selector lever. (See B and C in fig. 3.14.)
B If the lever is pushed in completely, the light is routed to the binocular. In this
case, the sample can be viewed only by looking through the binocular.
C If the lever is pulled out completely, the light is routed to the video camera. In this
case, the video image of the sample can be viewed on the LCD monitor at the front
side of the microscope and the PC monitor using the OPUS/VIDEO software pro-
gram. (Refer also to OPUS/VIDEO Manual.)
Note: The microscope variant HYPERION 1000 is not equipped with a LCD monitor.
Depending on the dimensions of the objectives, the revolving nosepiece allows for the
attachment of up to four objectives. Objectives with different magnifications and objec-
tives for special IR spectroscopic measurement techniques (e.g. ATR1, GIR2) are avail-
able.
B Objectives
Figure 3.15 shows the following objectives:
• 15x Schwarzschild objective (This objective is designed for both sample
viewing and IR spectroscopic measurements.)
• 4x glass objective (This objective can be used for sample viewing only.)
Note: These two objectives are included in the standard delivery scope.
For an overview of the optionally available objectives, see section 5.1.1.
C Two vacant positions: If not used, they are covered with caps.
Note: Before attaching an objective, remove the cap.
☞ For information about the optionally available objectives, see section 5.1.1.
Due to the dimensions of the objectives, only up to two objectives designed for IR mea-
surements and the 4x objective (for sample viewing only) can be attached at the revolv-
ing nosepiece at the same time. Opposite to the 15x objective, you can attach either the
36x objective or the ATR objective or the GIR objective. When attaching the ATR objec-
tive, you have to remove the plastic sleeve of the 15x objective first. The 36x objective or
the GIR objective cannot be attached to the nosepiece if there are already two other
large objectives (e.g. 15x objective and ATR objective). In this case, you have to remove
one of these two large objectives first.
3.10 Binocular
The following microscope variants are equipped by default with a high-resolution, color
LCD monitor: HYPERION 2000 and HYPERION 3000.
B C D E F
Figure 3.17: a) HYPERION 2000 (front side) b) Right microscope side- Operating elements of the LCD monitor
A LCD monitor: allows for a comfortable sample viewing of the video image in real
time.
Note: The sample can be viewed on the LCD monitor also during a IR spectro-
scopic measurement, providing that the VIS/IR mode (A in fig. 3.4) is activated.
B UP button and DOWN button: Use these two buttons to adjust the value of the
currently selected parameter (e.g. brightness, contrast etc.).
C Menu button: to open the menu for adjusting display parameters (e.g. brightness,
contrast etc.) for den LCD monitor.
3.12 Detectors
All microscope variants of the HYPERION series have two detector compartments. In
the left compartment, there is the standard MCT detector (single-element detector) cov-
ering a spectral range from 12,000 - 600 cm-1. Optionally, the right compartment can be
equipped with an second detector.
☞ The optionally available detectors are listed in section A.5.
A B A’ B’
A and A’ HYPERION 1000 / 2000 / 3000: left detector compartment housing the
standard MCT detector
MCT detector
The mid-band MCT detector is the standard detector
for all microscope variants of the HYPERION series.
This detector cover a spectral range from 12,000 -
600 cm-1.
In addition to the standard MCT detector, there are
other optional MCT detectors available which differ
from the standard detector with regard to spectral
range, detection sensitivity and hold time.
☞ See section A.5.
The MCT detector is a single-element detector (ele-
ment size: 0.25 mm x 0.25 mm).
This type of detector is designed for spectroscopic
measurements in the mid-infrared range.
FPA detector
The FPA detector can be installed in a
HYPERION 3000 microscope only.
The FPA detector is a multi-element detector. The avail-
able FPA detectors have a different number of detector
elements.
☞ See section A.5.
11
22
10
13a
14a
12
9
8 14b
13b
25
23 4 2
5 3
1
7 20
21
19
18
24
15
17 16
Figure 3.19: HYPERION 1000 and 2000 - Beam path in transmission mode and in reflection mode
11 22
10
13a
14a
12
9
8 14b
13b
25
23 4 2
5 3
1
7 20
19 21
18
24
15
17 16
Figure 3.20: HYPERION 3000 - Beam path in transmission mode and in reflection mode
2 Iris aperture for setting the Koehler illumination: to adjust the visible light intensity and
the contrast in the reflectance mode. The lever for adjusting the iris diameter is situ-
ated on the right side of the microscope (E in fig. 3.10).
6 Objective
7 Sample
8 Aperture (manual or motorized knife-edge aperture): to define the sample area for the
analysis (transmittance or reflectance mode).
17 Pinhole aperture for adjusting the condenser (in transmission mode only)
18 Iris aperture for setting the Koehler illumination in transmittance mode: to enhance
the image contrast
23 Optional polarizer (for reflectance mode): either for visible light only or for visible light
and IR light (two polarizers). An analyzer (component no. 25) is required in addition.
(It is part of the VIS polarizer.)
24 Optional polarizer (for transmittance mode): either for visible light only or for visible
and IR light (two polarizers). The IR polarizer (A675-P) requires the holder (A 675)
including the polarizer for visible light.
25 Optional analyzer: either for visible light only or for visible and IR light (two polarizers).
The HYPERION microscope is designed for the visualization and infrared spectroscopic
measurements of micro samples, small sample areas as well as the examination of
inhomogeneities in samples. For this purpose, the microscope needs to couple to a FT-
IR spectrometer of the TENSOR or VERTEX-series. (Note: Coupling the microscope to
an older Bruker spectrometer model might be possible as well.)
In case of a TENSOR spectrometer, the microscope can be coupled only to the right
spectrometer side. In case of a VERTEX spectrometer, the microscope can be coupled
only to the right as well as to the left spectrometer side.
In addition to the spectrometer, other optional accessories (e.g. external sample cham-
ber IMAC) can be coupled to the left or right IR-beam outlet port of the microscope.
Optionally, the IR-beam can be passed through the microscope to further accessories.
Depending on the demands made on the analysis system by the application, a large
variety of different instrumental setups with the HYPERION microscope is possible.
Figure 3.21 shows some examples thereof.
Figure 3.21: Examples of possible instrumental setups with the HYPERION microscope
Before you start to work with the HYPERION microscope for the first time, it is
highly recommended to familiarize yourself with the operating elements of the
microscope and the relevant OPUS functions.
how to validatea the analysis system (i.e. Procedure Guide OVP Test Procedure
FT IR spectrometer plus HYPERION Guide and VALIDATION Manualb
microscope) For general information about OVPc refer
to the OPUS Reference Manual.
a. Validating means performing a PQ test (Performance Qualification) and/or an OQ test (Operational Qualifi-
cation) using OVP.
b. This VALIDATION Manual is only included in the delivery scope of a validated analysis system.
c. OVP - OPUS Validation Program (It is integral part of the OPUS software.)
3. Cooling down the FPA detector with liquid nitrogen to its operating tempera-
ture
☞ See section 4.4
➣ Important note: After each reboot of the PC, you have to switch off the FPA detec-
tor and then to switch on again. Before switching on the FPA detector, make sure
that the FPA detector is cooled down to its operating temperature. For information
about how to cool down the FPA detector, see section 4.4.
After having switched the analysis system and before starting your sample analyses,
you have to do the following preparatory works:
Checking whether the detector is cooled Note: The detector temperature warn-
down to its operating temperature. If not, ing indicator (G in fig. 3.4) is situated
cool down the detector using liquid nitro- on the operating panel of the micro-
gen. scope. If it lights up red, the detector in
question needs to be cooled down.
☞ For information about how to cool
down the detector, see section 4.4
Resetting the motorized microscope stage The motorized stage is reset using the
to its home position (i.e. x=0; y=0). corresponding OPUS function.
Note: Skip this step if the microscope is ☞ For information about how to reset
equipped with a manual stage. the motorized stage, refer to the
OPUS/VIDEO Manual and/or the
OPUS/MAP Manual.
Checking the condenser setting and cor- ☞ For information about how to
recting it, if required. adjust the condenser, see
section 4.6.
Note: This is only in the transmission mode
of relevance.
The operating temperature of the available MCT detectors and FPA detectors is signifi-
cantly below room temperature. A low detector temperature ensures an optimum signal
detection. To achieve the required operating temperature, the detector needs to be
cooled down by funneling liquid nitrogen into the detector. Depending on the nominal
hold time1 of the detector in question, the cooling procedure needs to be repeated in
regular time intervals.
When the cooling effect of the liquid nitrogen decreases and the detector temperature
exceeds a certain value, the detector temperature warning indicator (G in fig. 3.4) on the
operating panel of the microscope lights up red. Other indications of a weakened or dis-
appeared cooling effect are a low signal intensity or no detected signal at all. In case no
signal is detected, the OPUS status lamp turns to red. This problem is also indicated by
the following instrument status message in OPUS: Detector not ready.
☞ For information about how to check the signal intensity, see section 4.7.
The liquid nitrogen is poured in using the supplied funnel. The funnel is inserted in the
corresponding opening on the top side of the detector compartment. The microscope is
delivered with this opening being closed by a plug.
WARNING
Injury due to improper handling of liquid nitrogen
Non-observance of the following safety instructions may result in an injury.
➣ Risk of frostbites! Avoid any skin contact!
➣ Protect yours eyes against extremely cold gases! Wear a suitable eye or
face protection! Also the gases escaping from the liquid nitrogen are extremely
cooled and can cause frostbites. The delicate eye tissue can be damaged if
exposed to these cold gases even for a short time. Protect your eyes by wearing a
face shield or safety goggles. Attention: Goggles without side shields do not pro-
vide sufficient protection.
CAUTION
Risk of asphyxiation due to lack of oxygen
Non-observance of the following safety instructions may cause health problems.
➣ Use liquid nitrogen only in well-ventilated areas! High nitrogen gas concentra-
tions in an enclosed area can cause asphyxiation! Note: Nitrogen gas is colorless,
odorless and tasteless. Therefore, it can not be detected by human senses and
will be inhaled as if it were normal air.
1. The hold time indicates how long the cooling effect of the liquid nitrogen lasts. The available MCT detectors
have different nominal hold times: 8, 12 and 24 hours.
The procedure is identical for both types of detector - MCT and FPA.
CAUTION
Liquid nitrogen boils and splashes at first when it is poured in a warm container. Especially
at the beginning when die temperature difference between detector dewar and liquid nitro-
gen is still very large, the liquid nitrogen may squirt out forcefully. Therefore observe the
2 following safety note to avoid frostbites:
➣ Pour the liquid nitrogen slowly in the funnel to minimize boiling and splashing.
➣ Stand clear of boiling and splashing liquid nitrogen and escaping gases. Wear
suitable protective goggles or a face shield.
➣ Be aware that liquid nitrogen can squirt out of the detector dewar from time to
time during the entire filling process.
Wait until the funnel is empty before refilling it. When the liquid nitrogen stops streaming
out, the detector dewar has cooled down to liquid nitrogen temperature. Then, pour again
some liquid nitrogen in the funnel.
Repeat this procedure until the dewar is filled to maximum. As a rough rule of thumb for
the MCT detector: the maximum capacity is about the quantity of two to three funnel fill-
ings. Note that the first two funnel fillings will evaporate almost completely at the begin-
ning.
Avoid overfilling the dewar! Otherwise the liquid nitrogen flows out.
After having poured in sufficient liquid nitrogen, remove the funnel and reinsert the plug in
3
the filling hole.
➣ Wait about 20 minutes before starting the first spectroscopic measurement to allow
4
the detector to stabilize thermally.
• Always cool down the FPA detector with liquid nitrogen first. Then switch on the
detector. This sequence of actions is necessary to ensure a trouble-free opera-
tion of he FPA detector.
• When the FPA detector is switched on, the nominal hold time is 8 hours. When it
is switched off the nominal hold time is 12 hours. For this reason it is advisable to
switch off the FPA detector if it is not in use.
➣ Note: The ON/POFF switch of the FPA detector is at the bottom side of the right
detector comportment.
☞ The motorized microscope stage is reset using the corresponding OPUS functions.
For information about how to rest the stage, refer to the OPUS/VIDEO Manual and
the OPUS/MAP Manual.
• Stage reset means that the stage moves to its home position (x-position =0 and
y-position =0). The motorized stage is resettable only x- and y-direction, but not
in z-direction.
• The motorized stage needs to be reset after each PC reboot!
• Precondition for resetting the motorized stage: When setting up the mapping
device and the imaging device, make sure that the correct stage (lstepMICstage)
has been selected. (Note: In case motorized stage is to be used for mapping
measurement with the ATR objective, make sure that the stage option lste-
pATRMICstage is selected as well.
➣ Attention: Before starting the stage reset, make sure that the current condenser
height and the current stage height allow for a hindrance-free stage movement. If
not, move the condenser slightly downwards and/or the stage upwards. Otherwise
the condenser may hinder the stage from reaching its home position. If the stage
does not succeed in reaching its home position due to a hinderance switch off the
PC to abort the reset process.
NOTE
Risk of damaging the ATR objective crystal
The ATR objective crystal can get damaged due to mechanical impact (e.g. shock).
To avoid an ATR crystal damage, observe the following notes when resetting the
motorized stage:
➣ In case the ATR objective is in the beam path, make sure that there is noting on
the stage (e.g. a sample lying on the stage) which could hit against the ATR crys-
tal when the stage moves to its home position
➣ Swing the ATR objective out of the beam path.
CAUTION
Risk of crushing the fingers
Non-observance of the following notes may lead to minor injuries.
➣ When the stage is moving, make sure that your hands and other parts of the
human body are not in the movement range of stage, especially when you control
the stage by the OPUS software or by the joystick. Otherwise there is a potential
risk of crushing the fingers.
Before you start with the signal intensity check in the transmission mode, it is advisable
to check the condenser setting first and correct it, if required.
Make sure that the beam path is not obstructed, for example by a polarizer, a
2 sample or a closed knife-edge aperture (i.e. the knife-edge aperture has to be
open completely).
Activate the viewing/measur-
ing mode by using the VIS/IR-
button ② on the operating
3 panel.
②
Activate the transmission
③
mode by using the corre-
sponding button ③ on the
4 operating panel.
Before starting the spectroscopic sample analyses, it is advisable to check the detected
IR signal intensity. The precious procedure depends on the measurement technique
(transmission, reflection, ATR) you intend to apply.
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a
3
closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Amplitudenwert im
Transmissionsmodus
If there is not any IR signal detected or if the amplitude value displayed in OPUS deviates
significantly from the amplitude value of the supplied OVP test protocol, see section 7.2
for possible causes and troubleshooting solutions.
6 Note: A detected amplitude value above 32.000 is an indication of an oversaturated
detector. In this case you first have to reduced the signal intensity until the detector is no
longer oversaturated. For information about how to reduce the signal intensity, see
section 4.8.
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a
2
closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Activate the viewing mode by actuating
③
the VIS button ② on the operating panel
of the microscope.
Activate the reflection mode by actuating
3
the corresponding button ③ on the
operating panel of the microscope.
②
4 Place the supplied gold mirror on the microscope stage underneath the objective.
Make sure that the light path selector
lever ④ is pushed in completely, i.e. the
④ light is routed to the binocular.
8 ➣ The precious procedure depends on whether you work with a validated or a non-
validated analysis system and wether the HYPERION microscope is equipped with a
manual knife-edge aperture (standard) or a motorized knife-edge aperture (option).
Amplitudenwert im
Reflexionsmodus
If there is not any IR signal detected or if the amplitude value displayed in OPUS deviates
significantly from the amplitude value of the supplied OVP test protocol, see section 7.2
for possible causes and troubleshooting solutions.
12 Note: A detected amplitude value above 32.000 is an indication of an oversaturated
detector. In this case you first have to reduced the signal intensity until the detector is no
longer oversaturated. For information about how to reduce the signal intensity, see
section 4.8.
☞ Important: First become thoroughly familiar with the ATR objective. For infor-
mation about how to operate the ATR objective, see section 4.12.
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a
2
closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Activate the reflection mode by actuating
②
the corresponding button ② on the
operating panel of the microscope.
3
ATR crystal
in the lower
position
Contact
pressure
level display
Amplitude value
with ATR objective
If there is not any IR signal detected or if the amplitude value displayed in OPUS deviates
significantly from the amplitude value of the supplied OVP test protocol, see section 7.2
for possible causes and troubleshooting solutions.
12 Note: A detected amplitude value above 32.000 is an indication of an oversaturated
detector. In this case you first have to reduced the signal intensity until the detector is no
longer oversaturated. For information about how to reduce the signal intensity, see
section 4.8.
General information
Especially when you measure in transmittance or when you measure highly reflecting
samples in reflectance, it is advisable to check the detector saturation before each mea-
surement. If the detector is oversaturated, the IR spectroscopic measurement may not
yield meaningful results.
Procedure
Enlarged section
Enlarged section
With the HYPERION microscope, you can view the sample through the binocular, on the
LCD monitor at the microscope front side (except for HYPERION 1000) and in the OPUS
video view on the PC monitor.
For examining the sample using the microscope and selecting the measurement area you
intend to analyze spectroscopically, you have to carry out the following actions:
1. Activating the viewing mode (VIS): You can activate the VIS mode either by actuat-
ing the VIS button on the operating panel of the microscope or by using the OPUS/
VIDEO software.
2. Activating the measuring method - transmission or reflection: You can activate
the measuring method either by actuating the corresponding button on the operating
panel of the microscope or by using the OPUS/VIDEO software. The measuring
method is determined by the physical nature of the sample (e.g. transparent or reflect-
ing).
3. Deciding whether you want to view the sample through the binocular or the video
image on the monitor using the light path selector lever
4. Putting the sample on the microscope stage and positioning it in the beam path
(Possibly, the condenser needs to be reset, e.g, if the sample is on a transparent sub-
strate material.)
5. Swinging an objective with a suitable magnification in the beam path: Note: Nor-
mally use the 15x IR-objective for viewing the sample and searching for areas of inter-
est. In case of a large sample, you can use also an objective with a lower
magnification, e.g. 4x objective. Attention: The 4x objective is a VIS-objective, i.e. it
cannot be used for spectroscopic measurements. For spectroscopic measurements,
use only IR-objectives (e.g. 15x IR-objective or 20x ATR-objective)!
6. Focussing on the sample: Make that the sample on the stage or the stage itself
does not hit the objective while you move the stage upwards for focussing purposes.
7. Setting the brightness: Set the brightness in such a way that the sample in question
is illuminated optimally. Always start with a low brightness level and increase it step-
wise. (Note: The currently set brightness level is indicated by the brightness indica-
tor at the microscope control panel. See fig. 3.4.)
➣ Attention: Do not look through the binocular when the brightness is set at maximum.
Temporary eye irritations may occur. In this case, close your eyes for about one
minute until the irritation has disappeared.
8. Optimizing the image contrast: using the iris aperture for setting the Koehler illumi-
nation. Which of the two apertures of this type you have to use depends on the mea-
suring method (transmission or reflection).
➣ Note: Opening or closing this aperture has an effect on the brightness. BUT: Do not
use this aperture to set the brightness but use the thumb wheel for controlling the
brightness (B in fig. 3.5) instead! With the brightness control, the microscope lamp
voltage is changed. This has an effect on the color temperature.
9. Moving the microscope stage in x- and/or y-direction until you find a sample area
which is of interest to you and which you intend to analyze spectroscopically.
10. Masking off that sample area which is not intended for spectroscopic analysis
using the knife-edge aperture.
➣ In case of a manual knife-edge aperture, the aperture setting is not registered by the
software. Therefore, it is advisable to take a snapshot of the video image in order to be
able to reconstruct the aperture setting later, if required. (For information about how to
take a snapshot, refer to the OPUS/VIDEO Manual. For taking a snapshot of the cur-
rent knife-edge aperture setting it is important that the currently used objective and
the objective selected in OPUS are identical.
1. Activate the viewing mode. either the VIS button on the operating
panel (B in fig. 3.4) or in the OPUS
video wizard
☞ See OPUS/VIDEO Manual.
2. Activate the reflection mode. either the reflection mode button on the
operating panel (E in fig. 3.4) or in the
OPUS video wizard
☞ See OPUS/VIDEO Manual.
5. Set the microscope either for sample Light path selector lever (A in fig 3.14)
viewing through the binocular or for video
image display.
Note: It is recommended to use the video
image displayed on the monitor.
6. Adjust the brightness starting with a either the thumb wheel of the bright-
low brightness level. ness control at the microscope (B in
Caution: Do not look through the binocu- fig. 3.5) or the brightness control in the
lar when the brightness is set at maxi- OPUS video wizard
mum. Temporary eye irritations may The currently set brightness is dis-
occur. played by the brightness indicator (A in
fig. 3.5).
8. Enhance the image contrast by closing Iris aperture for setting the Koehler illu-
the iris aperture for setting the Koehler mination (B in fig. 3.10)
illumination in transmission. Knurled ring underneath the condenser
Attention: Do not forget to reopen this
aperture before starting a spectroscopic
measurement!
10. Move the stage in x- and/or y-direc- Manual x/y-stage: Rotary knobs (A
tion to find a sample area which is of and B in fig. 3.6)
interest to you. Motorized x/y-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
12. Mask off that sample area which is Manual knife-edge aperture (D in
not intended for spectroscopic analysis. fig. 3.10 and fig. 3.11)
Motorized knife-edge aperture (F in
fig. 3.10) This aperture is operated by
the corresponding OPUS functions.
☞ See OPUS/VIDEO Manual.
15. Move the stage in x- and/or y-direc- Manual x/y-stage: Rotary knobs (A
tion until a sample-free area of the sub- and B in fig. 3.6)
strate is in the beam path. Motorized x/y-stage: Joystick and cor-
Note: Make sure that the detector does responding stage control functions in
not oversaturate. Do not change the set- OPUS
ting of the knife-edge aperture! ☞ See OPUS/VIDEO Manual.
16. Move the pinhole aperture in the Thumb wheel of the pinhole aperture
beam path. If required, correct the con- for setting the condenser (A in fig. 3.9),
denser setting. Note: When you see a condenser focussing knobs (C/C’ in
sharp image of a bright circle which is fig. 3.9) and centering screws (D/D’ in
aligned to the center of the cross hairs, fig. 3.9)
then the condenser is set correctly. After- ☞ See section 4.6.
wards, move the pinhole aperture out of
the beam path again.
17. Activate the measuring mode. either using the IR button on the oper-
ating panel of the microscope (C in
fig. 3.4) or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
19. Move the stage in x- and/or y-direc- Manual x/y-stage: Rotary knobs (A
tion to return to the sample area, you and B in fig. 3.6)
have chosen in step 10. Motorized x/y-stage: Joystick and cor-
In case of a motorized stage, return the responding stage control functions in
stage to the x/y-position, you have saved OPUS
in step 14. ☞ See OPUS/VIDEO Manual.
20. Check again the condenser setting. If Thumb wheel of the pinhole aperture
required, readjust the condenser height. for setting the condenser (A in fig. 3.9)
and the condenser focussing knobs (C/
C’ in fig. 3.9)
☞ See section 4.6.
1. Activate the viewing mode. either the VIS button on the operating
panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
2. Activate the reflection mode. either the reflection mode button on the
operating panel (E in fig. 3.4) or in the
OPUS video wizard
☞ See OPUS/VIDEO Manual.
5. Set the microscope either for sample Light path selector lever (A in fig 3.14)
viewing through the binocular or for
video image display.
Note: It is recommended to use the
video image displayed on the monitor.
6. Adjust the brightness starting with a either the thumb wheel of the brightness
low brightness level. control at the microscope (B in fig. 3.5)
Caution: Do not look through the bin- or the brightness control in the OPUS
ocular when the brightness is set at video wizard
maximum. Temporary eye irritations The currently set brightness is displayed
may occur. by the brightness indicator (A in fig. 3.5).
8. Enhance the image contrast. Lever for operating the iris aperture for
setting the Koehler illumination in reflec-
tion (fig. 3.12 and E in fig. 3.10)
9. Move the stage in x- and/or y-direc- Manual x/y-stage: Rotary knobs (A and
tion to find a sample area which is of B in fig. 3.6)
interest to you. Motorized x/y-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
11. Mask off that sample area which is Manual knife-edge aperture (D in
not intended for spectroscopic analysis. fig. 3.10 and fig. 3.11)
Motorized knife-edge aperture (F in
fig. 3.10) This aperture is operated by
the corresponding OPUS functions.
☞ See OPUS/VIDEO Manual.
15. Activate measuring mode. either using the IR button on the operat-
ing panel of the microscope (C in
fig. 3.4) or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
17. Activate viewing mode. either the VIS button on the operating
panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
18. Return to the sample area you have Manual x/y-stage: Rotary knobs (A and
chosen in step 9 for spectroscopic anal- B in fig. 3.6)
ysis. Motorized x/y-stage: Joystick and cor-
In case of the manual stage, move the responding stage control functions in
stage in x- and/or y-direction until you OPUS
have found the sample area in question
☞ See OPUS/VIDEO Manual.
again.
In case of a motorized stage, return
the stage to the x/y-position, you have
saved in step 13.1.
21. Activate measuring mode. either using the IR button on the operat-
ing panel of the microscope (C in
fig. 3.4) or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
➣ Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
The ATR crystal is fragile. To prevent the ATR crystal from getting damaged, observe the
following handling instructions when working with the ATR objective:
Note
Risk of damaging the ATR crystal
➣ Handle the ATR objective with utmost care. Prevent the ATR crystal tip from fitting
the microscope stage. Especially in the following situations, be aware of the
potential risk of damage:
• attaching the ATR objective to the revolving nosepiece or removing the ATR
objective from the revolving nosepiece,
• swinging the ATR objective in the beam path with the microscope stage being
set too high,
• moving the microscope stage upwards to focus on the sample and
• pulling down the outer casing of the ATR objective to bring the ATR crystal in
the measuring position and/or set a certain contact pressure level.
➣ Using the ATR objective, the sample temperature should not exceed 40°C. In
case of a higher sample temperature, the ATR crystal may become detached.
Before each measurement, check whether the ATR crystal is clean (i.e. free of any parti-
cles from the previous sample). Residuals of the previous sample may lead to falsified
results.
Clean the ATR crystal using a lint-free cloth and a suitable solvent (e.g. ethanol, isopro-
pyl), if required.
Attach the ATR objective opposite to the 15x objective at the revolving nosepiece.
Before attaching the ATR objective, remove the plastic sleeve of the 15x objective. In
case there is another IR objective (e.g. 36x objective) attached at the nosepiece, remove
it before you attach the ATR objective.
To remove the ATR objective from the nosepiece, first disconnect the cable than detach
the objective.
4.12.4 Setting the viewing mode / measuring mode at the ATR objective
Viewing mode
ATR-crystal in
lower position
The measurement technique ATR requires an intimate contact between ATR crystal and
sample to obtain meaningful sample spectra. In case of the ATR objective, the optimal
contact pressure is obtained by pressing the ATR crystal against the sample with a pres-
sure that is adequate to the degree of hardness of the sample. Five different pressure
levels can be set: pressure level 1 (contact pressure: 0.5 N) for very soft samples up to
pressure level 5 (contact pressure: 8 N) for very hard samples.
4.12.6 Focussing
In viewing mode
Proceed as follows:
1. Bring the ATR crystal in the viewing mode position (i.e. upper position). See
section 4.12.4.
2. Focus on the sample by moving the stage slowly upwards.
➣ Attention: When moving the stage upwards, take care the ATR crystal tip does not
hit the stage. Potential risk of damaging the ATR crystal!
In measuring mode
Proceed as follows:
Bring the ATR crystal in the measuring mode position (i.e. lower position).
1
☞ See section 4.12.4.
Set a contact pressure level which is adequate to the degree of hardness of the
2 sample you intend to analysis.
☞ See section 4.12.5.
1. Activate the viewing mode. either the VIS button on the operating
panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
2. Activate the reflection mode. either the reflection mode button on the
operating panel (E in fig. 3.4) or in the
OPUS video wizard
☞ See OPUS/VIDEO Manual.
5. Set the microscope either for sam- Light path selector lever (A in fig 3.14)
ple viewing through the binocular or for
video image display.
Note: It is recommended to use the
video image displayed on the monitor.
6. Move the stage in x- and/or y-direc- Manual stage: Rotary knobs (A and B in
tion to find a sample area which is of fig. 3.6)
interest to you. Motorized stage: Joystick and corre-
sponding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
9. Exchange the sample for the plastic Note: The plastic ring is included in the
ring. Place the plastic ring underneath delivery scope of the ATR objective.
the ATR objective.
11. Activate the measuring mode at either using the IR button on the operat-
the microscope. ing panel of the microscope (C in fig. 3.4)
or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
12. Move the stage slowly upwards Manual stage and motorized x/y-
until the ATR crystal is in the focus stage: coarse and fine focus knobs at
position. the microscope (B/B’ and C/C’ in fig. 3.7)
Note: The focus position is indicated Motorized x/y/z-stage: Joystick and cor-
acoustically by a beep and optically by responding stage control functions in
the In-focus LED. When the ATR crys- OPUS
tal has reached the focus position, the ☞ See OPUS/VIDEO Manual.
In-focus LED turns from red to green
☞ See also section 4.12.6.
for a short moment. Then it goes off.
14. Move the stage downwards as far Manual stage and motorized x/y-
as it will go. Exchange the plastic ring stage: coarse and fine focus knobs at
for the sample. the microscope (B/B’ and C/C’ in fig. 3.7)
Motorized x/y/z-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
16. Activate the viewing mode at the either the VIS button on the operating
microscope. panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
17. Focus on the sample by moving Manual stage and motorized x/y-
the stage slowly upwards. stage: coarse and fine focus knobs at
the microscope (B/B’ and C/C’ in fig. 3.7)
Motorized x/y/z-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
18. Find a sample area which you Manual stage: Rotary knobs (A and B in
intend to analyze spectroscopically by fig. 3.6)
moving the stage in x- and/or y-direc- Motorized stage: Joystick and corre-
tion. sponding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
19. Move the stage downwards as far Manual stage and motorized x/y-
as it will go. stage: coarse and fine focus knobs at
the microscope (B/B’ and C/C’ in fig. 3.7)
Motorized x/y/z-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
21. Activate the measuring mode at either using the IR button on the operat-
the microscope. ing panel of the microscope (C in fig. 3.4)
or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
22. Move the stage slowly upwards Manual stage and motorized x/y-
until the ATR crystal tip contacts the stage: coarse and fine focus knobs at
sample and the ATR crystal is pressed the microscope (B/B’ and C/C’ in fig. 3.7)
in the focus position. Motorized x/y/z-stage: Joystick and cor-
Note: The focus position is indicated responding stage control functions in
acoustically by a beep and optically by OPUS
the In-focus LED. When the ATR crys-
☞ See OPUS/VIDEO Manual.
tal has reached the focus position, the
☞ See also section 4.12.6.
In-focus LED turns from red to green
for a short moment. Then it goes off.
➣ Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
For performing a spectroscopic measurement using the ATR objective, the following
hardware and software components are required:
Hardware • ATR objective with focus sensor (end switch for stage
movement in z- direction)
• motorized x/y/z-stage with computer-controlled focussing
assembly (option A673-FA)
For performing a mapping measurement with the ATR objective, special components
and options need to be selected in OPUS when configuring the mapping device and the
imaging device.
☞ For detailed information about how to configure the mapping device and the imag-
ing device, refer to the OPUS/VIDEO Manual.
Procedure
3. Prepare the microscope for the back- 3.1. Operating panel: IR button and
ground measurement: reflection mode button (C and E in
3.1. Activate the measuring mode and fig. 3.4)
the reflection mode at the microscope. 3.2. ATR objective (See section 4.12.4
3.2. Bring the ATR crystal in the measur- and section 4.12.5.)
ing mode position (i.e. lower position). 3.3. revolving nosepiece with ATR
Set a contact pressure level which is objective
adequate to the degree of hardness of 3.4. Plastic ring which is included in the
the sample you intend to analyze. delivery scope of the ATR objective.
3.3. Swing the ATR objective in the beam 3.5. corresponding OPUS functions
path. (See OPUS/MAP and OPUS/VIDEO
Caution: Before swinging the ATR objec- Manual.) See also section 4.12.6.
tive in the beam path, make sure that the Note: In case an imaging device has
stage is low enough so that the crystal been selected in OPUS which is meant
will not hit the stage. Attention: Potential for ATR mapping (see operating step 1),
risk of damaging the ATR crystal! the joystick-controlled stage movement
3.4. Place the plastic ring on the stage in z-direction is automatically disabled!
underneath the ATR objective.
3.5. Move the stage slowly upwards until
the ATR crystal is in the focus position.
Note: The focus position is indicated
acoustically by a beep and optically by
the In-focus LED. When the ATR crystal
has reached the focus position, the In-
focus LED turns from red to green for a
short moment. Then it goes off.
6. Prepare the microscope for sample 6.1. Operating panel: VIS button (B in
viewing: fig. 3.4) or OPUS video wizard
6.1. Activate the viewing mode at the 6.2. ATR objective (See section 4.12.4.)
microscope. 6.3. Light path selector lever (A in
6.2. Bring the ATR crystal in the viewing fig. 3.14)
mode position (i.e. upper position). 6.4. Brightness control thumb wheel (B
6.3. Set the microscope for video image in fig. 3.5)
display. 6.5. Iris aperture for setting the Koehler
6.4. Set the brightness optimally. illumination in reflection (E in fig. 3.10)
6.5. Set the image contrast optimally. 6.6. Coarse and fine focus knob (B and
6.6. Focus on the sample. C in fig. 3.7)
6.7. Move the stage in x- and/or y-direc- Note: The joystick-controlled stage
tion to find a sample area which you movement in z-direction is automatically
intend to analyze spectroscopically. disabled!
6.7. Joystick or corresponding OPUS
functions
8. Prepare the microscope for the sample 8.1. operating panel: IR button (C in
measurement: fig. 3.4) or OPUS video wizard
8.1. Activate the measuring mode at the 8.2. ATR objective (See section 4.12.4.)
microscope. 8.3. Coarse and fine focus knob (B and
8.2. Bring the ATR crystal in the measur- C in fig. 3.7)
ing mode position (i.e. lower position). Note: The joystick-controlled stage
Note: Do not change the contact pres- movement in z-direction is automatically
sure level you have set in step 3.2.! disabled!
8.3. Move the stage upwards until the
distance between sample and ATR crys-
tal tip is less than 2 mm.
➣ Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
After you have started the sample measurement in OPUS, the ATR mapping measure-
ment runs automatically, i.e. no user-interaction is required.
During the ATR mapping measurement, the analysis system carries out following steps
automatically:
1. The microscope stage moves to the first x/y-position of the measurement grid you
have defined in OPUS.
2. After having reached this x/y-position, the stage moves upwards (in z-direction) until
the ATR crystal is in focus position. (Note: The focus position is indicated acousti-
cally by a beep and optically by the In-focus LED. When the ATR crystal has
reached the focus position, the In-focus LED turns from red to green for a short
moment. Then it goes off.)
3. Then, an IR sample spectrum is acquired.
4. Afterwards, the stage moves downwards (in z-direction). Then, the stage moves to
the next x/y-position of the measurement grid and moves upwards until the ATR
crystal is in the focus position. Then a spectrum is acquired.
5. This procedure is repeated at each measurement grid position.
6. Afterwards, OPUS calculates automatically the result spectra of the sample by
dividing the sample spectra by the background spectrum.
7. The mapping measurement result is saved automatically in a 3D file.
☞ For detailed information about this OPUS file type including the available OPUS
functions regarding editing, manipulation and evaluation, refer to the OPUS/3D
Manual.
For defining the measurement area and for measurements with polarized light, it is of
crucial importance that the GIR objective1 is attached at the revolving nosepiece with an
exact alignment.
☞ For information about measurements with polarized light in conjunction with the GIR
objective, see section 5.1.2.
The GIR objective is attached in an exactly aligned manner if the two VIS-GIR knobs
(see fig. 4.4) lie on an imaginary line which runs straight from the front to the back side of
the microscope. (Note: Only with this alignment of the GIR objective, it is ensured that
the incident light beam runs exactly from the right to the left.)
When you screw the GIR objective in the thread of the revolving nosepiece, however,
the exact alignment of the GIR objective is not always ensured a priori because the
threads vary slightly from microscope to microscope and from GIR objective to GIR
objective. For this reason, you first have to attach the GIR objective to the revolving
nosepiece and check the alignment of the GIR objective before starting the very first
measurement. (See section 4.15.5.) In case the GIR objective is not aligned as
described above, you have to readjust the alignment of the plane mirrors. (See
section 4.15.6.)
In case you have already readjusted the GIR objective but then you have removed it
from the revolving nosepiece, it is highly recommended to recheck the alignment before
using the GIR objective again. (See section 4.15.5.) When you screw the GIR objective
in the same thread of the revolving nosepiece again, normally a readjustment might not
be necessary.
The GIR objective is equipped with one ellipsoidal mirror and two plane mirrors which
are arranged in parallel. The two plane mirrors form a pair of which the position can be
shifted. (See section 4.15.3.)
The following figure shows the arrangement of the mirrors inside the GIR objective.
The following modes of operation can be set by means of the GIR objective mirror
optics: viewing mode (VIS) and measuring mode (GIR). To set the desired mode,
grasp the two VIS-GIR knobs (one knob is at the GIR objective front side, the other knob
is at the GIR objective back side) and shift them either to left (VIS) or to the right (GIR)
up to the stop. See fig. 4.4. In doing so, the position of the plane mirror pair is slightly
shifted as well.
VIS-GIR knobs
for setting the
desired mode of
operation
Viewing mode (VIS): The plane mirror pair is positioned in such a way that the focal
point of the 15x GIR objective is displaced allowing a sample viewing vertically from
above with a 15x magnification.
Measuring mode (GIR): The plane mirror pair is positioned in such a way that IR-beam
is reflected on the sample surface at a grazing incidence angle. After being reflected
from the sample surface, the beam impinges on the ellipsoidal mirror. The ellipsoidal mir-
ror reflects the IR beam back to the sample surface where the beam is focussed on the
same point. Afterwards, the IR beam is redirected through the objective into the micro-
scope and impinges on the detector.
This unique geometry has several advantages. Firstly, the GIR objective has a very high
throughput. Secondly, as the beam is reflected twice from the same sample surface
spot, the sample absorbs the light twice. The combination of these two factors provides
excellent sensitivity.
Depending on the currently set mode of operation (VIS or GIR), the GIR objective gener-
ates the following images:
• Viewing mode (VIS): Image of the sample surface (See fig. 4.6a.)
• Measurement mode (GIR): There are two images of the same sample surface
spot because the light is reflected twice from the sample surface. These two
images will be referred to as the primary image (from the first reflection) and the
secondary image (from the second reflection, after the light has been reflected
from the ellipsoidal mirror). The secondary image is both inverted and mirrored
relative to the primary image. (See fig. 4.6c.) Ideally, both images should lie one
upon the other.(See fig. 4.6b.)
➣ Note: With regard to the image generated in the viewing mode, the primary image is
mirrored and the secondary image is inverted.
Figure 4.6: b) Image of the measurement Figure 4.6: c) Image of the measurement
spot in GIR mode - primary spot in GIR mode - primary
image and secondary image lie image and secondary image do
one upon the other not lie one upon the other
➣ Important note: Realigning the GIR objective requires knowledge about the mirror
optics design and the functional principal of the GIR objective as well as about the
images generated in the VIS mode and in the GIR mode. For this reason, read thor-
oughly the sections 4.15.2 to 4.15.4 before starting to check the alignment of the
GIR objective and starting to realign the GIR objective, if required.
1. Attach the GIR objective to the revolving nosepiece opposite to the standard 15x
objective. (Note: Due to lack of space, first remove the plastic purge shroud of the
standard 15x objective, if present.)
2. Swing the GIR objective in the beam path. Make sure that the incident light beam
runs from the right (GIR) to the left (VIS).
3. Set the mirror optics of the GIR objective to the viewing mode (VIS).
4. Microscope: Activate the reflection mode.
5. Microscope: Activate the viewing mode.
6. Put the mirror on the microscope sample stage. (Note: The mirror is included in the
delivery scope.)
7. Focus on the mirror by moving the stage upwards.
NOTE
Potential risk of damaging the GIR objective
➣ Move the stage upwards carefully. Attention: The working distance of the GIR
objective is only ca. 0.7 mm. Prevent the stage or the sample lying on the stage
from hitting against the bottom side of the GIR objective. Otherwise the mirror
optics of the GIR objective might be damaged.
8. Move the stage in x- and/or y-direction until you see an edge of the mirror. Align the
mirror edge vertically. Position the mirror in such a way that the vertical mirror edge
is more or less in the center of the image. See fig. 4.7.
9. Set the mirror optics of the GIR objective to the measurement mode (GIR). Be care-
ful not to displace the mirror lying on the stage unintentionally!
In case you see an image as shown in fig. 4.8a, the GIR objective is attached at revolv-
ing nosepiece in an exactly aligned manner. In this case, no realignment is required. If,
however, you see an image of a mirror edge which is not vertically aligned (e.g. in
fig. 4.8b), you need to readjust the GIR objective mirror optics as described in the follow-
ing section.
Figure 4.8: a) GIR mode- Image of a vertically Figure 4.8: b) GIR mode - mirror edge is not
aligned mirror edge - alignment of vertically aligned - alignment of
the mirror optics is OK the mirror optics is not OK
Required tools
• flat-tip screwdriver
• Allen wrench (wrench size 2 mm)
Procedure
1. Remove the GIR objective from the revolving nosepiece and turn it upside down.
2. Remove the bottom part of the objective housing by loosening the two slotted-head
screws (VIS-GIR knobs) at the long side of the objective and the two slotted-head
screws at the bottom side of the objective. See fig. 4.9.
3. Loosen the four Allen screws at the bottom side of the GIR objective (fig. 4.10), but
do not remove them!
4x Allen screws
4. Attach the GIR objective to the revolving nosepiece opposite to the standard 15x
objective. (Note: Due to lack of space, first remove the plastic purge shroud of the
standard 15x objective, if present.)
5. Swing the GIR objective in the beam path.
6. Set the mirror optics of the GIR objective to the viewing mode (VIS).
7. Microscope: Activate the reflection mode and the viewing mode, if not yet done.
8. Put the mirror on the microscope sample stage. (Note: The mirror is included in the
delivery scope.)
9. Focus on the mirror by moving the stage upwards.
Note
Potential risk of damaging the GIR objective
➣ Move the stage upwards carefully. Attention: The working distance of the GIR
objective is only ca. 0.7 mm. Prevent the stage or the sample lying on the stage
from hitting against the bottom side of the GIR objective. Otherwise the mirror
optics of the GIR objective might be damaged.
10. Move the stage in x- and/or y-direction until you see an edge of the mirror. Align the
mirror edge vertically. Position the mirror in such a way that the vertical mirror edge
is more or less in the center of the image. See fig. 4.7.
11. Set the mirror optics of the GIR objective to the measurement mode (GIR).
12. Rotate the lower part of the GIR objective slightly to the left or to the right (fig. 4.11)
until the displayed image shows a vertically aligned mirror edge. See fig. 4.8a. Be
careful not to displace the mirror lying on the stage unintentionally!
13. Rotate the revolving nose piece until the GIR objective is in the front.
14. Fasten the four Allen screws at the bottom side of the GIR objective. (See fig. 4.10.)
In doing so, do not misalign the mirror optics again!
15. Remove the GIR objective from the revolving nosepiece.
16. Fit the bottom part of the housing on the objective and fasten it using the four slot-
ted-head screws. See fig. 4.9.
1. Microscope: Activate the viewing either the VIS button on the operating
mode. panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
2. Microscope: Activate the reflection either the reflection mode button on the
mode. operating panel (E in fig. 3.4) or in the
OPUS video wizard
☞ See OPUS/VIDEO Manual.
4. Swing the GIR objective in the beam GIR objective (fig. 4.4)
path. Set the mirror optics of the GIR ☞ See section 4.15.3
objective to the viewing mode (VIS).
5. Focus on the mirror, e.g. on a mirror Manual stage and motorized x/y-stage:
edge or on a scratch on the mirror sur- coarse and fine focus knobs at the micro-
face. scope (B/B’ and C/C’ in fig. 3.7)
Attention: Due to the very small work- Motorized x/y/z-stage: Joystick and cor-
ing distance (0.7 mm) of the GIR objec- responding stage control functions in
tive, move the stage upwards carefully. OPUS
Prevent the stage from hitting against ☞ See OPUS/VIDEO Manual.
the GIR objective bottom side. Other-
wise, the mirror optics of the GIR objec-
tive might get damaged.
6. Set the mirror optics of the GIR GIR objective (fig. 4.4)
objective to the measurement mode ☞ See section 4.15.3.
(GIR).
7. Microscope: Activate the measuring either using the IR button on the operat-
mode. ing panel of the microscope (C in fig. 3.4)
or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
10. Move the stage downwards. Manual stage and motorized x/y-stage:
Exchange the mirror for the sample. coarse and fine focus knobs at the micro-
scope (B/B’ and C/C’ in fig. 3.7)
Motorized x/y/z-stage: Joystick and cor-
responding stage control functions in
OPUS
☞ See OPUS/VIDEO Manual.
11. Set the mirror optics of the GIR GIR objective (fig. 4.4)
objective to the viewing mode (VIS). ☞ See section 4.15.3.
12. Microscope: Activate the viewing either the VIS button on the operating
mode. panel (B in fig. 3.4) or in the OPUS video
wizard
☞ See OPUS/VIDEO Manual.
13. Move the stage in x- and/or y-direc- Manual stage and motorized x/y-stage:
tion to find a sample area which is of coarse and fine focus knobs at the micro-
interest to you. scope (B/B’ and C/C’ in fig. 3.7)
Note: The sample area which is to be Motorized x/y/z-stage: Joystick and cor-
measured has to be in the center of the responding stage control functions in
cross hairs. OPUS
☞ See OPUS/VIDEO Manual.
15. Set the mirror optics of the GIR GIR objective (fig. 4.4)
objective to the measurement mode ☞ See section 4.15.3.
(GIR).
16. Microscope: Activate the measuring either using the IR button on the operat-
mode. ing panel of the microscope (C in fig. 3.4)
or in the OPUS video wizard
☞ See OPUS/VIDEO Manual.
➣ Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
i Due to the low signal intensity, it is recommended to perform the measurement with a
large number of scans (e.g. 500 or 1000 Scans).
Purging the microscope with dry air or nitrogen gas is only of relevance for performing IR
spectroscopic measurements. It is recommended, but not required.
Purging with dry air or nitrogen gas reduces the content of unwanted atmospheric com-
ponents like water vapor and carbon dioxide inside the microscope. Especially the water
vapor in the ambient air absorbs IR radiation. These absorptions are unwanted because
they manifest in the spectrum. In the worst case, H2O bands mask the spectral bands
resulting from the sample. Therefore, purging the microscope is recommended, espe-
cially in areas with a high relative air humidity.
Despite purging the microscope, the IR beam is normally exposed to the ambient air in
the area between the objective and the sample. Optionally, you can shield this area for
purging purposes as follows:
• by pulling down the plastic shroud of the 15x objective (See fig. 4.12a.)
• by using the optional purge housing1 (A684-3) (See fig. 4.12b.)
☞ For information about the purge gas supply requirements, see section 2.5.
☞ For information about how to connect the microscope to the purge gas supply line,
see section 2.8.
1. The purge housing design ensures a reduction of environmental influences on the sample area.
5.1.1 Overview
For the HYPERION microscope, the following optional objectives are available:
Due to the exactly defined plane of incidence, the orientation of polarized light is main-
tained. For this reason, the GIR objective is ideal for measurements with polarized light.
☞ For information about polarizers, see section 5.4.
The GIR objective is especially well-suited for spectroscopic measurements of very thin
layers (e.g. impurities, monolayer structure) on highly reflecting substrates (e.g. metals).
Also for the determination of molecular orientations, the use of an IR polarizer is recom-
mended. However, for analyzing thin layers on paper or impurities in polymers, the GIR
objective is not suited.
When you analyze a very thin layer (< 100 nm) on a metallic surface using p-polarized
light (i.e. the IR light is polarized in parallel to the incidence direction), absorptions are
well-recognizable in the spectrum. If, however, s-polarized light (i.e. the IR light is polar-
ized perpendicular to the incidence direction) is used, the spectrum shows only very
weak or no absorption bands at all.
Figure 5.1: Sample spectra of a aluminum mirror acquired with the GIR objective using
differently polarized IR light
You can check the orientation of the polarized light by acquiring a sample spectrum of
the aluminum mirror1. When this sample spectrum has been acquired with p-polarized
light, there is a prominent absorption band at approx. 950 cm-1 which results from the
aluminum oxide layer on the mirror surface. In case of s-polarized light, however, this
absorption band does not exist. See fig. 5.1.
As is usual practice for analyzing small sample areas, enclose the intended measure-
ment area using the knife-edge aperture. In case of the GIR objective, pay attention to
the following fact: Due to the grazing incidence angle of the IR beam, the measurement
spot is stretched approx. fourfold in the incidence direction of the IR beam, whereas per-
pendicular to the incidence direction of the IR beam, the diameter of the measurement
spot remains unchanged. To take this into account, set the knife-edge aperture to
25 µm x 100 µm to cover an area of 100 µm x 100 µm at the spectroscopic measure-
ment, for example. Note: Background measurement and sample measurement have to
be performed with identical knife-edge aperture setting.
1. The aluminum mirror is included in the standard delivery scope. Note: For measuring the background spec-
trum use the gold mirror which is included in the standard delivery scope as well.
5.2.1 Overview
For the HYPERION microscope, the following optional apertures are available:
The aperture wheel has 12 apertures of different diameters which can be rotated in the
beam path. The following table provides information about the diameter of the individual
apertures and the corresponding measurement spot diameter depending on the objec-
tive magnification.
A B C
i The wheel aperture and the manually-operated knife-edge aperture which can be
installed at place A and B (in fig. 5.2) are interchangeable with each other. However, the
apertures which can be installed in place C (in fig. 5.2) are not interchangeable with the
apertures which can be installed at place A and B (in fig. 5.2).
5.3.1 Overview
Motorized stage
The motorized stage can have the following optional fea-
tures:
• max. travel range in x- and y-direction: 100 mm x 80 mm
• a third motor allowing a computer-controlled and joystick-
controlled stage movement in z-direction
The heating/freezing stage THMS 600 (Linkam) can be used in conjunction with both the
manually-operated and the motorized microscope stage. The heating/freezing stage
THMS 600 is put on the corresponding microscope stage. Note: In case of the motorized
microscope stage, the base plate heating/freezing stage THMS 600 (Linkam) fits in the
cut-out of the microscope stage.
If required, the heating/freezing stage THMS 600 can be mounted directly on the height
adjustment unit of the microscope stage. (See fig. 5.3.) For this purpose, the microscope
stage needs to be removed. Note: In case the microscope is equipped with a motorized
stage, this variant is not recommended.
Figure 5.3: Microscope with installed heating/freezing stage THMS 600 (Linkam)
Temperatures above ambient temperature are realized by the connected heating unit
(Linkam). Cooling down and temperatures below ambient temperature are achieved by
pumping liquid nitrogen through the heating/cooling block of the stage. For more detailed
information about this topic, refer to the documentation accompanying the stage THM
S 600 (Linkam).
The desired temperature can be set as follows:
i Temperature information is stored together with the spectra if the temperature has been
controlled by the OPUS software. Measurements during temperature ramps are only
possible with the OPUS measurement function Protein Dynamics (optional software
package OPUS/PRO) or the temperature control software LinkSys by Linkam.
The utilizable temperature range of the stage is minus 196°C to plus 600°C. So depend-
ing on the set temperature, the stage and the sample can become very hot or cold dur-
ing the operation.
CAUTION
Risk of burn injuries or frostbites caused by touching the heating /
freezing stage
➣ Do not touch the hot or cold stage.
➣ Wait until the stage and the sample have cooled down or warmed up sufficiently
before touching the stage and removing the sample.
➣ Attention: Depending on the property of the sample, it can dramatically change its
physical appearance (e.g. melt) or even ignite. For this reason, determine in
advance how the sample in question will behave at the intended temperature.
The heatable sample holder can be used in conjunction with both the manually-operated
and the motorized microscope stage. (See fig. 5.4a.) Note: Note: In case of the motor-
ized microscope stage, the heatable sample holder fits in the cut-out of the microscope
stage.
For measurements with the heatable sample stage, Bruker recommends using only the
15x objective.
The sample is placed in the round opening of the sample holder. This opening has a
diameter of 13 mm which is the standard pellet size. Smaller samples can be fixed on or
sandwiched between two IR-transparent pellets. The pellet material (e.g. KBr or NaCl)
should have a low refraction index in order to reduce reflection losses and minimize
focus shifts as far as possible. To ensure a good contact between sample and pellet use
the supplied tightening ring to compress the sample sandwiched between two pellets. In
doing so, the sample thickness and the occurrence of possible interferences are
reduced.
The sample holder can be heated up to 180°C. So during operation, the sample holder
can become very hot.
CAUTION
Risk of burn injuries caused by touching the heatable sample holder
➣ Do not touch the hot sample holder.
➣ Wait until the sample holder and the sample have cooled down before touching
the holder or removing the sample.
➣ Attention: Depending on the property of the sample, it can dramatically change its
physical appearance (e.g. melt) or even ignite. For this reason, determine in
advance how the sample in question will behave at the intended temperature.
A temperature controller is included in the delivery scope of the heatable sample holder.
(See fig. 5.4b.) The desired temperature can be set as follows:
i Temperature information is stored together with the spectra if the temperature has been
controlled by the OPUS software. Measurements during temperature ramps are only
possible with the OPUS measurement function Protein Dynamics (optional software
package OPUS/PRO).
5.4 Polarizer
For analyzing samples with polarized light, the following polarizers are available:
• Polarizer for visible light (VIS polarizer)
• Polarizer for infrared light (IR polarizer)
D B
The polarizer holder has two positions: one position for the IR polarizer (A in fig. 5.5) and
another position for the VIS polarizer (B in fig. 5.5). There are two indentations (C in
fig. 5.5) at the polarizer holder for ensuring the correct slide-in depth of the two polariz-
ers. When you slide the polarizer in the microscope, the polarizer holder snaps notice-
ably in the correct position. Thus it is ensured that a polarizer (VIS or IR) is in the beam
path. In case you want to analyze the sample with non-polarized light, pull the polarizer
holder out of the microscope.
i The IR polarizer (A675-P) requires a holder for visible light (A675) because this holder
has a rotatable mount for the IR polarizer. If you have purchased the IR polarizer (A675-
P) separately, you have to insert the IR polarizer with the correct orientation into the
rotatable mount of the polarizing device. Attention: Be careful not touch the delicate
grating structure on the polarizer crystal surface.
The polarizer material is zinc selenide (ZnSe). Zinc selenide is toxic. During normal
operation and in an undamaged state, the polarizer material does not pose any health
hazard. However, if the material breaks because of mechanical impact, be extremely
careful and observe the following safety instructions:
WARNING
Health hazard because of improper handling of broken polarizer mate-
rial
Non-observance of the following safety instructions could result in death or serious
health problems (e.g. poisoning symptoms).
➣ Avoid generating dust of broken polarizer material. This material is toxic if swal-
lowed or inhaled.
➣ Avoid skin and eye contact.
➣ Dispose the toxic material according to the laboratory regulation and national reg-
ulations.
➣ Observe the safety instructions of the attached safety data sheet.
At the left microscope side, there are three slide-in slots for polarizers:
In slot A in fig. 5.6, the analyzer for transmission and reflection measurements can be
inserted.
For viewing the sample surface in reflection mode with crossed polarizers, a second
polarizer needs to be inserted into slot B in fig. 5.6.
For sample viewing in transmission mode, a second polarizers needs to be inserted into
slot C in fig. 5.6.
For IR spectroscopic measurements, usually one IR polarizer is sufficient. The IR polar-
izer can be inserted into any slot (A, B or C in fig. 5.6).
The polarizer holders are interchangeable. They can be inserted into any slot (A, B or C
in fir. 5.6).
Do not use an IR polarizer in combination with a VIS polarizer or vice versa. Polarizer
and analyzer have to be intended for the same spectral range.
Before starting a IR spectroscopic measurement, make sure that there is not any VIS
polarizer in the beam path. Reason: The VIS polarizer contains glass and glass absorbs
light in the mid-infrared region.
For enhanced sample visualization with visible light two polarizers (i.e. a polarizer in
front of the sample and an analyzer behind the sample) are recommended. The first
polarizer produces linearly polarized light. When this light goes through an anisotropic
sample, the direction of polarization may change. The second polarizer can be rotated,
using thumbwheel (D in fig. 5.5), to permit polarized light to pass only in a certain direc-
tion. If the two polarizers are ’crossed’, (i.e. their polarization directions are perpendicu-
lar to each other) an isotropic sample such as liquid will appear black. An anisotropic
sample (e.g. an oriented polymer or many crystalline materials) will appear brightly col-
ored. In transmitted light, a single visible light polarizer can sometimes improve the
image contrast. In reflected light, a polarizer-analyzer pair will produce effects similar to
those obtained in transmitted light if some or all of the light passes through at least one
layer of the sample.
A single IR polarizer can be used to measure the dichroism of micro samples. Each
anisotropic sample has two (or possibly three) independent infrared spectra, depending
on the polarizing direction of the IR light in relation to the optical axis of the material.
Measurements of IR dichroism can be used, for example, to determine the orientation of
polymer fibers.
The external sample cabinet IMAC1 is designed for sample viewing by means of a video
camera video camera and imaging spectroscopy using a FPA detector. It allows for ana-
lyzing larger sample areas than using the microscope. (Note: For this purpose, you need
to remove the FPA detector, the video camera and the light source from the microscope.
In case you have an additional light source and/or video camera, the removal and rein-
stallation of these components are not necessary.)
For measurements with IMAC, the sample is placed in the sample compartment of
IMCA. For this purpose a sample holder for transmission measurements is included in
the delivery scope. Optionally, additional accessories with QuickLock baseplate are
available which can placed in the IMAC sample compartment, for example: reflection
unit A517-P/Q for reflection measurements and ATR unit A529-S/Q for attenuated total
reflection measurements.
Figure 5.7: External sample cabinet IMAC with open sample compartment
☞ For detailed information about the external sample cabinet IMAC, refer to the
accompanying documentation.
These compression cells are used compress and flatten the sample material (e.g. rub-
ber, plastics, polymers) to an uniform thickness across the measuring area to ensure
maximum signal throughput without oversaturating the detector.
Perform only those repair and maintenance works which are described in this manual.
Adhere strictly to the described procedures and observe all relevant safety precautions.
Otherwise, personal injury and/or microscope damage can be the result. In this case,
Bruker does not assume any liability. Repair and maintenance works which are not
described in this manual have to be performed by Bruker service personnel only.
☞ For the Bruker service contact data, see section 1.5.
NOTE
All available detectors are installed on a special base plate which ensures a precise
installation of the detector. A realignment is not required.
The removal and installation procedure of the MCT detector and the FPA detector differ
from each other.
Step 1
Interrupt the power supply of the
MCT detector by switching off the
coupled spectrometer.
☞ See the user manual of the
spectrometer in question.
Step 3
Disconnect the ground cable from
the detector.
Ground cable
(yellow-green)
Step 4
Disconnect the cable of the temper-
ature sensor from the detector.
Cable of the
temperature
sensor (white
brown)
Step 5
Disconnect the data cable from the
detector.
Data cable
(gray)
Step 6
Loosen the two mounting screws at
the base plate of MCT detector
using an Allen wrench (3 mm).
Mounting screws
Step 7
Remove the MCT detector carefully
from the detector compartment.
Caution: Be careful not to dam-
age the mirrors!
To reinstall the MCT detector, perform the above steps in reverse order:
1. Insert the MCT detector carefully into the detector compartment.
2. Fasten the detector base plate.
3. Reconnect all cables to the MCT detector.
4. Reinstall the detector compartment housing.
5. Switch on the spectrometer.
Step 1
Switch off the FPA detector. On / Off switch
Note: The On/Off switch is located on
the bottom side of the FPA detector
compartment.
Step 2
Remove the housing of the FPA detec- Fastening
tor compartment. Loosen the six fasten- screws of the
ing screws (Allen screws) using an Allen housing
wrench (2 mm) and remove the hous-
ing.
Step 3
Disconnect all cable at the rear side of
the FPA detector. Data cable
Power cable
Trigger cable
Step 4
Loosen the three mounting screws at
Mounting
the base plate of the FPA detector. screws
Note: For loosening the two front
screws, use an Allen wrench (5 mm).
The back screw is factory-equipped with
a kind of screw driver.
Step 5
Remove the FPA detector from the
detector compartment.
To reinstall the FPA detector, perform the above steps in reverse order:
1. Insert the FPA detector into the detector compartment. Make sure that the detector
base plate snaps into the guide rail.
2. Fasten the detector base plate.
3. Reconnect all cables to the FPA detector.
4. Reinstall the detector compartment housing.
5. Switch on the FPA detector.
The operating temperature of the MCT detectors is significantly below room tempera-
ture. To achieve the required operating temperature, the MCT detectors are cooled down
with liquid nitrogen. The available MCT detectors have different nominal hold times1: 8,
12 or 24 hours. To provide for the longest possible hold time, the MCT detector is inte-
grated in a dewar. So, the actual hold time strongly depends on the quality of the vac-
uum in the detector dewar.
If the actual hold time decreases considerably with regard to the nominal hold time, the
detector dewar vacuum needs to be restored. The existence of condensation water on
the detector outside indicates that the vacuum must be stored soon. Another indication
that a vacuum restoration is required is a failed Ice Band Test2. If the MCT detector out-
side is iced the detector dewar vacuum must be restored immediately.
The MCT detector element is situated in an evacuable dewar. The dewar vacuum is
restored by evacuating the detector dewar with a vacuum pump. For this purpose, the
MCT detector needs to be removed from the microscope.
• Vacuum pump (turbo molecular pump or oil-free high-vacuum pump that is capa-
ble of generating a vacuum of at least < 10-5mbar)
• Adapter for connecting the vacuum pump to the MCT detector dewar
• Shut-off valve
• 2x flexible metal hoses
i The above listed evacuating equipment is NOT included in the standard delivery scope
of the MCT detector. If desired, Bruker offers suitable evacuating equipment (part num-
ber S105-V2, D126 and I10290). Alternatively, Bruker also offers the service of evacuat-
ing the MCT detector dewar (part number SD128). This option requires the removal of
the MCT detector from the microscope and the sending of the complete MCT detector to
Bruker for evacuation.
1. The hold time indicates how long the cooling effect of the liquid nitrogen lasts.
2. The Ice Band Test checks whether there is a thin ice layer on the detector element. This in turn is an indica-
tion of the vacuum quality in the MCT detector dewar. The Ice Band Test is part of the PQ test protocol. For
detailed information, refer to the OPUS Reference Manual.
A B C D
Figure 6.1: a) Adapter b) Adapter with flexible metal hose and flange
B Flange
Procedure
➣ Before starting to evacuate the MCT detector dewar, make sure that the dewar does
not contain any more liquid nitrogen and that the detector has warmed up to room
temperature. Take into consideration that the detector warming-up from operating
temperature to room temperature takes at least 3 hours after the residual liquid
nitrogen has been emptied.
1. Remove the MCT detector from the microscope. See section 6.2.2.
2. Connect the adapter to the vacuum pump by flanging a flexible metal hose to the
connecting piece of the adapter (E in fig. 6.26.3) and to the vacuum pump. See
fig. 6.1b. (Note: The connecting piece of the adapter has an OD of 9.7mm.) In addi-
tion, install a shut-off valve between adapter and vacuum pump.
3. Make sure whether the shut-off valve is closed. Switch on the vacuum pump. Leave
the pump running until it has reached its operating temperature.
4. Inspect the O-ring inside the adapter (C in fig. 6.3) for signs of wear.
➣ The O-ring inside the adapter is a wearing part that needs to be replaced after 4 or 5
evacuations at maximum.
5. Remove the cap from the connection nozzle of the detector. (See fig. 6.2a.)
6. Pull the adapter knob (G in fig. 6.3) to the open position and loosen the coupling nut
(A in fig. 6.3).
7. Push the adapter carefully over the connection nozzle of detector dewar and fasten
the coupling nut (A in fig. 6.3) hand-tight while holding the adapter and the detector
as shown in fig. 6.2b. (A hand-tight tightening of the coupling nut is sufficient.)
➣ Hold the adapter and the detector always as shown in fig. 6.2b when you have to
carry out the following tasks: opening and closing the evacuation valve by pushing
or pulling the adapter knob (step 8, 12, 14 and 17), screwing the threaded adapter
rod in or out of the connection thread of the dewar evacuation valve (step 11 and
15) and loosening the coupling nut (step 18).
Connection nozzle
(without cap)
Figure 6.2: a) MCT detector Figure 6.2: b) How to hold the MCT detector when oping or
closing the dewar evacuation valve
8. Push the adapter knob (G in fig. 6.3) in the closed position until the threaded rod (D
in fig. 6.3) of the adapter is in contact with the sealing plug of the dewar evacuation
valve.
9. Before you begin to evacuate the detector dewar, check the connections for leak
tightness by evacuating the section between vacuum pump and detector at first. To
do this, open the shut-off valve. If a vacuum of 10-4mbar is generated within a few
minutes it is an indication of the leak tightness of this section.
10. Close the shut-off valve again.
11. Screw the threaded rod of the adapter (D in fig. 6.3) in the connection thread of
dewar evacuation valve by turning the adapter knob (G in fig. 6.3) clockwise; 2 to 3
rotations are sufficient. Attention: In case of more than 2 or 3 knob rotations
there is a risk that the threaded connection becomes inseparable! That means
the threaded rod of the adapter cannot be screwed out of the connection
thread of the dewar evacuation valve again.
12. Pull the knob (G in fig. 6.3) to the open position in order to open the dewar evacua-
tion valve.
13. Begin to evacuate the detector dewar by opening the shut-off valve.
➣ We recommend an evacuation time of at least 3 days to allow for generating an opti-
mal vacuum inside the dewar. The final pressure in the detector dewar should be
less than 10-5 mbar.
14. When the optimal vacuum is achieved, close the dewar evacuation valve by push-
ing the adapter knob (G in fig. 6.3) to the closed position. Press the adapter knob
firmly to the stop position to ensure that the dewar evacuation valve is sealed air-
tightly.
15. Screw the threaded rod of the adapter (D in fig. 6.3) out of the connection thread of
the dewar evacuation valve by rotating the adapter knob (G in fig. 6.3) several turns
counterclockwise until you sense that the threaded adapter rod and the connection
thread of the dewar evacuation valve are not joint any more. Be careful in order to
prevent an unintentional opening of the evacuation valve and consequently to pre-
vent the detector dewar from being vented again.
16. Vent the section between vacuum pump and adapter.
17. Pull the knob (G in fig. 6.3) to the open position. Attention: Make sure that the seal-
ing plug of the evacuation valve is NOT pulled out! This may occur when you have
screwed the threaded adapter rod too far in the connection thread of the dewar
evacuation valve. (See step 10.) In this case repeat the dewar evacuation. If you do
not succeed in closing the evacuation valve at all you have to send the detector in to
Bruker.
18. Loosen the coupling nut (A in fig. 6.3) and remove the adapter from the connection
nozzle of the detector dewar.
19. Reinstall the MCT detector in the spectrometer. See section 6.2.2.
➣ If a tiny amount of air should unawares get into the detector dewar during the evac-
uation procedure (e.g. when you close the evacuation valve) you can perform mea-
surements with this MCT detector for the moment but after a relatively short period
of time you have to repeat the detector evacuation.
C
A G
D
B F
closed
open
A Coupling nut
B O-ring retainer
C O-ring
D Threaded rod (to remove the valve closure of the detector dewar)
G Knob
The ATR crystal is fragile. To prevent the ATR crystal from getting damaged, observe the
following handling instructions when working with the ATR objective:
Note
Risk of damaging the ATR crystal
➣ Handle the ATR objective with utmost care. Prevent the ATR crystal tip from fitting
the microscope stage. Especially in the following situations, be aware of the
potential risk of damage:
• attaching the ATR objective to the revolving nosepiece or removing the ATR
objective from the revolving nosepiece,
• swinging the ATR objective in the beam path with the microscope stage being
set too high,
• moving the microscope stage upwards to focus on the sample and
• pulling down the outer casing of the ATR objective to bring the ATR crystal in
the measuring position and/or set a certain contact pressure level.
➣ Using the ATR objective, the sample temperature should not exceed 40°C. In
case of a higher sample temperature, the ATR crystal may become detached.
1. Activate the viewing mode using the VIS button on the microscope operating panel
(B in fig. 3.4).
2. Set the ATR crystal in the viewing mode position (i.e. upper position), if not yet
done. (See section 4.12.4.)
3. Put the supplied mirror on the microscope stage. Position the mirror below the ATR
crystal.
4. Move the stage carefully upwards until the distance between ATR crystal tip and
stage is approx. 2 mm.
NOTE
➣ Do not view through the binocular while moving the stage upwards, but keep an
eye on the decreasing distance between ATR crystal tip and stage. Potential risk
of damaging the ART crystal! Prevent the ATR crystal tip from hitting against the
mirror or the microscope stage.
5. Move the stage slowly upwards until you see a sharp image.
It is the mirror image of the ATR crystal tip which shows possible fissures and / or frac-
tions in the crystal. See fig. 6.4.
Figure 6.4: a) Image of an intact ATR Figure 6.4: b) Image of a damaged ATR
crystal crystal
If the check should reveal that the ATR crystal is damaged, it needs to be replaced. For
the order number of a replacement crystal, see appendix C.
General information
Procedure
For replacing the crystal assembly, the ATR objective needs to be removed from the
microscope.(See section 4.12.3.) Put the ATR objective on an even surface with the
crystal pointing upwards.
Required tools:
• small flat tip screwdriver
• tweezers ((Note: They are in the tool box supplied with the microscope.))
• hex wrench (Note: This hex wrench is included in the delivery scope of the ATR
crystal.)
Pins
Step 2
Take the three pins out of the recesses
using the tweezers.
Step 6 Pins
NOTE
➣ The ATR crystal is fragile. For this reason, move the microscope stage always
carefully upwards. Prevent the ATR crystal tip from hitting against the stage.
5. Move the microscope downwards a little bit. Do not change the position of the
mirror on the stage!
6. Set the ATR crystal in the viewing mode position (i.e. upper position). (See
section 4.12.4.)
7. Focus on the mirror.
If the imprint of the crystal tip is in the center of the crosshairs as shown in fig. 6.6a, the
ART crystal is in the center position. In this case, no realignment in horizontal direction is
required. Otherwise, you have to align the ATR crystal centrically.
Figure 6.6: a) ATR crystal in center position b) ATR crystal not aligned centrically
General information
For aligning the ATR crystal in horizontal direction, the three slotted-head screws at the
inner ring at the ATR objective bottom side have to be tightened only loosely, not firmly.
(See section 6.4.3, step 9 of the crystal assembly replacement procedure.)
Correct the horizontal alignment of the crystal with the ATR objective being attached at
the revolving nosepiece and being placed in the beam path.
Required tools
• hex wrench (Note: This hex wrench is included in the delivery scope of the ATR
crystal.)
Procedure
1. Adjust the crystal position in the horizontal plane by rotating the adjusting screws
(fig. 6.7) using the hex wrench. In doing so, the crystal assembly is moved in the
corresponding direction in horizontal plane. The direction in which the crystal
assembly needs to be moved depends on the position of the crystal tip imprint in
relation to crosshairs center. (An example is shown in fig. 6.6b.)
2. Recheck the ATR crystal position for centrality. (See section 6.4.4.)
3. If the check reveals that the ATR crystal is in the center position, tighten firmly the
three slotted-head screws at the inner ring at the ATR objective bottom side
(fig. 6.8). Otherwise, repeat step 1 and step 2 above. When tightening firmly the
three slotted-head screws at the ATR objective bottom side, be careful not to dis-
place the crystal assembly again!
Slotted-head screws
(Note: They are used
for fastening the crystal
assembly at the ATR
objective bottom side.)
1. Make sure that the ATR objective is connected to the microscope. (For information
about how to connect the ATR objective to the microscope, see section 4.12.3.
2. Make sure that the beam path is not blocked, for example by a polarizer or a knife-
edge aperture (i.e. the knife-edge aperture has to be open completely).
3. Move the microscope stage downwards.
4. Swing the ATR objective in the beam path.
5. ATR objective: Set the ATR crystal in the measurement mode position (i.e. lower
position), if not yet done. (See section 4.12.4.)
6. ATR objective: Set contact pressure level 1. (See section 4.12.5.)
7. Put the plastic ring1 on the microscope stage. Position the ring concentrically under-
neath the ATR objective.
8. Microscope: Activate the measurement mode using the IR button on the micro-
scope operating panel (C in fig. 3.4).
9. Microscope: Activate the reflection mode using the reflection mode button on the
microscope operating panel (E in fig. 3.4).
10. Start the OPUS software. Select in the Measure menu the Advanced measurement
function. In the Measurement dialog, click on the Advanced tab. Click on the Load
button and load an adequate experiment file (’*’.xpm). (See appendix B.)
11. In the Measurement dialog, click on the Check Signal tab. Activate the Interfero-
gram option button, if not yet activated. (See fig. 6.9b.)
12. Move the microscope stage slowly upwards until the plastic ring pushes the ATR
crystal in the focus position.
1. The plastic ring is included in the delivery scope of the ATR objective.
➣ Note: The focus position is indicated acoustically by a beep and optically by the In-
focus LED (fig. 6.9a). When the ATR crystal has reached the focus position, the In-
focus LED turns from red to green for a short moment. Then it goes off.
When the ATR crystal is in the focus position, maximum signal (amplitude value) has to
be displayed in OPUS. (See fig. 6.9b.) If this is not the case, the height setting of the
ATR crystal needs to be corrected (i.e. adjustment of the ATR crystal in vertical direc-
tion).
Amplitude value
In-Focus LED (Signal intensity)
General information
The screw for adjusting the height setting of the ATR crystal is situated at the ATR objec-
tive top side next to the In-focus LED cable outlet. (See fig. 6.10a.)
Correct the height setting of the crystal (i.e. adjustment of the ATR crystal position in z-
direction) with the ATR objective being attached at the revolving nosepiece and being
placed in the beam path.
Required tools
hex wrench (Note: This hex wrench is included in the delivery scope of the ATR crystal.)
Procedure
1. Move the microscope stage downwards and swing it out of the beam path in the
front position.
2. Actuate the rocker switch and pull the outer casing of the ATR objective downwards
as far as it will go (i.e. until it snaps into place at pressure level 5). (See
section 4.12.5.)
3. Insert the long part of the hex wrench straight into the opening. (See fig. 6.10a and
6.10b.) Note: The hex wrench has to snap in the head of the hex countersunk
screw.
Figure 6.10: a) ATR objective top side b) Inserting the hex wrench
4. Actuate the rocker switch and pull the outer casing of the ATR objective downwards
until it snaps into place at pressure level 1. (See section 4.12.5.)
5. Swing the ATR objective in the beam path.
6. Put the plastic ring1 on the microscope stage. Position the ring concentrically under-
neath the ATR objective.
7. Move the microscope stage slowly upwards until the plastic ring pushes the ATR
crystal in the focus position. Note: The focus position is indicated acoustically by a
beep and optically by the In-focus LED (fig. 6.9a). When the ATR crystal has
reached the focus position, the In-focus LED turns from red to green for a short
moment. Then it goes off.
8. While watching the signal display in OPUS (fig. 6.9b), correct the height setting of
the ATR crystal by slightly rotating the adjusting screw using the hex wrench. Cor-
rect the setting until the maximum signal intensity (amplitude value) is displayed in
OPUS.
1. The plastic ring is included in the delivery scope of the ATR objective.
This chapter deals mainly with the most common microscope problems that may occur
as experience has shown. Possible problems may be caused by operator errors, sam-
ples unsuitable for the measurement technique in question or misaligned, damaged or
defect microscope components, for example.
Important note: Due to complex instrumental setup, it is recommended to proceed sys-
tematically. First try to find out which instrument (FT IR spectrometer or HYPERION
microscope) has cause the problem. For this reason, consult also the User Manual of
the FT IR spectrometer in question for troubleshooting. Not until you can preclude the FT
IR spectrometer being the trouble source, consult the chapter Troubleshooting in the
HYPERION User Manual.
Depending on how a microscope problem becomes apparent, they are dived in the fol-
lowing categories:
• Sample viewing through the binocular: No field of view or dark field of view
• No video image displayed on the LCD monitor and/or in OPUS
• Problems regarding the motorized microscope stage
• Problems regarding the ATR objective
• Problems regarding the mapping measurements
• Problems regarding the FPA detector
• IR signal check in OPUS reveals that no signal is detected or the signal intensity
is too low.
• IR signal check in OPUS shows an unusual spectrum curve shape
This chapter provides information about possible causes of the problem and presents
solutions for troubleshooting. If the solutions listed in this chapter do not solve the prob-
lem, contact the Bruker service.
☞ For the Bruker service contact data, see section 1.5.
7.2.1 Sample viewing through the binocular: No field of view or dark field
of view
General causes
There is not any objective in the beam path. Swing an objective in the beam path.
In transmission mode
Beam path is blocked by the sample stage or a Check the beam path for objects blocking the
sample holder, for example. beam path and remove them.
In reflection mode
☞ For information about how to check the IR signal intensity, see section 4.7.
General causes
The beam path is blocked by one or more Open the aperture(s) until you get a satisfying
apertures (e.g. knife-edge aperture, iris aper- IR signal intensity.
ture for setting the Koehler illumination, pinhole ☞ For an overview of the apertures, see sec-
aperture for condenser adjustment). tion 3.7.
In transmission mode
In reflection mode
The motorized stage control The motorized stage is not Check the cables for correct
fails to operate completely (i.e. connected at all or not con- connection. Connect them
the motorized stage cannot be nected properly (e.g. plug fits correctly.
controlled at all). loosely in connector socket). ☞ See section 2.7.2.
In OPUS, an experiment file is loaded of which In OPUS, load an experiment file of which the
the parameter settings are not defined for map- parameter settings are defined for a mapping
ping measurements (i.e. the selected Imaging measurement.
Device option is not for mapping measure-
ments). ☞ See appendix B.
At the mapping measurement start, the dis- Abort the measurement. Move the stage
tance between sample and crystal tip (with the upwards until the distance between sample
ATR crystal being in the measuring mode posi- and crystal tip is ≤ 2 mm. Restart the mapping
tion) was more than 2 mm. measurement.
In OPUS, an experiment file is loaded of which OPUS: Select an imaging device which is
the selected imaging device is not defined for defined for mapping measurements with ATR
mapping measurements with ATR objective. objective.
Besides the causes listed in section 7.2.3, this type of problem may have also the follow-
ing causes in case of measurements with the FPA detector.
The power supply cable and/or the signal cable Check the cable for correct connection. Con-
is/are not connected at all or not connected nect it correctly.
properly. ☞ See section 2.7.6.
Data have been acquired up to the convolution Insert the optical filter in the optical adaptation
limit of 3900 cm-1 without the optical filter. box. See fig. 7.1.
Spectral
depends on the FT IR spectrometer coupled to the microscope
resolution
Area covered by
Optimized for a diameter of 250 µm;
the measure-
Minimum diameter of 10 µm with the standard objective
ment
A.2 Objectives
Parameter Specification
Standard: 50 mm x 75 mm
max. travel range in x- and y-direction
optional: 100 mm x 80 mm
Positioning accuracy ± 0.1 µm at measurement point
Parameter Specification
A.5 Detectors
Mode of cooling /
Detector Spectral range Detection sensitivity
nominal hold time
Standard MCT detector with liquid N2 12,000 - 600 cm-1 D*>2x10**10cm Hz1/2W-1
mid band, D316025 8h
optionaler MCT detector with liquid N2 12,000 - 600 cm-1 D*>2x10**10cm Hz1/2W-1
mid band, D316025MU > 12 h
optionaler MCT detector with liquid N2 10,000 - 780 cm-1 D*>4x10**10cm Hz1/2W-1
narrow band, D313025 8h
optionaler MCT detector with liquid N2 10,000 - 780 cm-1 D*>4x10**10cm Hz1/2W-1
narrow band, D313025M > 12 h
optionaler MCT detector with liquid N2 10,000 - 450 cm-1 D*>5x10**9cm Hz1/2W-1
broad band, D315025 8h
optionaler MCT detector with liquid N2 10,000 - 450 cm-1 D*>5x10**9cm Hz1/2W-1
broad band, D315025M > 12 h
InSb-detector (optional) with liquid N2 10,000 - 1,850 cm-1 D*: >1.5x10**11cm Hz/W
near-infrared region, 8h
D413
The FPA1 detectors listed in the table below are multi-element detectors.
Parameter Specification
Parameter Specification
Cable length ~ 50 cm
The following table gives an overview about the experiment files delivered with the
OPUS software for IR spectroscopic measurements with the HYPERION microscope.
File name of the supplied xpm files For measurements with HYPERION 1000
In the delivered experiment files, the default parameter settings are store. If required,
they need to modified.
Normally, the default parameter settings (especially the optics parameter) of the deliv-
ered experiment files need to be adapted to configuration of the analysis system in ques-
tion. To do this, proceed as follows:
1. Select in the OPUS Measure menu the Video-assisted measurement function.
2. Load a supplied experiment which is appropriate for the measurement mode and
the measurement technique (transmission, reflection, mapping measurement1,
measurement with ATR objective, measurement with FPA detector2) you intend to
perform.
3. Select the corresponding parameter options. (See the following sections.)
4. Save the modified parameter settings. To do this, click in the Video assisted Mea-
surement dialog on the Advanced tab. On this dialog page, click on the Save button.
(Note: It is advisable to save the modified experiment file with a different file name.)
To modify the optics parameter, click on the Optics tab. See the following figure.
Figure A.1: OPUS dialog Video assisted Measurements - Dialog page Optics parameter
1. Mapping measurements are only possible if the microscope is equipped with a motorized sample stage.
2. The FPA detector is only available for the microscope variant HYPERION 3000.
Aperture setting 6 mm
Note: This parameter refers to the aperture in the FT IR spec-
trometer.
Scanner velocity It is the velocity of the movable interferometer mirror which is situ-
ated in the FT IR spectrometer.
☞ The parameter settings and values on the other dialog pages (Advanced, Acquisi-
tion and FT) depend on the FT IR spectrometer to which the HYPERION micro-
scope is coupled. For information about the default settings of these parameters,
refer to the User Manual of the FT IR spectrometer in question. Consult also the
OPUS Reference Manual.
A697-R10 Ge crystal, replacement ATR crystal assembly for ATR objective in case of
HYPERION 1000 and HYPERION 2000
A697-R10B Ge crystal, replacement ATR crystal assembly for ATR objective in case of
HYPERION 3000
Numerics C
Coarse focus ......................................27, 33
15x GIR objective ...................................111
Coarse focus knob ....................................33
15x objective .................. 44, 63, 68, 77, 161
Compression cell ................... 124, 149, 152
Plastic shroud ........................................110
Condenser .26, 28, 33, 36, 52, 63, 149, 152
20x ATR objective ...................................111
Centering screws ...............................36, 65
36x objective .................................. 111, 162 Checking the setting .................................63
40x objective ...........................................161 Correcting the setting ...............................65
4x objective ................ 44, 77, 111, 150, 161 Condenser focussing knob .......... 33, 36, 65
Control panel ............................................26
A
Analysis system D
Switching off ............................................57 Data cable ................................................10
Switching on ............................................56
Detector ................. 27, 28, 47, 51, 151, 153
Analyzer ........................................... 52, 121 Checking the saturation ............................75
Aperture ....................................................51 Installation locations .................................47
Diameter ...............................................113 Mode of cooling .....................................163
Installation locations ........................ 39, 114 Nominal hold time ..................................163
Measurement spot diameter ....................113 Overview of single-element detectors .......163
Overview ........................................ 37, 113 Sensitivity .............................................163
ATR crystal assembly .............................137 Spectral range .......................................163
ATR objective 72, 86, 111, 135, 153, 155, 162 Detector evacuation
Aligning the crystal centrically ..................142 Required equipment ...............................130
Attaching at the revolving nosepiece ..........87 Detector oversaturation ............................76
Checking the crystal position for centrality .141 Detector temperature warning indicator ...30
Checking the height setting of the crystal ..143
Connecting to the microscope ...................87 E
Contact pressure ....................................162
Contact pressure level ..............................72 Environmental conditions
Contact pressure levels ............................89 Ambient temperature range .......................11
Correcting the height setting of the crystal .144 Ambient temperature variations .................11
Crystal material ......................................162 Humidity .................................................11
Crystal tip diameter ................................162 Experiment file ........................................167
Focussing in measuring mode ...................90 Modifying ..............................................168
Focussing in viewing mode .......................89 External power supply unit .......... 10, 13, 14
Handling instructions ................................86 External sample cabinet .........................123
In-focus LED ...................... 73, 90, 98, 144
Mapping measurement procedure ..............95 F
Replacing the crystal assembly ................136
Single point measurement procedure .........91 Filling hole for detector .............................60
ATR objective crystal Fine focus ...........................................27, 33
Checking for damages ............................135 Fine focus knob ........................................33
Cleaning .................................................86 Focussing .................................................77
Measuring mode position ................... 72, 88 FPA detector ........ 25, 47, 48, 158, 159, 164
Viewing mode position ..............................88 Cooling .............................................59, 61
Mode of cooling .....................................164
B Nominal hold time ............................61, 164
Number of detector elements ..................164
Beam attenuator 76, 123, 124, 158, 159, 160
ON / OFF switch ..............................57, 128
Beam path ................................................49 Removing / reinstalling ...........................128
HYPERION 1000 and 2000 .......................49 Spectral range .......................................164
HYPERION 3000 .....................................50
Binocular ..............26, 29, 42, 45, 51, 64, 68
Brightness
R
Reflection mode ........................................77
Viewing and measuring a sample ...............82
Reflection mode button ........ 29, 68, 72, 148
Revolving nosepiece .......................... 26, 43
Rotatable wheel aperture ............... 113, 115
S
Sample holder
Heatable ...................................... 116, 118
Miniature ...............................................116
Site requirements
Environmental conditions ..........................11
Space requirements .................................11
Spectral range ........................................161
Spectral resolution ..................................161
Stage ........................................................26
manually operated stage ...........................25
motorized x/y-stage ..................................25
Overview ...............................................116
Stage movement
Joystick-controlled ....................................35
Start button ........................................ 29, 30
Switch-on procedure with FPA detector ...56
Switch-on procedure without FPA detector 56
T
Transmission mode ..................................77
Viewing and measuring a sample ...............78
Transmission mode button .............. 29, 148
V
Video camera ..................................... 26, 42
Video camera port ....................................52
Viewing mode
ATR objective ..........................................88
GIR objective .........................................101
Microscope ..............................................29
VIS button ............................ 29, 68, 77, 148
VIS polarizer .......... 120, 122, 148, 151, 159