Bruker HYPERION User Manual

HYPERION
User Manual
I 24319
3rd edition 2017, publication date March 2017
© 2017 BRUKER OPTIK GmbH, Rudolf-Plank-Straße 27
D-76275 Ettlingen, www.brukeroptics.com
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
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Table of Contents
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
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Table of Contents
4.15 GIR objective - Important operating notes......................................................... 99
4.15.1 General information................................................................................................ 99
4.15.2 Design of the mirror optics ................................................................................... 100
4.15.3 Setting the viewing mode (VIS) or measuring mode (GIR) .................................. 101
4.15.4 Images generated by the GIR objective ............................................................... 102
4.15.5 Checking the alignment of the GIR objective ....................................................... 103
4.15.6 Realigning the GIR objective................................................................................ 104
4.16 Measuring a sample with the GIR objective .................................................... 107
4.17 Purging the microscope .................................................................................... 110
5 Options and Accessories .........................................................................111
5.1 Optional objectives .............................................................................................111
5.1.1 Overview ...............................................................................................................111
5.1.2 Additional information about the GIR objective .....................................................112
5.2 Optional apertures ............................................................................................. 113
5.2.1 Overview ...............................................................................................................113
5.2.2 Installation location of the exchangeable apertures ..............................................114
5.3 Optional microscope stages and sample holders........................................... 116
5.3.1 Overview ...............................................................................................................116
5.3.2 Heating/freezing stage THMS 600 (Linkam) .........................................................117
5.3.2.1 General information...............................................................................................117
5.3.2.2 Controlling the temperature...................................................................................117
5.3.2.3 Safety notes ..........................................................................................................118
5.3.3 Heatable sample holder ........................................................................................118
5.3.3.1 General information...............................................................................................118
5.3.3.2 Safety notes ..........................................................................................................119
5.3.3.3 Controlling the temperature...................................................................................119
5.4 Polarizer .............................................................................................................. 120
5.4.1 General information.............................................................................................. 120
5.4.2 Safety notes ......................................................................................................... 120
5.4.3 Installation location............................................................................................... 121
5.4.4 Performing IR spectroscopic analyses using polarized light ................................ 122
5.5 External sample cabinet - IMAC........................................................................ 123
5.6 Compression cells ............................................................................................. 124
6 Repair and Maintenance ...........................................................................125
6.1 General information ........................................................................................... 125
6.2 Removing and installing the detector .............................................................. 125
6.2.1 General information.............................................................................................. 125
6.2.2 Removal and installation procedure of the MCT detector .................................... 125
6.2.3 Removal and installation procedure of the FPA detector ..................................... 128
6.3 Evacuating the detector dewar ......................................................................... 130
6.3.1 General Information.............................................................................................. 130
6.3.2 Evacuating the MCT detector dewar .................................................................... 130
6.4 Replacing a damaged ATR objective crystal ................................................... 135
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6.4.1 General handling instructions............................................................................... 135
6.4.2 Checking the ATR crystal for damages ................................................................ 135
6.4.3 Replacing the ATR crystal assembly .................................................................... 136
6.4.4 Checking the ATR crystal position for centrality ................................................... 141
6.4.5 Aligning the ATR crystal centrically ...................................................................... 142
6.4.6 Checking the height setting of the ATR crystal..................................................... 143
6.4.7 Correcting the height setting of the ATR crystal ................................................... 144
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
B Measurement parameters .........................................................................167
C Spare parts and consumables..................................................................171
D System diagram.........................................................................................173
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HYPERION - User Manual Bruker Optik GmbH

1 Safety

1.1 General safety information

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 micro­scope 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 instruc­tions. Never remove or deactivate any supporting safety systems during micro­scope 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.

1.2 Classification of the safety notes

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.
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Safety 1

1.3 Overview of possible types of hazard

1.3.1 Possible hazards during installation, operation, maintenance and repair

Hazards that can possibly occur during installing, operating and repairing the micro­scope 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 symbol
Definition
General hazard
This warning symbol indicates a general hazard area. Consult the man­ual and inform yourself about the concrete nature of the hazard in ques­tion. Observe the safety instructions and follow the precautions described in the manual to avoid personal injury and/or property dam­age.
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 sub­stances
Exposure to cryogenic substances or cooled components causes frost­bite 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 compo­nents 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 / freez­ing sample stage THMS600 (Linkam)
Important: All warning labels on the microscope must always be kept legible. Immedi­ately replace a worn or damaged label!
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HYPERION User Manual Bruker Optik GmbH

1.3.2 Possible hazardous sample materials

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
Safety 1
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 correspond­ing 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 sub­stances etc.) according to the prevailing laboratory regulations. Detergents and cleaning agents must be disposed according to the special waste regulations.
Corrosive substances
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Safety 1

1.4 Intended use

The microscope HYPERION is intended for the microscopic examination and FT-IR spectroscopic analysis of micro-samples, small sample areas and inhomogeneous sam­ples. For the FT-IR spectroscopic analysis, the microscope needs to be coupled to a FT­IR spectrometer of the TENSOR or VERTEX series. It is suited for all kinds of solid sam­ples 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 acces­sories made by other manufacturers and used in conjunction with the microscope, Bruker Optik GmbH does not assume any liability for safe operation and proper function­ing.
Health hazard because of unintended use of the microscope
Non-observance of the following safety instruction could result in injury and/or micro­scope 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.

1.5 Service contact data

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
WARNING
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.
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HYPERION User Manual Bruker Optik GmbH

2 Installation

2.1 General information

The installation of the complete analysis system (i.e. microscope plus FT IR spectrome­ter 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.

2.2 Inspecting the packaging

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.

2.3 Transporting the microscope

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.
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Installation 2

2.4 Scope of delivery

Standard components: The standard scope of delivery includes:
Required components • PC compatible data system (Note: If desired, the PC
• Standard version of the HYPERION microscope vari-
a
in question (including the user manual)
ant
• External power supply unit with low-voltage cable, country-specific power cord
• miscellaneous cables
• Tool case (The blue case includes miscellaneous tools, sample preparation tools, spare lamp, pinhole, mirrors, microscope slides)
• OPUS software, basic IR package (including the OPUS Reference Manual as pdf file on the OPUS CD)
• Software package OPUS/VIDEO for video-assisted measurements (including the OPUS/VIDEO Manual as pdf file on the OPUS CD)
can also be provided by the operating company.)
• FT-IR spectrometer of the TENSOR or VERTEX series
Note: The microscope is an accessory which needs to be coupled to a FT-IT spectrometer. In case the micro­scope has been ordered at a later date, spectrometer and PC are possibly already on site.
Optional components:
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 scope of delivery may also include following optional components:
• Miscellaneous optional components and accessories (e.g. objectives, detectors, polarizer etc.)
• Optional OPUS software packages (e.g. OPUS/3D) including the corresponding manuals
• Fluorescence option
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2.5 Site requirements

The operating company has to provide an installation site that meets the following site requirements:
Space requirements: Depending on the microscope model, the HYPERION
Installation 2
microscope has different dimensions:
HYPERION 1000 and HYPERION 2000: 45 cm (w) x 60 cm (d) x 82 cm (h)
HYPERION 3000: 55 cm (w) x 80 cm (d) x 92 cm (h)
• When preparing the installation site, take into account that the ocular at the microscope front side is easily accessi­bly.
• At the rear side, the microscope requires a clearance of at least 25 cm (10“).
• Also take the installation site of the data station into account. The distance between microscope and data sta­tion should not exceed 2m.
• a stable and horizontal base which is rated for the weight of the complete analysis system (HYPERION microscope plus FT IR spectrometer plus data station possible acces­sories)
Environmental conditions:
Installation site: • a closed room, max. 2000m above sea level
• Ambient temperature range: 18°C - 30°C (64°F to 86°C)
• Ambient temperature variations: max. 1°C/h and max. 2°C/day (Temperature variations can impair the results of long-term measurements.)
• Humidity (non-condensing):
• The microscope should not be installed near vibration sources (e.g. ventilation hoods, air conditioners, motors elevators) or in rooms with intense floor vibrations.
• The microscope should not be installed near sources of potential inductive electrical interference (e.g. pumps, switching motors, microwave ovens etc.), sources of high energy pulses, and sources that might cause magnetic or radio frequency interference. These devices can interfere with the spectrometer and cause spectrometer malfunc­tion. Ensure that these types of devices are not connected to the same electrical circuit as the spectrometer.
70% (relative humidity)
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Installation 2
Power supply requirements:
Possibilities of inter­rupting the mains power supply:
The microscope power supply is realized by the supplied external power supply unit which has a wide input range. This means that it is able to adapt itself to the most com­mon public supply mains.
• Input range: 100 - 240 V AC, ~ 1,5V, 50 - 60 Hz
Connect the microscope only to a socket outlet with earth­ing contact that complies with VDE 0620-1 or IEC!
The microscope is constructed for the connection to a SELV (safety extra low voltage) circuit.
For safety reasons, make sure that the interfaces of electric accessories connected to the spectrometer comply with SELV (safety extra low voltage) circuit requirements. Nor­mally, this condition is met if the accessory design is based on the requirements described in EN 61010 or EN 60950.
If there are problems concerning main power supply (e.g. brownouts, power surges, frequent thunderstorms or power blackouts) use an UPS unit (U to ensure an uninterruptible power supply and conse­quently an operation without interruptions.
The mains power supply of the microscope can be inter­rupted as follows:
• 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
ninterruptible Power Supply)
Purge gas supply requirements:
Important: When preparing the installation site, take
into account that the mains power supply connections are easily accessible at any time.
• dry air or nitrogen gas (dew point < -40°C corresponds to 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.)
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Installation 2

2.6 Connecting the microscope to the power supply

2.6.1 General information

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.
Depending on the local conditions, the original power cord may need to be exchanged
i
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).

2.6.2 Safety note

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.
CAUTION
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Installation 2

2.6.3 Procedure

1 Make sure that the spectrometer is
switched off. To do this, check the setting of the ON/OFF switch
Switch position in off-state: O
①.
2
3
Connect the power cord connector of the external power supply unit
②.
Connect the low-voltage cable low-voltage socket rear side.
at the microscope
to the C5
to the
14
4
Connect the power plug cord to the mains socket outlet
Important note: Connect the power cord only to a socket outlet with earthing con­tact. Make sure that the socket complies with IEC.
of the power
②.
HYPERION User Manual Bruker Optik GmbH

2.7 Cable connections

Microscope rear side - total view
A
C
D
E
F
B
Microscope rear side - detail view
Spectrometer rear side - detail view
(For example purposes, it is a spectrome­ter of the TENSOR series.)
Rear side of the supplied PCs
Figure 2.1: Relevant connection sockets at the microscope (upper images), spectrometer (lower left image) and PC
(lower right image)
I
J
K
L
H
G
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.

2.7.1 Overview of the connection sockets

Installation 2
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Installation 2
Microscope
Fig. 2.1 Connection socket
A Z-IN: socket for connecting the cable which comes from the stage motor
B Z-OUT: socket for connecting the cable which is used for controlling the
C ACC.CONTROL 1, 2, 3: CAN BUS sockets for connecting the spectrome-
D DET.A: socket for connecting the signal transmission cable of the detector
which drives the motorized stage in z-direction
This cable is factory-connected to the stage motor.
motorized stage movement in z-direction
The cable for controlling the motorized stage movement in z-direction
comes from the PC.
ter and possibly additional accessories (e.g. HTS-XT module)
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
Fig. 2.1 Connection socket
G external detector
H CAN bus socket (for connecting the microscope)
PC
Fig. 2.1 Connection socket
16
I FPA detector
J Video signal cable
K Joystick
L motorized microscope stage
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 compo­nents. For detailed information about the other sockets, refer to the corresponding manual.
HYPERION User Manual Bruker Optik GmbH
Installation 2

2.7.2 Connecting the motorized microscope stage

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 computer­controlled or a joystick-controlled stage movement in z-direction.
The required cables are included in the delivery scope.
1 Connect the cables labeled X and Y to
the corresponding connectors right side of the motorized stage.
Important: Make sure that the labeling of the cables corresponds with the labeling of the stage connectors.
at the
2 In case the stage is equipped with two
motors, skip this step. In case the stage is equipped with an third motor, proceed as follows:
[1] Connect the cable, which is already
factory-connected to stage, to the Z- IN socket side.
[2] Connect the cable labeled Z to the Z-
OUT socket rear side.
3 At the other cable end, the cables labeled
X, Y and possibly Z are pooled together into one D-sub plug.
Insert this plug in the corresponding D­sub socket
at the microscope rear
at the microscope
at the PC.
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Installation 2

2.7.3 Connecting the joystick

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!
1

2.7.4 Connecting the video camera

1
Connect the 15-pole D-sub connector of the joystick cable to the corresponding male socket
Connect the video signal cable video camera to the S-VHS socket the converter box.
at the PC.
of the
of
Connect the USB cable verter box to an USB port
of the con-
at the PC.
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HYPERION User Manual Bruker Optik GmbH
Installation 2

2.7.5 Connecting the MCT detector(s)

HYPERION 1000 and HYPERION 2000 can be equipped with at most two MCT detec­tors; HYPERION 3000 with at most one MCT detector.
The required cables are included in the deliv­ery scope.
Between microscope and spectrometer, there is an A/D-converter analog detector signals coming from the micro­scope into digital signals. These digital signals are transmitted to the spectrometer electron­ics.
1 Connect the signal cable of the standard
MCT detector to the socket DET.A the microscope rear side.
which converts the
at
In case the microscope is equipped with a second MCT detector (option), connect the signal cable of this optional MCT detector to the socket DET.B microscope rear side.
2 Connect the signal cable coming from the
A/D converter to the corresponding socket
Note: In case of a spectrometer of the TENSOR series, a distributor box is required for connecting the second MCT detector.
at the spectrometer rear side.
at the
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Installation 2
Bottom side of the FPA detector compartment
A
Figure 2.2: Cable connectors of the FPA detector
E
D
B C

2.7.6 Connecting the FPA detector

Only HYPERION 3000 can be equipped with a FPA detector.
The following cables are included in the delivery scope of the FPA detector: :
Signal cable
Trigger cable
Power supply cable (including external power supply unit)
Fig. 2.2 Sockets and switches
A ON / OFF switch
B Outlet of the signal cable
CLED
Note: This LED lights green when the FPA detector is switched on.
D Socket for connecting the trigger cable
E Socket for connecting the power supply cable
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Installation 2
1 Connect the signal cable of the FPA
detector to the corresponding socket at the PC.
2 Connect the trigger cable to the RS42
Sync Input socket of the FPA detector compartment as well as to the corresponding socket spectrometer rear side.
Attention: Before connecting the
trigger cable, make sure that the spectrometer is switched off!
at the bottom side
at the
Note: In case of a spectrometer of the TENSOR series, a distributor box is required.
3 Connect the power supply cable to the
Power socket the FPA detector compartment.
The power is supplied by a dedicated external power supply unit. Connect this external power supply unit to a mains socket outlet.
Important note: Connect the power sup­ply cable only to a socket outlet with earthing contact socket complies with IEC.
at the bottom side of
⑤. Make sure that the
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Installation 2

2.7.7 Connecting the microscope to the spectrometer

The CAN BUS cable is included in the standard delivery scope of the microscope.
Note: Via this CAN BUS connection, the motor­ized mode mirrors inside the microscope are controlled in case the modes (transmission mode / reflection mode and viewing mode / measurement mode) are to be activated by the corresponding OPUS/VIDEO functions and not by pressing the corresponding buttons at the microscope control panel.
1 Connect the CAN BUS cable to the CAN
BUS socket side and to one of the three CAN BUS sockets
at the spectrometer rear
at the microscope rear side.
Note: The three CAN BUS sockets at the microscope rear side are labeled ACC.CONTROL. Connect the CAN BUS cable to one of them.
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Installation 2
A
B
Figure 2.3: Purge gas inlet (microscope rear side)

2.8 Connecting the microscope to the purge gas supply line

2.8.1 General information

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.
Fig. 2.3 Component
A Valve for controlling the purge gas flow rate
B Connection opening for the purge gas inlet hose

2.8.2 Procedure

The required hose is not included in the standard delivery scope of the microscope. It is
i
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.
Note: The connection opening has a lock ring which prevents the hose from being pulled out unintentionally.
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Installation 2
1
Insert the hose in the connection opening
①.
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.
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3Overview

3.1 Microscope variants

The HYPERION microscope is available in three different variants:
HYPERION 1000 - Basic variant
This variant is designed for IR spectro­scopic measurements in transmission and reflection. In addition, optional objec­tives (e.g. ATR objective, GIR objective) can be used with this microscope variant.
By default, it is equipped with a manually operated microscope stage which allows for single point measurements.
HYPERION 2000 - Advanced variant
This variant includes in addition a LCD color monitor and a motorized x/y-stage instead of a manually operated stage. The motorized x/y-stage allows for per­forming mapping measurements.
Bruker Optik GmbH HYPERION User Manual
HYPERION 3000 - Variant for imaging microscopic FT IR spectroscopy
This variant includes all technical fea­tures of the HYPERION 2000 variant plus a FPA detector for imaging FT IR spectroscopy.
25
Overview 3
A
B
C
D
E
F
Figure 3.1: HYPERION 2000 - Front view
G

3.2 Complete overview - operating elements & components

Front view
26
Fig. 3.1 Component / Control element
A Control panel
B Sample stage (motorized stage)
C Revolving nosepiece with objective(s)
D LCD monitor
E Binocular
F Video camera
G Rotating knobs for focussing the condenser
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Right side view
Figure 3.2: HYPERION 2000 - Right side view
B
C
E
H
F
G
A
I
D
Overview 3
Fig. 3.2 Component / Control element
A Brightness control
B Installation site of an optional aperture (aperture for confocal microscopy)
C Knife-edge aperture (manually operated type)
D Visible light routing control (i.e. control element for routing the light either
to the video camera or to the binocular)
E Operating elements of the LCD monitor
For detailed information about these operating elements, see
section 3.11.
F Detector comportment housing the optional detector
G Koehler aperture control (for opening and closing the iris aperture to set
the Koehler illumination in the reflection mode
H Rotating knobs for focussing (coarse and fine focus)
Note: In case of a motorized x/y/z-stage, joystick-controlled and computer­controlled focussing is possible. The third stage motor for a motorized stage movement in z-direction is an optional feature.
I Opening for coupling the spectrometer or an external accessory on the
right side of the microscope
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Overview 3
Figure 3.3: HYPERION 2000 - Left side view
A
B
C
D
F
G
E
Left side view
28
Fig. 3.3 Component / Control element
A Microscope lamp (visible light source for transmission microscopy)
B Opening for coupling the spectrometer or an external accessory on the
left side of the microscope
C Rotating knobs for focussing (coarse and fine focus)
Note: In case of a motorized x/y/z-stage, joystick-controlled and com­puter-controlled focussing is possible. The third stage motor for a motor­ized stage movement in z-direction is an optional feature.
D Microscope lamp (visible light source for reflection microscopy)
E Detector comportment housing the standard MCT detector
F Polarizer insertion slots (polarizers for visible and infrared light)
G Pinhole aperture for adjusting the condenser
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3.3 Operating panel

Figure 3.4: Operating panel
H
G
F
E
D
C
B
A
Overview 3
Fig. 3.4 Control element and explanation
A VIS/IR button: to activate the viewing and measuring mode.
Note: With this mode being activated, the sample can be viewed by means of the bin­ocular or on the monitor and a spectroscopic measurement can be performed. Acti­vating this button automatically deactivates the VIS button and the IR button.
B VIS button: to activate the viewing mode.
Note: With this mode being activated, the sample can only be viewed by means of the binocular or on the LCD monitor. Performing a spectroscopic measurement is not possible. Activating this button automatically deactivates the VIS/IR button and the IR button.
C IR button: to activate the measuring mode.
Note: With this mode being activated, only spectroscopic measurements can be per­formed, e.g. by operating the START button (H in fig. 3.4). Sample viewing is not pos­sible. Activating this button automatically deactivates the VIS button and the VIS/IR button.
D Brightness indicator: indicates the current brightness intensity of the visible illumi-
nation in relation to the maximum possible brightness intensity by means of a bar graph display.
Note: The brightness intensity can be adjusted by means of a thumb wheel (B in fig. 3.5).
E Reflection mode button: to activate the reflectance mode for reflection microscopy
and spectroscopic measurements in reflection. Use this mode in case of a reflecting sample.
Note: Activating this button automatically deactivates the transmittance mode button.
Bruker Optik GmbH HYPERION User Manual
F Transmission mode button: to activate the transmittance mode for transmission
microscopy and spectroscopic measurements in transmission. Use this mode in case of a transparent sample.
Note: Activating this button automatically deactivates the reflectance mode button.
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Overview 3
Figure 3.5: Adjusting the brightness intensity of the microscope illumination
A
B
C
Fig. 3.4 Control element and explanation
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 informa­tion 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 Ref­erence Manual.)

3.4 Brightness control and brightness indicator

Fig. 3.5 Control element and explanation
A Brightness indicator: indicates the current brightness intensity of the
visible illumination in relation to the maximum possible brightness inten­sity by means of a bar graph display.
B Brightness control: Thumb wheel for adjusting the brightness intensity
of the microscope illumination in a continuous manner.
C Icon legend to illustrate how to increase / decrease the brightness inten-
sity
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3.5 Microscope stages

3.5.1 Overview

Overview 3
Manual stage
This type of stage is standard for the HYPERION 1000 variant. It can be moved in x-, y- and z-direction only man­ually.
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 measure­ments 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 y­direction by means of a joystick and the corresponding OPUS functions. Optionally, a joystick- and computer-con­trolled 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 measure­ments 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 computer­controlled 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.
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Overview 3
Figure 3.6: Manual stage - Right side view
D
A
B
C

3.5.2 Manual stage

Fig. 3.6 Control element and explanation
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 micro­scope.
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.
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3.5.3 Focus control elements

Figure 3.7: Focus control elements (upper image: right side view,
lower image: left side view)
C
A
B
A’
C’
B’
Overview 3
Fig. 3.7 Control element and explanation
A and A’ Condenser focussing knob: to raise or lower the condenser in relation
to the sample or sample stage in order to maximize the beam intensity in transmittance mode.
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 con­trol.
C and C’ Fine focus knob: Using this rotary knob, the distance between sample
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.
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and objective is changed in smaller increments than with the coarse focus control.
33
Overview 3
Figure 3.8: Motorized stage (front view)
B
A

3.5.4 Motorized stage

Fig. 3.8 Component and Explanation
A Motorized sample stage
Note: After each computer reboot, the motorized stage needs to be reset (i.e. the stage needs to move to its home position x=0; y=0). See section 4.5.
B Joystick: to control the stage movement in x- and y-direction
Note: In case of a motorized x/y/z stage, a joystick-controlled stage movement also in z-direction is possible.
A joystick- or computer-controlled stage movement is only possible if the stage option
i
lstepMICstage has been selected when configuring the mapping device and the imaging device in OPUS. For performing mapping measurements with the ATR objective, the stage option stepATRMICstage needs to be selected. For information about how to con- figure the mapping device and the imaging device, refer to the OPUS/VIDEO Manual.
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3.5.5 Joystick-controlled stage movement

The movement of the motorized stage is con­trolled by the joystick as follows:
Stage movement in z-direction (focussing): Rotating the joystick clockwise Stage
moves downwards. Rotating the joystick coun­ter-clockwise Stage moves upwards.
When the stage is moved in z-direction
using the joystick, the stage is moved only by the fine drive.
Stage movement in x-direction: Tilting the joystick to the right or to the left
Stage movement in y-direction: Tilting the joystick forward or backward
Overview 3
The stage velocity in case of a movement in
horizontal plane depends on the tilt angle of the joystick: The larger the tilt angle, the faster the stage moves in the corresponding direction As soon as you release the joy­stick, it returns automatically to its center position and the stage stops.
A joystick-controlled stage movement is only possible if the corresponding functionality
i
is activated in OPUS. To check whether it is activated or to activate it, proceed as fol­lows: Select in the OPUS Measure menu the Non-video-assisted mapping measurement function. On the XY Stage dialog page, make sure that the Activate joystick checkbox is activate. If not, activate it now.
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Overview 3
Figure 3.9: Condenser (upper image: left side view, lower image: right side view)
D
A
C
D’
C’
B

3.6 Condenser

Fig. 3.9 Component and Explanation
A Pinhole aperture for adjusting the condenser
Note: The condenser is adjusted exclusively in the transmission mode.
B Condenser
C and C’ Condenser focussing knob: to raise or lower the condenser in relation
to the sample or sample stage in order to maximize the beam intensity in transmittance mode.
D and D’ Centering screws: to center the condenser by moving it in x- and/or y-
direction.
36
For detailed information about how to adjust the condenser, see section 4.6.
HYPERION User Manual Bruker Optik GmbH

3.7 Apertures

3.7.1 Overview

The apertures in the microscope have different functions:
•The knife-edge aperture is used to mask off that sample area which is not intended for spectroscopic analysis. The knife-edge aperture is a field dia­phragm.
The iris apertures are used for setting the Koehler illumination. The HYPERION microscope is equipped with two apertures of this type: one iris aperture for set­ting the Koehler illumination in transmission and another iris aperture for setting the Koehler illumination in reflection.
Depending on their locations, the pinhole aperture are used for adjusting the condenser and for narrowing the sample area used for analysis.
By default, the HYPERION microscope is equipped with the following apertures and dia­phragms:
Overview 3
Manual knife-edge aperture
This aperture is included in the standard delivery scope. Depending on the material of the knife edges, there are two types of knife-edge apertures available:
aperture with knife edges made of metal
aperture with knife edges made of glass
The knife-edge aperture with the metal knife edges can be used for measurements in VIS, NIR and MIR range, whereas the transparent knife edge aperture with the glass knife edges can only be used for measurements in the MIR range.
This aperture is used to narrow 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.
For information about how to operate the manual
knife-edge aperture, see section 3.7.3.
Iris aperture for setting the Koehler illumination in reflection
This aperture is included in the standard delivery scope. It is used for setting the Koehler illumination in case of reflection microscopy.
The lever for opening and closing the iris aperture (I in fig. 3.2) is at the right microscope side.
For information about how to operate this iris aper-
ture, see section 3.7.4.
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Overview 3
Iris aperture for setting the Koehler illumination in transmission
This aperture is included in the standard delivery scope. It is used for setting the Koehler illumination in case of transmission microscopy.
The knurled ring for opening and closing the iris aperture is below the condenser.
For information about how to operate this iris aper-
ture, see section 3.7.4.
Pinhole aperture for condenser adjustment
This aperture is included in the standard delivery scope. It is used for adjusted the condenser for transmitted light microscopy and for checking the signal intensity in the transmission.
For information about how to adjust the condenser,
see section 4.6. For information about how to check the signal intensity in the transmission mode, see section 4.7.1.
The pinhole aperture for checking the signal intensity in the reflection mode is included in the standard delivery scope only for validated analysis systems.
For information about how to check the signal inten-
sity in the reflection mode, see section 4.7.2
For information about the optional apertures, see section 5.2.
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3.7.2 Installation locations of the apertures

Figure 3.10: Apertures and their location in the microscope
A
B
C
E
F
D
Overview 3
Fig. 3.10 Aperture and explanation
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!
C Installation location for an additional aperture for measurements in reflection:
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: It is a confocal aperture which is located in the beam path before the sample.
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Overview 3
Figure 3.11: Operating elements of the manual knife-edge aperture
C
A
B
Fig. 3.10 Aperture and explanation
D Manual knife-edge aperture (with transparent knife edges made of glass):
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.
For information about how to operate this aperture, see section 3.7.3.
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

3.7.3 Manual knife-edge aperture

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 open­ing with the two opposite knife edges forming a pair each.
Fig. 3.11 Operating elements of the knife-edge aperture
40
A
Thumbwheels:
• increasing or reducing the distance between two opposite knife edges (i.e. setting the size of the
• rotating the complete knife-edge aperture with the previously adjusted 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.)
These two thumbwheels are used for realizing the following functions:
rectangular aperture opening
HYPERION User Manual Bruker Optik GmbH
)
rectangular
Fig. 3.11 Operating elements of the knife-edge aperture
Figure 3.12: Operating element of the aperture for setting Koehler illumination in reflection mode
Lever
Overview 3
B
C
Lever in front position:
rotated by max. 360° using the thumbwheels (A in fig. 3.11). In this case, the previ­ously 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.
Lever in back position:
two opposite knife edges (i.e. the size of the increased or reduced using the two thumbwheels (A in fig. 3.11). In doing so, the size of the
rectangular aperture opening is set.
When the lever is in the front position, the aperture can be
When the lever is in the back position, the distance between
rectangular aperture opening

3.7.4 Iris aperture for setting the Koehler illumination

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.
) can be
Lever position Aperture setting
Lever is pushed in completely. Aperture is open.
Lever is pulled out completely. Aperture is closed.
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.
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41
Overview 3
Knurled ring under­neath the condenser
Figure 3.13: Operating element of the aperture for setting Koehler illumination in transmission mode
Figure 3.14: a) Right microscope side - Light path
selector lever
A
B
C
b) Icon legend
Important note:
forget to open this aperture completely before starting a spectroscopic measurement.
This aperture is situated in the IR beam path. For this reason, do not

3.8 Light path selector lever

Fig. 3.14 Component and explanation
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
C If the lever is pulled out completely, the light is routed to the video camera. In this
42
case, the sample can be viewed only by looking through the binocular.
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 pro­gram. (Refer also to OPUS/VIDEO Manual.)
Note: The microscope variant HYPERION 1000 is not equipped with a LCD monitor.
HYPERION User Manual Bruker Optik GmbH

3.9 Revolving nosepiece and objectives

Figure 3.15: Revolving nosepiece with objectives
A
C
B
Overview 3
1
, GIR2) are avail-
Fig. 3.15 Component and explanation
A Revolving nosepiece: to attach objectives at the microscope and to posi-
tion the desired objective in the beam path with which you intend to work. Note: Depending on the dimensions of the objectives, up to four objec-
tives can be attached at the nosepiece at the same time. To place an objective in the optical path do NOT rotate the nosepiece by gripping an objective but the nosepiece itself. Rotate the nosepiece until the wanted objective is in the optical path. The nosepiece snaps automatically into the exact position, i.e. it clicks into position.
B Objectives
C Two vacant positions: If not used, they are covered with caps.
1. ATR - Attenuated Total Reflection (abgeschwächte Totalreflexion)
2. GIR - G
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.
Note: Before attaching an objective, remove the cap.
razing Incidence Reflection (Reflexion bei streifenden Lichteinfall)
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Overview 3
The following objectives are included in the standard delivery scope:
4x objective (with glass lens)
Due to its low magnification, it is primarily suitable for obtaining an overview of the sample if the viewing area of a higher magnification objective is not large enough.
Use this objective for sample viewing only. Do not use
it for performing IR spectroscopic measurements!
Reason: The glass lens of the objective absorbs light in the mid-infrared range.
15x objective (Schwarzschild)
This objective can be used for both sample viewing and IR spectroscopic measurements.
It is equipped with a transparent plastic sleeve on the outside. This sleeve can be pulled down. With the sleeve being pulled down, the area between the objec­tive and the microscope stage can be purged effec­tively with dry air or nitrogen gas. If required, the sleeve can be removed from the objective.
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 mea­surements and the 4x objective (for sample viewing only) can be attached at the revolv­ing 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 objec­tive, 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.
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3.10 Binocular

Figure 3.16: Binocular
B
A
Overview 3
Fig. 3.16 Component and explanation
A Binocular: to view the magnified sample image with both eyes.
The distance between the two eyepieces can be adjusted to the individual interpup­pillary distance. Each eyepiece of the binocular can be focussed separately. In the right eyepiece, there is a cross hairs.
B Interpupillary scale: to facilitate the readjustment of the binocular eyepieces to
your individual interpupillary distance. The interpupillary scale is on the left eye­piece. While looking through the binocular, increase or reduce the distance between the two eyepieces until you can view the sample comfortably.
An index mark next to the interpupillary scale indicates the currently adjusted inter­pupillary distance. This information facilitates the readjustment of your individual eyepieces distance at a later point in time.
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Overview 3
Figure 3.17: a) HYPERION 2000 (front side) b) Right microscope side- Operating elements of the LCD monitor
A
B
C
D
E
F

3.11 LCD monitor

The following microscope variants are equipped by default with a high-resolution, color LCD monitor: HYPERION 2000 and HYPERION 3000.
Fig. 3.17 Component and explanation
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.
D Input signal switch
This switch is inactive. Actuating this switch has no effect.
E ON / OFF switch: to switch on / off the LCD monitor
F LED display of the switching status of the LCD monitor
red LED: LCD monitor is switched off. green LED: LCD monitor is switched on.
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3.12 Detectors

Figure 3.18: a) HYPERION 1000
B’
A’
A
B
b) HYPERION 3000

3.12.1 Installation locations

All microscope variants of the HYPERION series have two detector compartments. In the left compartment, there is the standard MCT detector (single-element detector) cov­ering a spectral range from 12,000 - 600 cm equipped with an second detector.
The optionally available detectors are listed in section A.5.
Overview 3
-1
. Optionally, the right compartment can be
Fig. 3.18 Component and description
A and A’ HYPERION 1000 / 2000 / 3000: left detector compartment housing the
B HYPERION 1000 / 2000: right detector compartment housing an
B’ HYPERION 3000: right detector compartment housing the optional FPA
Bruker Optik GmbH HYPERION User Manual
standard MCT detector
optional MCT detector, if desired
detector
47
Overview 3

3.12.2 Types of 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 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 (ele­ment size: 0.25 mm x 0.25 mm).
This type of detector is designed for spectroscopic measurements in the mid-infrared range.
-1
.
FPA detector
The FPA detector can be installed in a HYPERION 3000 microscope only.
The FPA detector is a multi-element detector. The avail­able FPA detectors have a different number of detector elements.
See section A.5.
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3.13 Beam path

11
22
10
19
9
3
8
6
7
25
18
12
5
14b
13a
14a
13b
23
4
16
2
24
21
17
1
20
15
Figure 3.19: HYPERION 1000 and 2000 - Beam path in transmission mode and in reflection mode
Overview 3
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49
Overview 3
Figure 3.20: HYPERION 3000 - Beam path in transmission mode and in reflection mode
1
20
15
21
2
4
23
5
3
12
13a
13b
14a
14b
22
10
11
9
8
6
7
19
24
18
17
16
25
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Overview 3
Fig. 3.19 and 3.20
1 Visible light source (reflectance 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 situ­ated on the right side of the microscope (E in fig. 3.10).
3 Three-position motorized mirror
Position 1: Only visible light can pass. Position 2: Only IR light can pass. Position 3: Both visible light and IR light can pass. A beam splitter (Option A689-R) is required.
4 Aperture (optional): to define the measurement area in reflectance mode.
5 Four-position motorized mirror
Position 1: Transmittance mode (open). Position 2: Reflectance mode (glass beamsplitter), for visible light. Position 3) Reflectance mode for IR light (spectroscopic measurement) and VIS/IR (viewing and spectroscopic measurement). 50% of the light is reflected by a mirror. Position 4: Dichroic mirror that transmits only fluorescent light for fluorescence option
6Objective
Component and Description
7Sample
8 Aperture (manual or motorized knife-edge aperture): to define the sample area for the
analysis (transmittance or reflectance mode).
9 Three-position motorized mirror
Position 1: Viewing only (An opening allows visible light to reach the binocular eye­piece or the camera port.) Position 2: Spectral data acquisition only (IR beam is routed only to the detector using a mirror.) Position 3: Simultaneous viewing and spectral data acquisition (optional). (The IR beam is directed to the detector, while the visible light is routed to the binocular eye­piece or the camera port.)
10 Two-position, manually operated mirror
Position 1: All light goes to the binocular eyepiece (11). Position 2: All light goes to the camera port (22).
11 Binocular eyepiece: to view the sample.
12 Two-position detector selection mirror:
Position 1: IR beam is routed to the standard detector 1 (14a) Position 2: IR beam is routed to optional detector 2 (14b).
13a Mirror: routes IR beam to detector 1 (14a).
13b Mirror: routes IR beam to detector 2 (14b).
14a Infrared detector
14b IR detector or FPA detector (optional)
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51
Overview 3
Fig. 3.19 and 3.20
15 Visible light source for transmittance mode.
16 Three-position motorized mirror.
Position 1: Only visible light can pass. (hole) Position 2: Only IR light can pass. (mirror) Position 3: Both visible light and IR light can pass (Option A689-R). This option includes a beamsplitter.
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
19 Condenser (adjustable in height): to maximize the light intensity on the sample in
transmittance mode.
20 IR beam coming from the spectrometer.
21 Three-position motorized mirror.
Position 1: Mirror deflects the IR beam to the transmittance optics. Position 2: Mirror deflects the IR beam to the reflectance optics. Position 3: No mirror intercepts the IR beam. The beam can go to the external acces­sory port.
Component and Description
22 Video camera port
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).
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3.14 Possible instrumental setups

Figure 3.21: Examples of possible instrumental setups with the HYPERION microscope
HYPERION plus spectrometer
(standard)
HYPERION 3000 plus spectrometer plus IMAC
HYPERION plus vacuum
spectrometer plus bolometer
HYPERION plus spectrometer plus PMA50
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 FT­IR 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 cham­ber 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.
Overview 3
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Overview 3
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4Operation

4.1 General information

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.
For information about ...: refer to ...:
operating elements of the microscope chapter 3 in this manual
how to perform a video-assisted mea­surement
software-controlled operation of the motorized stage and resetting the motor­ized stage to its home position
how to set up the mapping device and the imaging device in OPUS
measurement parameters appendix B in this manual and the OPUS
how to operate the ATR objective section 4.12 in this manual
how to operate the motorized knife-edge aperture
how to perform continuous scan mea­surements with the FPA detector
how to validate FT IR spectrometer plus HYPERION microscope)
a
the analysis system (i.e.
OPUS/VIDEO Manual
OPUS/MAP and OPUS/VIDEO Manual
OPUS/VIDEO Manual
reference manual.
OPUS/VIDEO Manual
OPUS/FPA Manual
Procedure Guide OVP Test Procedure
b
Guide and VALIDATION Manual
For general information about OVP to the OPUS Reference Manual.
c
refer
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 - O
Bruker Optik GmbH HYPERION User Manual
PUS Validation Program (It is integral part of the OPUS software.)
55
Operation 4
①①①

4.2 Switching on / off the analysis system

Switching on the analysis system (Procedure without FPA detector)
Important: When switching on the complete analysis system (i.e. microscope
plus spectrometer plus PC), always keep to the following sequence of actions:
1. Switching on the microscope
Switch on the microscope. (switch posi­tion: I).
The ON/OFF switch scope rear side.
2. Switching on the spectrometer
Switch on the spectrometer. (switch posi­tion: ON).
The ON/OFF switch trometer rear side.
Refer to the user manual of the spec-
trometer in question.
is at the micro-
is at the spec-
3. Switching on the PC and the monitor
For information about this topic, refer to the corresponding user manuals.
Switching on the analysis system (Procedure with
Important: When switching on the complete analysis system (i.e. microscope
with FPA detector plus spectrometer plus PC), always keep to the following sequence:
1. Switching on the microscope
Switch on the microscope. (switch posi­tion: I).
The ON/OFF switch scope rear side.
2. Switching on the spectrometer
Switch on the spectrometer. (switch posi­tion: ON).
The ON/OFF switch trometer rear side.
Refer to the user manual of the spec-
FPA detector)
is at the micro-
is at the spec-
trometer in question.
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HYPERION User Manual Bruker Optik GmbH
Operation 4
3. Cooling down the FPA detector with liquid nitrogen to its operating tempera­ture
See section 4.4
4. Switching on the PC and the monitor
For information about this topic, refer to the corresponding user manuals.
5. Switching on the FPA detector
The ON/OFF switch side of the FPA detector compartment
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.
is at the bottom
Switching off the analysis system
Note: When switching off the analysis system, there is no strict sequence of
actions you have to observe.
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57
Operation 4

4.3 Preparing the microscope for a spectroscopic measurement

After having switched the analysis system and before starting your sample analyses, you have to do the following preparatory works:
Action Notes / remarks / references
Checking whether the detector is cooled down to its operating temperature. If not, cool down the detector using liquid nitro­gen.
Resetting the motorized microscope stage to its home position (i.e. x=0; y=0).
Note: Skip this step if the microscope is equipped with a manual stage.
Checking the condenser setting and cor­recting it, if required.
Note: This is only in the transmission mode of relevance.
Checking the signal intensity
Note: The detector temperature warn­ing indicator (G in fig. 3.4) is situated on the operating panel of the micro­scope. 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
The motorized stage is reset using the corresponding OPUS function.
For information about how to reset
the motorized stage, refer to the OPUS/VIDEO Manual and/or the OPUS/MAP Manual.
For information about how to
adjust the condenser, see section 4.6.
For information about how to
check the signal intensity, see section 4.7
58
In addition, the performance of the analysis system (microscope plus spectrometer)
should be checked in regular time intervals which can be defined by the user in OVP (OPUS Validation Program). The performance can be checked by performing a PQ test (P intend to perform spectroscopic measurements. For detailed information about this topic, refer to the OPUS Reference Manual.
erformance Qualification) for the measurement channel with which you
HYPERION User Manual Bruker Optik GmbH

4.4 Cooling the detector

4.4.1 General information

The operating temperature of the available MCT detectors and FPA detectors is signifi­cantly 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 time 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 dis­appeared 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.
1
of the detector in question, the cooling procedure needs to be repeated in
Operation 4
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.

4.4.2 Safety notes

The temperature of the liquid nitrogen is minus 196°C (minus 320.8°F.)
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 pro­vide sufficient protection.
WARNING
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.
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Operation 4
Filling hole for stan­dard MCT detector
Filling hole for optional MCT detector
HYPERION 1000 and HYPERION 2000
HYPERION 3000
Filling hole for standard MCT detector
Filling hole for optional FPA detector

4.4.3 Funneling liquid nitrogen in the detector

The procedure is identical for both types of detector - MCT and FPA.
1
2
Open the corresponding filling hole by removing the plug and insert the funnel.
Note: The funnel is included in the deliv­ery scope.
Pour slowly liquid nitrogen into the funnel. Avoid spilling the liquid nitrogen on the microscope housing.
Pour liquid nitrogen only in a filling hole underneath which a detector is installed. Otherwise the microscope will get dam­aged.
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Operation 4
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-
2
gen is still very large, the liquid nitrogen may squirt out forcefully. Therefore observe the 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 fill­ings. Note that the first two funnel fillings will evaporate almost completely at the begin­ning.
Avoid overfilling the dewar! Otherwise the liquid nitrogen flows out.
3
4
After having poured in sufficient liquid nitrogen, remove the funnel and reinsert the plug in the filling hole.
Wait about 20 minutes before starting the first spectroscopic measurement to allow
the detector to stabilize thermally.
Special notes regarding the FPA detector
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 opera­tion 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.
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Operation 4

4.5 Resetting the motorized stage

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 crys­tal 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.
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Operation 4

4.6 Checking and correcting the condenser setting

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.
Checking the condenser setting
1
Make sure that the beam path is not obstructed, for example by a polarizer, a
2
3
4
sample or a closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Swing the 15x objective the beam path.
Activate the viewing/measur­ing mode by using the VIS/IR­button panel.
Activate the transmission mode by using the corre­sponding button operating panel.
on the operating
in
on the
5
Bruker Optik GmbH HYPERION User Manual
Move the pinhole aperture in the beam path by rotating the thumb wheel direction of the small circle.
in the arrow
63
Operation 4
6
Make sure that the light path selector lever completely, i.e. the light is routed to the binocular.
View through the binocular.
When you see a sharp image of a bright circle which is aligned to the center of the cross hairs, then the con­denser is set optimally.
is pushed in
7
When you see an unsharp image and / or the bright cir­cle is not aligned to the center of the cross hairs, then the condenser height needs to be adjusted and / or the con­denser needs to realigned in x- and / or y-direction.
When the check has revealed that the condenser is set opti­mally, rotate the thumb wheel
in the arrow direction of
8
the big circle to move the pin­hole aperture out of the beam path again.
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Correcting the condenser setting
Operation 4
In case of an unsharp image, focus on the bright circle using the con­denser focussing knobs
In case the circle is not aligned to the center of the cross hairs, move the condenser in x- and/or y-direction using the centering screws the circle is correctly aligned to the cross hairs center.
①.
in until
Attention: After having set the con­denser correctly, do not forget to move the pinhole aperture out of the beam path again by rotating the thumb wheel
in the arrow direction of the big cir-
cle.
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65
Operation 4
The amplitude value indicates the currently detected signal intensity.
Interferogram option button (activated)
Interferogram

4.7 Checking the IR signal intensity

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.

4.7.1 Procedure in transmission mode

First check the condenser setting and correct it, if required.
1
2
For information about this topic, see section 4.6.
Note: The condenser is set correctly, when you a sharp image of a bright circle and
the circle is aligned to the center of cross hairs when you look through the binocular.
Activate the measuring mode by actuat­ing the IR button panel of the microscope.
Make sure that the transmission mode is activated.
on the operating
3
4
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Open the OPUS software program. Select in the Measure menu the
Advanced Measurement function. Load an adequate experiment file.
For information about the available
standard experiment files, see appendix B.
Click in the Measurement dialog on the Check Signal tab.
Make sure that the Interferogram option button is activated.
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Operation 4
Amplitudenwert im Transmissionsmodus
For verifying the currently detected IR signal intensity, compare the amplitude value displayed in OPUS (see image in step 4) with the amplitude value for the transmission mode stated in the supplied OVP test protocol (see image in step 5).
The supplied test protocol Hyperion OVP Supplementary Sheet documents the result of a factory-performed signal check
5
using your analysis system. The test has been performed with all optics compo­nents being optimally adjusted. You will find the test protocol in the folder supply with the microscope.
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.
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Operation 4

4.7.2 Procedure in reflection mode

1
2
3
4 Place the supplied gold mirror on the microscope stage underneath the objective.
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
Swing the 15x objective path.
Activate the viewing mode by actuating the VIS button of the microscope.
Activate the reflection mode by actuating the corresponding button operating panel of the microscope.
Make sure that the light path selector lever is pushed in completely, i.e. the light is routed to the binocular.
on the operating panel
in the beam
on the
5
View through the binocular and adjust the brightness using the corresponding thumb wheel illuminated.
6
7
Focus on the mirror surface.
Note: In case the mirror surface is free of scratches, focus on a mirror edge.
until the image is well-
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HYPERION User Manual Bruker Optik GmbH
Define a measurement area of 100 x 100 µm using an aperture.
Operation 4
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).
Non-validated analysis system and manual knife-edge aperture:
Define the measurement area as shown in the lower image using the manual knife-edge aperture
For information about how to operate
the manual knife-edge aperture, see section 3.7.3.
Note: 100 microns correspond to 5 scale lines of cross hairs in the binocular (but not in the OPUS video view!).
Validated analysis system and pinhole aperture for reflection mode:
Define the measurement area as shown in the lower image using the pinhole aperture for the reflection mode this, swing the aperture in the beam path by rotating the thumb wheel arrow direction of the small circle up to the stop.
Note: Only validated analysis systems are equipped by default with this aper­ture.
⑥.
. To do
in the
Bruker Optik GmbH HYPERION User Manual
The result of this aperture setting is a cir­cular image of the mirror surface and the circular measurement area has a diame­ter of 100 µm.
69
Operation 4
The amplitude value indicates the currently detected signal intensity.
Interferogram option button (activated)
Interferogram
Microscope with motorized knife-edge aperture (option):
Define the measurement area as shown in the lower image using the motorized knife-edge aperture
For information about how to operate
the motorized knife-edge aperture, refer to the OPUS/VIDEO Manual.
Important note: Because the motorized knife-edge aperture is operated exclu­sively via the OPUS/VIDEO software, make sure that the light is routed to the video camera. In case the light path selector lever (see be pulled out completely.
⑧.
in step 5) needs to
9
10
Activate the measuring mode by actuat­ing the IR button panel of the microscope.
Open the OPUS software program. Select in the Measure menu the
Advanced Measurement function. Load an adequate experiment file.
For information about the available
standard experiment files, see appendix B.
Click in the Measurement dialog on the Check Signal tab.
Make sure that the Interferogram option button is activated.
on the operating
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11
Amplitudenwert im Reflexionsmodus
Operation 4
For verifying the currently detected IR signal intensity, compare the amplitude value displayed in OPUS (see image in step 10) with the amplitude value for the reflection mode stated in the supplied OVP test protocol (see image in step 11).
The supplied test protocol Hyperion OVP Supplementary Sheet documents the result of a factory-performed signal check using your analysis system. The test has been performed with all optics compo­nents being optimally adjusted. You will find the test protocol in the folder supply with the microscope.
12
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.
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.
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Operation 4
ATR crystal in the lower position
Contact pressure level display

4.7.3 Procedure with ATR objective

Important: First become thoroughly familiar with the ATR objective. For infor-
mation about how to operate the ATR objective, see section 4.12.
Swing the ATR objective path.
Attention: Potential risk of damaging
1
2
3
Make sure that the beam path is not obstructed, for example by a polarizer, a sample or a closed knife-edge aperture (i.e. the knife-edge aperture has to be open completely).
the ATR crystal by hitting the stage!
Before swinging the ATR objective in the beam path, make sure that the stage is low enough. If this is not the case, first lower the stage.
Activate the reflection mode by actuating the corresponding button operating panel of the microscope.
Bring the ATR crystal in the measuring mode position (i.e. lower position).
See section 4.12.4
in the beam
on the
72
4
Set the contact pressure level 1 at the ATR objective.
See section 4.12.5.
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Operation 4
The amplitude value indicates the currently detected signal intensity.
Interferogram option button (activated)
Interferogram
Put the plastic ring position the ring concentrically below the ATR objective.
Note: The plastic ring is included in the
6
7
delivery scope of the ATR objective.
Move the stage slowly upwards (i.e. in z­direction) until the plastic ring brings the ATR crystal in the focus position.
For information about how to move
the stage in z-direction, see section 3.5.
Reaching the focus position is indicated acoustically by a beep and optically by the In-focus LED crystal has reached the focus position, the In-focus LED turns from red to green for a short moment. Then it goes off.
on the stage and
. When the ATR
8
9
Activate the measuring mode by actuat­ing the IR button panel of the microscope.
Open the OPUS software program. Select in the Measure menu the
Advanced Measurement function. Load an adequate experiment file.
For information about the available
standard experiment files, see appendix B.
Click in the Measurement dialog on the Check Signal tab.
Make sure that the Interferogram option button is activated.
on the operating
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Operation 4
Amplitude value with ATR objective
10
For verifying the currently detected IR signal intensity, compare the amplitude value displayed in OPUS (see image in step 9) with the amplitude value with ATR objective stated in the supplied OVP test protocol (see image in step 10).
The supplied test protocol Hyperion OVP Supplementary Sheet documents the result of a factory-performed signal check using your analysis system. The test has been performed with all optics compo­nents being optimally adjusted. You will find the test protocol in the folder supply with the microscope.
12
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.
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.
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4.8 Checking the detector saturation

Figure 4.1: Spectrum acquired with a normally saturated detector
Enlarged section
This option but­ton needs to be activated.
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 mea­surement. If the detector is oversaturated, the IR spectroscopic measurement may not yield meaningful results.
Procedure
1. Prepare the microscope for a background or sample measurement in transmittance
or reflectance.
For measurements in transmittance, see section 4.10. For measurements in reflec-
tance, see section 4.11.
2. Activate the measuring mode by actuating the IR button (C in fig. 3.4) on the operat-
ing panel of the microscope.
3. Start the OPUS software. Select in the Measure menu the Advanced Measurement
function. Load an adequate experiment file (’*’.xpm).
For information about the available standard experiment files, see appendix B.
4. Click in the Measurement dialog on the Check Signal tab. Make sure that the Spec-
trum option button is activated. (See fig. 4.1.)
Operation 4
The spectrum in fig. 4.1 results from a normal detector saturation.
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75
Operation 4
Figure 4.2: Spectrum acquired at a beginning oversaturation of the detector
Enlarged section
Figure 4.2 shows a spectrum acquired at a beginning oversaturation of the detector. When the detector is totally oversaturated, the spectrum may have a completely different appearance, for example a cosine curve or a zero line.
Reducing the IR signal intensity in case of a detector oversaturation
In case an oversaturated detector, you can:
close the manual or motorized knife-edge aperture somewhat
select in OPUS a smaller spectrometer aperture (max. 3 mm or smaller) (Note: This solution variant involves the potential risk of forgetting to undo this aperture setting afterwards again.)
only in case of HYPERION 3000: insert a beam attenuator in the optical adapta­tion box between microscope and spectrometer
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Operation 4

4.9 Viewing the sample and selecting the measurement area

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):
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:
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 reflect­ing).
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 sub­strate material.)
5.
Swinging an objective with a suitable magnification in the beam path:
mally use the 15x IR-objective for viewing the sample and searching for areas of inter­est. 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
6.
Focussing on the sample: does not hit the objective while you move the stage upwards for focussing purposes.
7.
Setting the brightness:
is illuminated optimally. wise. (Note: The currently set tor at the microscope control panel. See fig. 3.4.)
Attention:
T
emporary eye irritations may occur. In this case, close your eyes for about one
minute until the irritation has disappeared.
8.
Optimizing the image contrast:
nation. Which of the two apertures of this type you have to use depends on the mea­suring 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 voltage is changed. This has an effect on the color temperature.
9.
Moving the microscope stage in x- and/or y-direction
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 rent knife-edge aperture setting it is important that the currently used objective and the objective selected in OPUS are identical.
Do not look through the binocular when the brightness is set at maximum.
(B in fig. 3.5)
(e.g. 15x IR-
Set the brightness in such a way that the sample in question
Always start with a low
instead! With the brightness control, the microscope lamp
OPUS/VIDEO Manual. For taking a snapshot of the cur-
You can activate the VIS mode either by actuat-
You can activate
Note: Nor-
objective
Make that the sample on the stage or the stage itself
brightness
using the iris aperture for setting the Koehler illumi-
.
or 20x ATR-
brightness
level is indicated by the
objective)!
level and increase it step-
until you find a sample area
brightness
indica-
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Operation 4

4.10 Viewing and measuring a sample in transmission

Operating step Corresponding operating element(s)
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.
3. Put the sample on the stage and posi-
tion it in the beam path.
4. Swing the 15x objective in the beam
path. Note: For large samples, use the 4x
objective with glass lens. With the 4x objective, however, spectroscopic mea­surements cannot be performed. So do not forget to swing an IR objective (e.g. 15x, 36x) in the beam path before start­ing a measurement.
5. Set the microscope either for sample
viewing through the binocular or for video image display.
Note: It is recommended to use the video image displayed on the monitor.
revolving nosepiece
Light path selector lever (A in fig 3.14)
6. Adjust the brightness starting with a
low brightness level. Caution: Do not look through the binocu-
lar when the brightness is set at maxi­mum. Temporary eye irritations may occur.
78
either the thumb wheel of the bright­ness control at the microscope (B in fig. 3.5) or the brightness control in the OPUS video wizard
The currently set brightness is dis­played by the brightness indicator (A in fig. 3.5).
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Operation 4
Operating step Corresponding operating element(s)
7. Focus on the sample. Manual stage and motorized x/y­stage: coarse and fine focus knobs at
the microscope (B/B’ and C/C’ in fig. 3.7)
Motorized x/y/z-stage: Joystick and corresponding stage control functions in OPUS
See OPUS/VIDEO Manual.
8. Enhance the image contrast by closing
the iris aperture for setting the Koehler illumination in transmission.
Attention: Do not forget to reopen this aperture before starting a spectroscopic measurement!
9. Activate the transmission mode. either the transmission button on the
10. Move the stage in x- and/or y-direc-
tion to find a sample area which is of interest to you.
Iris aperture for setting the Koehler illu­mination (B in fig. 3.10)
Knurled ring underneath the condenser
operating panel (F in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
Manual x/y-stage: Rotary knobs (A and B in fig. 3.6)
Motorized x/y-stage: Joystick and cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
11. Take a snapshot of the video image of
the sample.
12. Mask off that sample area which is
not intended for spectroscopic analysis.
Bruker Optik GmbH HYPERION User Manual
corresponding OPUS function See OPUS/VIDEO Manual.
Manual knife-edge aperture (D in 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.
79
Operation 4
Operating step Corresponding operating element(s)
13. Take a snapshot of the video image with aperture.
Note:
In case of a manual knife-edge aperture, it is advisable to take a snapshot in order to be able to reconstruct the aper­ture setting later, if required.
14. Save the current stage position. Note: This is only possible in case of a
motorized stage. In case of a manual stage, skip this step.
15. Move the stage in x- and/or y-direc­tion until a sample-free area of the sub­strate is in the beam path.
Note: Make sure that the detector does not oversaturate. Do not change the set­ting of the knife-edge aperture!
corresponding OPUS function See OPUS/VIDEO Manual.
corresponding OPUS function See OPUS/VIDEO Manual.
Manual x/y-stage: Rotary knobs (A and B in fig. 3.6)
Motorized x/y-stage: Joystick and cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
16. Move the pinhole aperture in the beam path. If required, correct the con­denser setting. Note: When you see a sharp image of a bright circle which is aligned to the center of the cross hairs, then the condenser is set correctly. After­wards, move the pinhole aperture out of the beam path again.
17. Activate the measuring mode. either using the IR button on the oper-
18. Start the background measurement. Attention: Before starting the measure-
ment, open the iris aperture for setting the Koehler illumination in transmission (B in fig. 18) again. See step 8.
Thumb wheel of the pinhole aperture for setting the condenser (A in fig. 3.9), condenser focussing knobs (C/C’ in fig. 3.9) and centering screws (D/D’ in fig. 3.9)
See section 4.6.
ating panel of the microscope (C in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
corresponding OPUS function See OPUS/VIDEO Manual. Iris aperture for setting the Koehler illu-
mination (B in fig. 3.10) Knurled ring underneath the condenser
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Operation 4
Operating step Corresponding operating element(s)
19. Move the stage in x- and/or y-direc­tion to return to the sample area, you have chosen in step 10.
In case of a motorized stage, return the stage to the x/y-position, you have saved in step 14.
20. Check again the condenser setting. If required, readjust the condenser height.
21. Start the sample measurement. corresponding OPUS function
Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
Manual x/y-stage: Rotary knobs (A and B in fig. 3.6)
Motorized x/y-stage: Joystick and cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
Thumb wheel of the pinhole aperture for setting the condenser (A in fig. 3.9) and the condenser focussing knobs (C/ C’ in fig. 3.9)
See section 4.6.
See OPUS/VIDEO Manual.
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Operation 4

4.11 Viewing and measuring a sample in reflection

Operating step Corresponding operating element(s)
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.
3. Put the sample on the stage and position it in the beam path.
4. Swing the 15x objective in the beam path.
Note: For large samples, use the 4x objective with glass lens. With the 4x objective, however, spectroscopic mea­surements cannot be performed. So do not forget to swing an IR objective (e.g. 15x, 36x) in the beam path before start­ing a measurement.
5. Set the microscope either for sample viewing through the binocular or for video image display.
Note: It is recommended to use the video image displayed on the monitor.
revolving nosepiece
Light path selector lever (A in fig 3.14)
6. Adjust the brightness starting with a low brightness level.
Caution: Do not look through the bin­ocular when the brightness is set at maximum. Temporary eye irritations may occur.
82
either the thumb wheel of the brightness control at the microscope (B in fig. 3.5) or the brightness control in the OPUS video wizard
The currently set brightness is displayed by the brightness indicator (A in fig. 3.5).
HYPERION User Manual Bruker Optik GmbH
Operation 4
Operating step Corresponding operating element(s)
7. Focus on the sample. Manual stage and motorized x/y­stage: coarse and fine focus knobs at
the microscope (B/B’ and C/C’ in fig. 3.7) Motorized x/y/z-stage: Joystick and
corresponding stage control functions in OPUS
See OPUS/VIDEO Manual.
8. Enhance the image contrast. Lever for operating the iris aperture for setting the Koehler illumination in reflec­tion (fig. 3.12 and E in fig. 3.10)
9. Move the stage in x- and/or y-direc-
tion to find a sample area which is of interest to you.
10. Take a snapshot of the video image
of the sample.
11. Mask off that sample area which is
not intended for spectroscopic analysis.
Manual x/y-stage: Rotary knobs (A and B in fig. 3.6)
Motorized x/y-stage: Joystick and cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
corresponding OPUS function See OPUS/VIDEO Manual.
Manual knife-edge aperture (D in 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.
12. Take a snapshot of the video image
with aperture.
Note:
In case of a manual knife-edge aperture, it is advisable to take a snap­shot in order to be able to reconstruct the aperture setting later, if required.
Bruker Optik GmbH HYPERION User Manual
corresponding OPUS function See OPUS/VIDEO Manual.
83
Operation 4
Operating step Corresponding operating element(s)
13. In case of a motorized stage:
13.1. Save the current x/y-stage posi­tion.
13.2. Put the supplied gold mirror on the stage and move the stage in x- and/ or y-direction until the mirror is in the beam path. Do NOT change the posi-
tion of the sample on the stage!
13. In case of a manual stage: Put the supplied gold mirror on the
stage and move the stage in x- and/or y-direction until the mirror is in the beam path.
14. Focus on a mirror edge or on a scratch of the mirror surface.
Note: The mirror surface needs to be clean! Do NOT change the knife-edge aperture setting!
Motorized stage: Step 13.1. corresponding OPUS function Step 13.2. Joystick / corresponding
OPUS function See OPUS/VIDEO Manua.
Manual stage: Rotary knobs (A and B in fig. 3.6)
Manual stage and motorized x/y­stage: coarse and fine focus knobs at
the microscope (B/B’ and C/C’ in fig. 3.7) Motorized x/y/z-stage: Joystick and
corresponding stage control functions in OPUS
See OPUS/VIDEO Manual.
15. Activate measuring mode. either using the IR button on the operat­ing panel of the microscope (C in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
16. Start background measurement. corresponding OPUS function 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.
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Operation 4
Operating step Corresponding operating element(s)
18. Return to the sample area you have chosen in step 9 for spectroscopic anal­ysis.
In case of the manual stage, move the stage in x- and/or y-direction until you have found the sample area in question again.
In case of a motorized stage, return the stage to the x/y-position, you have saved in step 13.1.
19. Focus on the sample. Manual stage and motorized x/y-
Manual x/y-stage: Rotary knobs (A and B in fig. 3.6)
Motorized x/y-stage: Joystick and cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
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 corresponding stage control functions in OPUS
See OPUS/VIDEO Manual.
21. Activate measuring mode. either using the IR button on the operat­ing panel of the microscope (C in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
20. Start the sample measurement. corresponding OPUS function
See OPUS/VIDEO Manual.
Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
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Operation 4

4.12 ATR objective - Important operating notes

4.12.1 General handling instructions

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.
Important note: Spectroscopic measurements performed with a damaged ATR
crystal do not deliver reliable measurement results!

4.12.2 Cleaning the ATR crystal

Before each measurement, check whether the ATR crystal is clean (i.e. free of any parti­cles 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, isopro­pyl), if required.
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Operation 4

4.12.3 Attaching the ATR objective at the revolving nosepiece

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.
Attaching the ATR objective at the revolving nosepiece
Position the ATR objective at the nose­piece with the two recesses ing towards the two neighboring objective positions at the revolving nosepiece.
point-
Screw on the objective by rotating the knurled locking ring so, the ATR objective is not yet
1
2
attached firmly at the revolving nose­piece.
Finally, to attach the ATR objective firmly by inserting the supplied pin in a hole of the knurled locking ring rotating the knurled locking ring clock­wise as far as it will go.
Important: Afterwards, check whether the outer casing of the ATR objective can be moved up and down all the way without being hindered by other objective.
Connecting the ATR objective to the microscope
Connect the cable of the ATR objec­tive at the corresponding socket the left microscope side.
. Note: In doing
and
at
To remove the ATR objective from the nosepiece, first disconnect the cable than detach the objective.
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Operation 4
Viewing mode
ATR crystal in upper position
Measuring mode
ATR-crystal in lower position

4.12.4 Setting the viewing mode / measuring mode at the ATR objective

The 20x ATR objective allows for both sample viewing by means of the micro­scope and spectroscopic analysis using the measurement techniques ATR (attentuated total reflection) or reflection.
For this purpose, the ATR crystal is brought either in the upper position (viewing mode) or in the lower position (measuring mode).
88
Setting the viewing mode:
Actuate the rocker switch the outer casing tive all the way up at the same time.
Then, release the rocker switch again.
Setting the measuring mode:
Actuate the rocker switch the outer casing tive all the way down at the same time.
Then, release the rocker switch again. Attention: When setting the measur-
ing mode, take care that the ATR crys­tal tip
Potential risk of damaging the ATR crystal!
HYPERION User Manual Bruker Optik GmbH
does not hit the stage.
of the ATR objec-
of the ATR objec-
and push
and pull

4.12.5 Setting contact pressure levels

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 pres­sure 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.
Operation 4
Setting a contact pressure level:
Actuate the rocker switch the outer casing tive down until it snaps into place at the desired pressure level.
Note: The currently set contact pres­sure level is indicated by the red point of the pressure level display
Then, release the rocker switch again.
of the ATR objec-
and pull
④.

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!
Attention: When setting a contact pressure level, take care that the ATR crystal tip
Potential risk of damaging the ATR crystal!
does not hit the stage.
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Operation 4
In measuring mode
Proceed as follows:
1
2
3
Bring the ATR crystal in the measuring mode position (i.e. lower position). See section 4.12.4.
Set a contact pressure level which is adequate to the degree of hardness of the sample you intend to analysis.
See section 4.12.5.
Focussing for the background mea­surement
Put the plastic ring Position the ring concentrically under­neath the ATR objective. Make sure that the ring does not yet contact the ATR objective.
Note: The plastic ring is included in the delivery scope of the ATR objective.
Focussing for the sample measure­ment
Put the sample on the stage under­neath the ATR objective.
on the stage.
Focus by moving the stage slowly upwards until the ATR crystal is pressed in the focus position by plastic ring or the sample. In case of a man­ual stage or a motorized x/y-stage, use the fine focus knobs (C/C’ in fig. 3.7). In case of a motorized x/y/z stage, use the joystick.
Note: The focus position is indicated acoustically by a beep and optically by
4
the In-focus LED crystal has reached the focus position, the In-focus LED turns from red to green for a short moment. Then it goes off.
Red: ATR crystal is not in focus posi­tion.
Green: ATR crystal is in focus position.
Note: In case the ATR crystal is in the viewing mode position, the In-focus LED does not light at all.
②. When the ATR
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Operation 4

4.13 Measuring a sample with the ATR objective (single point measurement)

Operating step Corresponding operating element(s)
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.
3. Put the sample on the stage.
4. Swing the ATR objective in the
beam path. Bring the ATR crystal in the viewing
mode position (i.e. upper position). Set a contact pressure level which is
adequate to the degree of hardness of the sample you intend to analyze.
5. Set the microscope either for sam-
ple viewing through the binocular or for video image display.
Note: It is recommended to use the video image displayed on the monitor.
ATR objective See section 4.12.4 and section
4.12.5
Light path selector lever (A in fig 3.14)
6. Move the stage in x- and/or y-direc-
tion to find a sample area which is of interest to you.
Bruker Optik GmbH HYPERION User Manual
Manual stage: Rotary knobs (A and B in fig. 3.6)
Motorized stage: Joystick and corre­sponding stage control functions in OPUS
See OPUS/VIDEO Manual.
91
Operation 4
Operating step Corresponding operating element(s)
7. Mask off that sample area which is not intended for spectroscopic analy­sis.
Note: In case of the ATR objective, the measuring spot diameter is about 32 µm.
8. Move the stage downwards. Manual stage and motorized x/y-
9. Exchange the sample for the plastic ring. Place the plastic ring underneath the ATR objective.
Manual knife-edge aperture (D in 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.
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 cor­responding stage control functions in OPUS
See OPUS/VIDEO Manual.
Note: The plastic ring is included in the delivery scope of the ATR objective.
10. Bring the ATR crystal in the mea­suring mode position (i.e. lower posi­tion).
Note: Do not change the contact pres­sure level you have set in step 4.
11. Activate the measuring mode at the microscope.
12. 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 tal 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 crys-
ATR objective See section 4.12.4.
either using the IR button on the operat­ing panel of the microscope (C in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
Manual stage and motorized x/y­stage: 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. See also section 4.12.6.
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Operating step Corresponding operating element(s)
13. Start background measurement. OPUS software See OPUS/VIDEO Manual.
Operation 4
14. Move the stage downwards as far
as it will go. Exchange the plastic ring for the sample.
15. Bring the ATR crystal in the view-
ing mode position (i.e. upper position).
16. Activate the viewing mode at the
microscope.
Manual stage and motorized x/y­stage: 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.
ATR objective See section 4.12.4.
either the VIS button on the operating panel (B in fig. 3.4) or in the OPUS video wizard
See OPUS/VIDEO Manual.
17. Focus on the sample by moving
the stage slowly upwards.
18. Find a sample area which you
intend to analyze spectroscopically by moving the stage in x- and/or y-direc­tion.
Bruker Optik GmbH HYPERION User Manual
Manual stage and motorized x/y­stage: 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.
Manual stage: Rotary knobs (A and B in fig. 3.6)
Motorized stage: Joystick and corre­sponding stage control functions in OPUS
See OPUS/VIDEO Manual.
93
Operation 4
Operating step Corresponding operating element(s)
19. Move the stage downwards as far as it will go.
20. Bring the ATR crystal in the mea­suring mode position (i.e. lower posi­tion).
Note: Do not change the contact pres­sure level you have set in step 4.
21. Activate the measuring mode at the microscope.
Manual stage and motorized x/y­stage: 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.
ATR objective See section 4.12.4.
either using the IR button on the operat­ing 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 until the ATR crystal tip contacts the sample and the ATR crystal is pressed in the focus position.
Note: The focus position is indicated acoustically by a beep and optically by the In-focus LED tal has reached the focus position, the In-focus LED turns from red to green for a short moment. Then it goes off.
23. Start the sample measurement. OPUS software
Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
. When the ATR crys-
Manual stage and motorized x/y­stage: 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. See also section 4.12.6.
See OPUS/VIDEO Manual.
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Operation 4

4.14 Measuring a sample with the ATR objective (mapping measurement)

Special technical requirements
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)
Software • optional software package OPUS/ATR (for controlling the
stage movement in z-direction)
Configuring the mapping device and the imaging device - Specials
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.
Mapping device • lstepATRMICstage
Imaging device An imaging device especially intended for ATR mapping
measurements must include the following components:
• Microscope/Device: Hyperion2000 or Hyperion3000 or a HYPERION1000 microscope which has been upgraded with a motorized x/y/z-stage and the option A673-FA
• Objective: 20x ATR
• Electronic options: Autofocus
• Motorized X/Y stage: lstepATRMICstage
For detailed information about how to configure the mapping device and the imag-
ing device, refer to the OPUS/VIDEO Manual.
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Operation 4
Procedure
Operating step Corresponding operating element(s)
1. Select in the OPUS Measure menu the Video-assisted Measurement function.
Load an experiment file which meant for ATR mapping (e.g. HYPERION_ ATR­Objective_Map.XPM)
(See also appendix B.)
2. Reset the motorized stage. OPUS/VIDEO or OPUS/MAP
3. Prepare the microscope for the back­ground measurement:
3.1. Activate the measuring mode and the reflection mode at the microscope.
3.2. Bring the ATR crystal in the measur­ing mode position (i.e. lower position). Set a contact pressure level which is adequate to the degree of hardness of the sample you intend to analyze.
3.3. Swing the ATR objective in the beam path.
Caution: Before swinging the ATR objec­tive in the beam path, make sure that the stage is low enough so that the crystal will not hit the stage. Attention: Potential risk of damaging the ATR crystal!
3.4. Place the plastic ring on the stage 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 has reached the focus position, the In­focus LED turns from red to green for a short moment. Then it goes off.
. When the ATR crystal
OPUS software
See section 4.5.
3.1. Operating panel: IR button and reflection mode button (C and E in fig. 3.4)
3.2. ATR objective (See section 4.12.4 and section 4.12.5.)
3.3. revolving nosepiece with ATR objective
3.4. Plastic ring which is included in the delivery scope of the ATR objective.
3.5. corresponding OPUS functions (See OPUS/MAP and OPUS/VIDEO Manual.) See also section 4.12.6.
Note: In case an imaging device has been selected in OPUS which is meant for ATR mapping (see operating step 1), the joystick-controlled stage movement in z-direction is automatically disabled!
4. Start the background measurement. OPUS software See OPUS/VIDEO Manual.
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Operation 4
Operating step Corresponding operating element(s)
5. Move the stage downwards as far as it will go. Exchange the plastic ring for the sample.
Note: For ATR mapping, it is advisable to fixate the sample on the stage in order to the prevent the sample from slipping out of position during the automatic mea­surement procedure.
6. Prepare the microscope for sample viewing:
6.1. Activate the viewing mode at the microscope.
6.2. Bring the ATR crystal in the viewing mode position (i.e. upper position).
6.3. Set the microscope for video image display.
6.4. Set the brightness optimally.
6.5. Set the image contrast optimally.
6.6. Focus on the sample.
6.7. Move the stage in x- and/or y-direc­tion to find a sample area which you intend to analyze spectroscopically.
corresponding OPUS functions
See OPUS/MAP and OPUS/VIDEO
Manual.
Note: The joystick-controlled stage movement in z-direction is automatically disabled!
6.1. Operating panel: VIS button (B in fig. 3.4) or OPUS video wizard
6.2. ATR objective (See section 4.12.4.)
6.3. Light path selector lever (A in fig. 3.14)
6.4. Brightness control thumb wheel (B in fig. 3.5)
6.5. Iris aperture for setting the Koehler illumination in reflection (E in fig. 3.10)
6.6. Coarse and fine focus knob (B and C in fig. 3.7)
Note: The joystick-controlled stage movement in z-direction is automatically disabled!
6.7. Joystick or corresponding OPUS functions
7. Take a snapshot or acquire a compos­ite overview image of the sample and define the desired measurement posi­tions.
8. Prepare the microscope for the sample measurement:
8.1. Activate the measuring mode at the microscope.
8.2. Bring the ATR crystal in the measur­ing mode position (i.e. lower position).
Note: Do not change the contact pres­sure level you have set in step 3.2.!
8.3. Move the stage upwards until the distance between sample and ATR crys­tal tip is less than 2 mm.
Bruker Optik GmbH HYPERION User Manual
OPUS video wizard See OPUS/VIDEO Manual.
8.1. operating panel: IR button (C in fig. 3.4) or OPUS video wizard
8.2. ATR objective (See section 4.12.4.)
8.3. Coarse and fine focus knob (B and C in fig. 3.7)
Note: The joystick-controlled stage movement in z-direction is automatically disabled!
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Operation 4
Operating step Corresponding operating element(s)
9. Start the sample measurement. OPUS software See OPUS/VIDEO Manual.
Afterwards, OPUS calculates automatically the result spectrum of the sample and displays
the sample spectrum in the OPUS spectrum window.
General information about the automatic measurement procedure
After you have started the sample measurement in OPUS, the ATR mapping measure­ment 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 acousti­cally by a beep and optically by the In-focus LED 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.
. When the ATR crystal has
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