Vertex 70vs Manual

VERTEX 70v User Manual

1007253

1st edition 2007, publication date November 2007

© 2007 BRUKER OPTIK GmbH, Rudolf Plank Str. 27, D-76275 Ettlingen, www.brukeroptics.com

All rights reserved. No part of this manual may be reproduced or transmitted in any form or by any means including printing, photocopying, microfilm, electronic systems etc. without our prior written permission. Brand names, registered trademarks etc. used in this manual, even if not explicitly marked as such, are not to be considered unprotected by trademarks law. They are the property of their respective owner.

The following publication has been worked out with utmost care. However, Bruker Optik GmbH does not accept any liability for the correctness of the information. Bruker Optik GmbH reserves the right to make changes to the products described in this manual without notice.

This manual is the original documentation for the VERTEX 70v spectrometer.

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T. .ABLE OF C ONTENTS ..................................... 1 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Warning Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Safety Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

2 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 3 Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Delivery Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Site Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Connecting VERTEX 70v to the Power Supply . . . . . . . . . . . . . . . . . . . 11 Connecting VERTEX 70v to a PC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Connecting VERTEX 70v to the Vacuum Pump . . . . . . . . . . . . . . . . . . 13 Connecting VERTEX 70v to the Purge Gas Line . . . . . . . . . . . . . . . . . . 15

4 Overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . External Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Internal Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Optical Path . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

19 20 25 29

5 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Switching VERTEX 70v On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . QuickLock. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Automatic Accessory Recognition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Performing a Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Evacuating and Venting the Spectrometer. . . . . . . . . . . . . . . . . . . . . . . Optimizing the Vacuum Operation of the Spectrometer. . . . . . . . . . . . . Purging the Spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Exchanging the Beamsplitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Exchanging the Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cooling an MCT Detector. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

31 31 33 35 35 36 40 43 46 50 52

6 Maintenance and Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Evacuating the MCT Detector Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Laser Module. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing a defective IR Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Fuses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . VERTEX 70v User Manual

57 58 61 66 68 iii

Ta b l e o f C o n t e n t s Replacing the Sample Compartment Windows . . . . . . . . . . . . . . . . . . . 69 Cleaning the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73 Maintaining the Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

7 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75 Diagnostic Means. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76 Problem - Possible Cause - Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

A Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101 B Consumable Spares . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103 C Default Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105 D Dimensional Drawings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109 E Connecting VERTEX 70v to PC . . . . . . . . . . . . . . . . . . . . . . 115 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Possible Connection Topologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Selecting Network Addresses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Assigning Network Addresses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Checking the Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

115 116 119 120 123

F Electronics and Power Supply . . . . . . . . . . . . . . . . . . . . . . . 125 Electronics Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125 Power Supply Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

G Firmware Update . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Updating the Firmware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Restoring a previous Firmware Version . . . . . . . . . . . . . . . . . . . . . . . . Backing up the current Firmware Version . . . . . . . . . . . . . . . . . . . . . .

131 132 134 135

H Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137 General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137 Sample Preparation Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

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Service Addresses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145

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S. . A. .F. E. .T. Y. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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GENERAL INFORMATION

.......................................................... Read the following safety instructions carefully before putting the spectrometer into operation. Keep this manual in a suitable place for future reference. Always observe the instructions described in this manual to ensure user safety and to avoid property damage. Improper use or failure to follow these safety instructions can result in serious injuries and/or property damage. Any non-observance of the precautions will infringe the intended use (i.e. performing spectroscopic measurements) of the spectrometer. In this case Bruker Optik GmbH will not assume any liability. 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 spectrometer is in proper functioning condition. A safe and faultless operation can only be guaranteed if the spectrometer is transported, stored, installed, operated and maintained properly according to the procedures described in this manual. Never remove or deactivate any supporting safety systems during spectrometer operation. Ensure that objects and/or material not required for the measurement is out of the spectrometer operating area. The spectrometer complies with the IEC/EN 61010-1 safety regulations.

Protective Earthing To avoid personal injuries and/or property damage caused by electrical power, the spectrometer is equipped with a safety plug. Connect this plug only to a socket outlet with earthing contact. Make sure that the socket complies with IEC (International Electrotechnical Commission).

Qualified Personnel Primary installation and all maintenance and repair works not described in this manual should only be performed by Bruker service personnel. Only authorized operating personnel that have been briefed about the spectrometer operation and all relevant safety aspects should operate and maintain (i.e. only maintenance works that are described in this manual) the spectrometer. All repairs, adjustments and alignments on any spectrometer component must be performed in accordance with the safety regulations and standards applied in the country in which the instrument is installed. VERTEX 70v User Manual

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SAFETY Warning Labels

Correct Usage The spectrometer and its components should only be used according to the instructions described in the manual or advised by a Bruker engineer. In case of accessories or components made by other manufacturers and used in connection with the spectrometer, Bruker does not assume any liability for safe operation and proper functioning.

WARNING LABELS

.......................................................... When operating the spectrometer you have to observe a number of safety instructions which are highlighted by various warning labels. This section describes the warning labels and explains their meaning. All warning labels on the spectrometer must always be kept legible. Immediately replace a worn or damaged label. The following warning labels indicate different dangerous situations which may be caused by improper use of the spectrometer.

Caut ion - Ge ne ral H azar d This warning symbol indicates general hazard. Observe the safety instructions and follow the precautions described to avoid personal injury and/or property damage.

Caution - Electrical Shock This warning symbol indicates electrical hazard. The symbol is located near live parts or on enclosures behind which are live parts that represent an accidental contact hazard. Never touch these parts. Before removing the corresponding compartment covers and beginning any maintenance or repair work, first turn off the mains switch and unplug the main power cable. Ensure that all live parts do not come into contact with a conductive substance or liquid. Non-observance of these safety instructions can cause severe personal injury and/or property damage.

Caution - Hot Surface This warning symbol indicates components and surfaces which can become very hot during spectrometer operation. Do not touch these components and surfaces. Risk of skin burn! Be careful when operating near hot components and/or surfaces.

Caution - Laser Radiation This warning symbol indicates the existence of laser radiation. Never look directly into the laser beam or use any kind of optical instruments to do so. Otherwise permanent eye damage can be the result.

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VERTEX 70v User Manual

Caution - Frostbite This warning symbol indicates cryogenic materials (e.g. liquid nitrogen) required to operate the spectrometer (e.g. cooling detector). Skin contact with these liquids or cooled components causes severe frostbite. Always handle the liquids with utmost care. Observe the safety instructions for handling of cryogenic liquids.

Caution - Ha rmful Material This warning symbol indicates the existence of harmful or irritant material (e.g. the window material BaF2). Observe the safety instructions on the packaging, and the safety data sheets attached. Non-observance may cause personal injury.

Caution - Toxic Material This warning symbol indicates the existence of toxic material (e.g. the window material KRS-5). Observe the safety instructions on the packaging, and the safety data sheets attached. Non-observance may cause severe personal injury or even death.

Besides the dangers described above, there can also be hazardous situations caused by the sample material. Depending on the type of hazardous substances you work with, you have to observe specific substance-relevant safety instructions. Put on the corresponding warning label on the appropriate spectrometer position. The label must be legible and permanently discernible. The following list contains some examples of hazardous substances:

Caution - Infectious Material This warning symbol indicates the possible presence of bio-hazardous and infectious material. When working with this kind of material always, observe the prevailing laboratory safety regulations and take all necessary precautions and disinfection measures (e.g. wearing protective clothing, masks, gloves etc.). Failure to do so may cause severe personal injury or even death. (For information on how to use, dilute and efficiently apply disinfectants, refer to the Laboratory Biosafety Manual: 1993 by WHO - World Health Organization.)

Caution - Radioactive Material This warning symbol indicates the possible presence of radioactivity. When working with radioactive material, always observe the safety regulations and take all necessary protective measures (e.g. wearing protective clothing, masks gloves etc.). Failure to do so may cause severe personal injury or even death.

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SAFETY Warning Labels

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SAFETY Safety Instructions

Caution - Corrosive Substance This warning symbol indicates the possible presence of corrosive substances. When working with corrosive substances, always observe the laboratory safety regulations and take protective measures (e.g. wearing protective masks and gloves). Failure to do so may cause severe personal injury or even death.

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 local waste regulations.

SAFETY INSTRUCTIONS

.......................................................... The following chapters describe all relevant safety aspects of the spectrometer operation. Depending on the degree of hazard the safety instructions are classified as follows: Danger

indicates that death, severe personal injury or substantial property damage WILL result if proper precautions are not taken.

Warning

indicates that death, severe personal injury or substantial property damage CAN result if proper precautions are not taken.

Caution

indicates that minor personal injury or property damage CAN result if proper precautions are not taken.

Note

draws your attention to particularly important information on the product, e.g. product operation or to a special part of the manual.

The safety instructions Danger, Warning and Caution stand out by the corresponding warning labels.

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VERTEX 70v User Manual

G. . E. .N. E. .R. A. .L. . . . . . . . . . . . . . . . . . . . . . . . . . .

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VERTEX 70v is an evacuable, fully digital FT-IR spectrometer for demanding R&D applications. The spectrometer is equipped with a number of features such as AAR (Automatic Accessory Recognition) ACR (Automatic Component Recognition) and PerformanceGuard that facilitate performing spectroscopic measurements and ensure reliable measurement results. The function AAR identifies automatically the accessory installed in the sample compartment, performs several tests and loads automatically the corresponding experiment file including the pre-defined measurement parameters. The feature ACR recognizes automatically the currently installed optical components like source, detector and beamsplitter. These components are electronically coded so that the spectrometer firmware can recognize them. This information is passed on to the application software OPUS. The purpose of ACR is to enable the user to select the right optics parameters in OPUS. In addition, the spectrometer components are monitored permanently to ensure that they operate within the specification range. This feature is called Performance Guard. Its purpose is to facilitate fault diagnostics and maintenance. The data acquisition is based on a free running delta-sigma, dual-channel A/D converter with 24-bit dynamic range. The A/D converter is integrated into the detector preamplifier electronics. The DigiTect technology ensures a signal transmission free from interferences and guarantees the highest signal-to-noise ratio. VERTEX 70v can be controlled by any data system (PC workstation, notebook etc.) on which the operating system Microsoft Windows and the spectroscopic software OPUS is installed. The Ethernet connection provides the possibility to control the spectrometer also via your intranet or the internet. The standard spectrometer configuration is designed for data acquisition in the mid IR region. Optionally, VERTEX 70v can be equipped with additional optical components to cover the whole spectral range - starting in the far infrared or THz region at 10cm-1 up to the ultraviolet region at 28,000cm-1. Due to the pre-aligned optical components and the permanently aligned RockSolid interferometer, the spectral range can be changed easily. If you work with the advanced spectrometer configuration (i.e. two detector positions and two source positions are available inside the spectrometer) you can select them using the software. Removable vacuum-tight covers provide access to the detector and beamsplitter if you want to exchange these components. VERTEX 70v has five IR-beam outlet ports (on the right, front and left side) and two IRbeam inlet ports (on the right and rear side) allowing the connection of a multitude of optional accessories and/or components like: • TGA-coupling • PMA 50 (Polarization Modulation Accessory for VCD and PM-IRRAS) • HYPERION 1000/2000 IR microscope and HYPERION 3000 imaging microscope with FPA detector (Focal Plane Array detector system) • IMAC module (Imaging Accessory with FPA detector) VERTEX 70v User Manual

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GENERAL

• External sample compartment (XSA) • HTS-XT module (High Throughput Screening Extension) • Fiber optic coupling module with MIR or NIR fiber probes for solid and liquid samples • FT Raman module (e.g. RAM II) • FIR bolometer • External, water-cooled sources There is also the possibility to connect several accessories simultaneously (e.g. a water-cooled Hg-arc source at the rear side, the RAM II FT-Raman module at the right side, a fibre optics coupling at the right front side, the HYPERION IR microscope at the left side and a bolometer detector at the front side). Diagnostic routines help to maintain optimum instrument status and performance. The internal validation unit (IUV) is located inside the spectrometer. It contains standards (test samples) used for the validation and testing of the instrument. Note: Depending on the spectrometer configuration you have ordered, your spectrometer may not include all options that are described in this manual. The evacuable VERTEX 70v spectrometer allows measurements under vacuum conditions, i.e. unwanted atmospheric interferents (e.g. water vapor or carbon dioxide) are eliminated nearly completely from the spectrometer interior. Evacuating the spectrometer is more efficient than purging it or using desiccant cartridges. The result of an optimal measurement under vacuum conditions is an IR spectrum in which no H2O or CO2 absorptions mask weak spectral features of the sample. The spectrometer design enables a separate evacuation of the spectrometer compartments, i.e. either the complete spectrometer interior (sample compartment plus the optical bench) or only the optical bench can be evacuated. Vacuum shutters (so called flaps), which can be equipped with optical or IR windows, allow a ventilation of only the sample compartment in order to preserve the vacuum in the rest of the optics compartment during a sample exchange or an accessory installation. Evacuating and venting the sample compartment and/or optics are computer-controlled. Moreover, the spectrometer is equipped with two pressure sensors providing for the display of the current pressure inside the spectrometer optics and/or sample compartment. VERTEX 70v is supplied with an efficient vacuum pump that can evacuate the spectrometer optics within a few minutes. The oil-free vacuum pump prevents the spectrometer optics from being contaminated by hydrocarbons.

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VERTEX 70v User Manual

I.N. .S. TA LLATION .................................

3

GENERAL INFORMATION

.......................................................... Unpacking and initial installation of VERTEX 70v is done by Bruker service engineers. The operating company has to provide an installation site that meets the site requirements described in this chapter. (See also the technical document Installation Requirements for VERTEX 70v provided by Bruker Optik GmbH in advance.) This chapter contains a list of the standard as well as the optional spectrometer components and describes the procedures for connecting the spectrometer:

• • • •

to the power supply, to a PC, to the vacuum pump and to the purge gas supply line, if necessary.

For detailed information about how to install the computer, refer to the PC manual.

DELIVERY SCOPE

.......................................................... The basic instrument of VERTEX 70v allows upgrading with additional components and/ or accessories. The delivery scope depends on the spectrometer configuration you have ordered.

Standard Components The basic instrument includes the following items:

• VERTEX 70v spectrometer (including the user manual) • Power cord • PC compatible data system (if desired, the PC can also be provided by the customer)

• Data cable (Cat5, crossover cable for 10Base-T Ethernet standard) • Purge gas hose (OD: 6mm, length: approx. 5m) • Tool kit (slot-head screw driver, cross-head screwdriver and hex keys of several sizes, sample preparation tools, 3x spare fuses, IR sensor card, metallic cap shown in fig. 28)

• Software package OPUS/IR (including the OPUS Reference Manual)

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INSTALLATION Delivery Scope

For installing the vacuum pump, the following items are included:

• • • • • •

Vacuum pump (including the user manual) Noise reduction hood Vibration absorber 2x flexible metal hoses 4x hose clamps 4x sealing rings

Optional Components Depending on the ordered spectrometer configuration, the delivery scope can also include following optional components:

• Optional spectrometer components (e.g. optional detectors) and/or accessories • Optional OPUS software packages (e.g OPUS/STEP) including the corresponding manuals

Inspecting the Packaging After the receipt of the spectrometer, inspect the packaging for damages. If there are any signs of damage, contact your local shipping representative before opening the shipping box. Warning: Do not put a spectrometer into operation that shows signs of damage. Failure to do so may result in severe personal injuries and/or property damage.

Transportation Due to its weight (about 105kg), VERTEX 70v has to be carried by at least four persons using the supplied transport handles. For transportation purposes, attach these handles properly to the right and left spectrometer side as shown in figure 1 using 12 screws (M5 x 16). Tighten the screws using a hex kex (size 4mm). After having transported the instrument to the desired place, you can remove the transport handles again. Alternatively, you can transport the instrument with a fork lifter. Warning: Due to the high instrument weight, improper transportation can lead to personal injuries and/or spectrometer damage.

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VERTEX 70v User Manual

Transport Handles

Figure 1: Installing the Transport Handles

SITE REQUIREMENTS

..........................................................

Space Requirements The spectrometer dimensions are 85cm (w) x 71cm (d) x 32cm (h). (For exact spectrometer dimensions refer to appendix D.) At the rear side, the spectrometer requires a clearance of at least 25cm (10“). The spectrometer should be placed on a stable and horizontal base. Note that the basic instrument has a weight of about 105kg. When preparing the installation location for the spectrometer, take into consideration that the mains power supply connection is easily accessible at any time. The mains power supply can be interrupted, for example, either by disconnecting the safety plug or switching off the mains switch on the spectrometer rear side or disconnecting the primary power receptacle.

Environmental Requirements To ensure optimum spectrometer performance and long-term reliability the following environmental conditions are essential: Temperature Range:

18 - 35 °C (64 - 95 °F)

In case the vacuum pump is operated with installed noise reduction hood ensure the ambient temperature does not exceed 32°C (90°F). Humidity (non-condensing): ≤ 80% (relative humidity) Temperature variations can impair the results of long-term measurements. Therefore, the temperature variations should be less than 1°C per hour and should not exceed 2°C per day for this type of measurement. VERTEX 70v User Manual

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INSTALLATION Site Requirements

3

INSTALLATION Site Requirements

Vibration Ideally, the spectrometer should not be installed near vibration sources (e.g. ventilation hoods, air conditioners, motors, elevator etc.) or in rooms with intense floor vibration.

Power Supply The spectrometer power supply unit automatically adapts to the most common power sources. Valid voltage range: 100 V AC to 240 V AC Valid frequency range: 50 to 60 Hz VERTEX 70v is an instrument of the protection class I. Caution: To avoid personal injury and spectrometer damage, connect the spectrometer only to a socket outlet with earthing contact. To provide for good data quality and a long spectrometer service life, ensure that the following site requirements are met:

• Do not install the spectrometer 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.

• Do not place devices such as large electric motors, heaters, welding equipment, radio transmitting equipment, units emitting pulsed NMRs, or high powered lasers in close vicinity to the spectrometer. 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.

• If a reliable mains power supply is a problem at your site (caused by brownouts, power surges, frequent thunderstorms, for example), take precautions to ensure an uninterruptible power supply.

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VERTEX 70v User Manual

CONNECTING VERTEX 70V TO THE POWER SUPPLY ..........................................................

Pow er Cord Before connecting the power cord, make sure that the spectrometer is switched off, i.e. the mains switch (B in figure 2) is in the “O” position. Connect the supplied power cord to the primary power receptacle (C in figure 2) as well as to the mains socket outlet. The power cord length should not exceed 3m. Depending on the local conditions, the original power cord may need to be exchanged for a power cord that complies with the standards of the country in question. The power cord must have approbation of at least your local authority, UL for US, CSA for Canada or VDE for Europe. The spectrometer power supply unit automatically adapts to the local voltage and frequency range. (See section Site Requirements.)

A

B

C

Figure 2: Spectrometer Rear Side - Connections for Power Supply and PC

Component A

Ethernet port

B

Mains switch

C

Primary power receptacle (for connecting the power cord)

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INSTALLATION Connecting VERTEX 70v to the Power Supply

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INSTALLATION Connecting VERTEX 70v to a PC

CONNECTING VERTEX 70V TO A PC ..........................................................

Data Cable The data cable included in the spectrometer delivery scope is a CAT5 crossover cable (labelled “Cross-over”) with two RJ-45 plugs. This cable is only used for the direct connection of VERTEX 70v to a computer. If you intend to connect the spectrometer to a network, a different type of cable (i.e. non-crossover, CAT 5 cable for the 10Base-T Ethernet standard) is required. (See appendix E.) The data cable length should not exceed 100m (without repeater). Connect one end of the data cable to the Ethernet port (ETH) (A figure 2) and the other end of the data cable to the RJ-45 socket of the computer network interface card. (For detailed information refer to the computer manual.) After having set up the data cable connection, turn on the spectrometer using the mains switch. After a few seconds, the spectrometer beeps once and starts a self test. After the initialization has been completed successfully, the “STATUS” LED (figure 10) turns from red to green. Now switch on the computer and the monitor. (For information on how to install the computer and how to set up signal and power cable connections for the computer, monitor etc. refer to the computer manual.)

Computer Setup VERTEX 70v and the delivered PC are already configured for the stand-alone operation. The spectrometer IP address is factory-set to 10.10.0.1. In case you have not purchased the computer together with the VERTEX 70v spectrometer, you have to assign an appropriate IP address to the computer to which you want to connect the spectrometer. For detailed information about how to assign an IP-address to the computer refer to appendix E.

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CONNECTING VERTEX 70V TO THE VACUUM PUMP ..........................................................

The attachment flange (NW25 flange) for connecting the vacuum pump is at the spectrometer rear side. Figure 3 shows the valve block with removed cover. Attachment Flange for the Vacuum Pump

Valve for evacuating the optical bench

Valve for evacuating the sample compartment

Valve for venting the optical bench

Valve for venting the sample compartment

Opening for venting the optical bench

Opening for venting the sample compartment

(Note: When purging the spectrometer this port is used as purge gas inlet for the optical bench.

(Note: When purging the spectrometer this port is used as purge gas inlet for the sample compartment. Figure 3: Valve Block (Spectrometer rear Side)

The vent openings are covered by a plug made from sintered-powder metal which is airpermeable (i.e. the spectrometer can be vented with the plugs installed on the vent opening). (See figure 8.) The plug functions like a filter preventing particles from entering the spectrometer together with the influent air. Note:

For detailed information about the vacuum pump refer to the user manual provided by the vacuum pump manufacturer.

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INSTALLATION Connecting VERTEX 70v to the Vacuum Pump

3

INSTALLATION Connecting VERTEX 70v to the Vacuum Pump

Installation Procedure • Remove the valve block cover shown in figure 4 by loosening the two Allen screws using a hex key (size 3mm) and pulling off the cover. Allen Screws

Valve Block Cover

Figure 4: Removing the Valve Block Cover

• Install the supplied sealing ring at the attachment flange. See figure 5. Attachment Flange

Sealing Ring

Flexible Metal Hose

Figure 5: Connecting VERTEX 70v to Vacuum Pump - Step 1

• Press the supplied flexible metal hose against the attachment flange (figure 6a) and attach the hose to the flange using the supplied hose clamp (figure 6b). Secure the hose clamp by fastening the wing screw.

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VERTEX 70v User Manual

Wing Screw

Hose Clamp

Figure 6: Connecting VERTEX 70v to Vacuum Pump -Step 2

During operation, the vacuum pump generates vibrations. In order to prevent these vibrations from being transferred to the spectrometer via the flexible metal hose, the supplied vibration absorber has to be installed between the vacuum pump and the spectrometer. The procedure for connecting the flexible metal hose to the vacuum pump and to the vibration absorber is identical to the procedure described above. Note:

Make sure that the vibrating metal hoses do not come into contact with the table on which the spectrometer is placed.

During the operation, the vacuum pump produces an increased noise level. In order to reduce the noise level install the supplied noise reduction hood over the vacuum pump. For information about the noise reduction hood installation refer to instructions provided by the pump manufacturer.

CONNECTING VERTEX 70V TO THE PURGE GAS LINE ..........................................................

As an alternative to the vacuum operation, VERTEX 70v can be purged with either dry air or dry nitrogen gas. The spectrometer has two purge gas inlets; one for purging the sample compartment and the other for purging the optical bench. The purge gas inlets are at the spectrometer rear side. See figure 7.

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

Purge gas inlet for optical bench.

Purge gas inlet for sample compartment.

(Note: In case of vacuum operation - vent opening for venting the optical bench.)

(Note: In case of vacuum operation - vent opening for venting the sample compartment.) Figure 7: Purge Gas Inlets

For detailed information about the required purge gas supply conditions refer to chapter Operation, section Purging the Spectrometer.

Installation Procedure Note:

In case the spectrometer is evacuated, first vent it before starting the installation procedure. Otherwise, a warning message regarding unstable pressure conditions inside the spectrometer will appear.

• To connect the spectrometer to the purge gas supply you need a stiff hose with an outer diameter of 6mm. Remove the plug (made from sintered-powder metal) from the purge gas inlet by pressing the lock ring inwards (figure 8) and pulling out the plug. Connect one end of the hose to your supply line for dry air or dry nitrogen gas and insert the other end of the hose into the purge gas inlet for either the sample compartment or optical bench.

• If you want to purge both the sample compartment and the optical bench, you need a T-shape connecting hose with two hose ends leading to the spectrometer. After having connected the main end of the hose to the supply line, insert one of the other two hose ends into the purge gas inlet for the sample compartment and the other hose end into the purge gas inlet for the optical bench.

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VERTEX 70v User Manual

Lock Ring

Plug

Figure 8: Purge Gas Inlet with removed Plug

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

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O. . V. .E. R. .V. I. E. .W. . . . . . . . . . . . . . . . . . . . . . . . . . GENERAL INFORMATION

.......................................................... This chapter describes all relevant external and internal spectrometer components. Note: The local indications right and left assume that the operator stands in front of the spectrometer. The indications forward and backward refer to the spectrometer front side and rear side, respectively. G H A B C

D

E I F

Figure 9: General Overview

Compartment A

Power Supply Connector

B

Status Indicator Board

C

Electronics Compartment

D

Interferometer Compartment

E

Detector Compartment

F

Sample Compartment

G

Laser

H

Vacuum Pump Connection Port

I

Beam Direction Control Compartment

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OVERVIEW External Components

The detector compartment, the interferometer compartment and the beam direction control compartment are not separated from each other but form one compartment. All spectrometer compartments are accessible by removing the corresponding cover.

EXTERNAL COMPONENTS

..........................................................

Status Indicator Board The status indicator board is in the left rear corner of the spectrometer, more precisely, on the electronic compartment cover. (See figure 10.) The color of the LEDs gives a general indication of the operating status of the corresponding spectrometer component. Moreover, the color of the Vacuum LED indicates the current pressure situation inside the spectrometer compartments (i.e it shows whether a certain compartment is being evacuated/vented just now or is already evacuated/vented). In case one of these LEDs lights up red indicating a spectrometer problem refer to chapter Troubleshooting. This chapter shows possible causes of a problem and provides solutions.

Figure 10: Status Indicator Board

VACUUM The color of VACUUM LED depends on the current pressure situation inside the individual spectrometer compartments. The following table explains the meaning of the different LED colors: LED is off.

Sample compartment and optical bench are vented.

LED flashes green.

Sample compartment and optical bench are being either evacuated or vented.

LED lights up green.

Sample compartment and optical bench are evacuated. The ultimate vacuum is achieved.

LED flashes yellow.

Sample compartment is being either evacuated or vented. (In case the sample compartment is already vented, it flashes yellow also when the optical bench is being vented.)

LED lights up yellow.

Sample compartment is vented.

LED lights up red.

When the spectrometer is being evacuated, but a certain threshold pressure value is not reached within a certain period of time (i.e. the ultimate vacuum is not achieved). A red VACUUM LED indicates a problem. See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator.

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LASER The LASER LED lights green when the laser is in operation and the laser signal is OK. The LASER LED lights up red if the laser power is too weak, the laser beam is blocked or if the laser module is defective or out of alignment. (See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator.) This control lamp also lights up red during the spectrometer initialization phase. After the initialization is completed successfully, this LED turns to green. STATUS A green STATUS LED indicates that the spectrometer is in proper operating condition. The STATUS LED lights up red in case of a spectrometer malfunction or during the initialization phase. After the initialization is completed successfully, this LED turns to green. (See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator.)

Sample Compartment Normally, you gain access to the sample compartment from the spectrometer top side by removing the blue cover using the handle. See figure 11a. In exceptional cases, if your measurement accessory requires access from the spectrometer front side (e.g. for exchanging the sample), you can remove the blue front cover by loosening the six Allen screws using a hex key size 3mm. See figure 11b. Note: When performing measurements under vacuum condition do not forget to reinstall the sample compartment front cover. The sample compartment dimensions are 25.5cm (w) x 27cm (d) x 16cm (h). For more information about the sample compartment interior refer to chapter Operation, section QuickLock.

Sample Compartment Cover Handle

Figure 11: a) Sample Compartment Top Cover

VERTEX 70v User Manual

Allen Screws

b) Sample Compartment Front Cover

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OVERVIEW External Components

IR Beam Ports VERTEX 70v has seven IR beam ports (five outlet ports and two inlet ports) allowing the adaptation of external accessories and/or components (e.g. microscope, TG-IR coupling or external light source). The IR beam ports are at the front and rear side as well as at the left and right hand side of the spectrometer. For the exact dimensions of the IR beam port positions refer to appendix D. A

Figure 12: a) Front Side

D

C

B

E

b) Rear Side

F

G

Figure 12: c) Right Side

d) Left Side

IR Beam Ports

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A

Outlet port for focussed beam (e.g. for connecting a bolometer)

B

Outlet port for parallel beam (e.g. for connecting a fiber optic coupling module)

C

Inlet port for connecting a light emission source (e.g. Hg source)

D

Outlet port for parallel beam

E

Outlet port for parallel beam (e.g. for connecting a microscope, PMA50, external sample compartment XSA)

F

Inlet port for connecting a light emission source (e.g. FT-Raman module, water-cooled, high-power MIR source)

G

Outlet port for parallel beam (e.g. for connecting a microscope) or focussed beam (e.g. for connecting a bolometer) VERTEX 70v User Manual

The IR beam ports are vacuum-tight sealed by circular covers. To remove a cover loosen the six Allen screws using a hex key size 3mm. See figure 13. Note: External accessories are installed by the Bruker service technicians.

Allen Screws

Figure 13: Removing an IR Beam Port Cover

Spectrometer Rear Side External Beam Port

Attachment Flange for Vacuum Pump

Vent Opening/ Purge Gas Inlet

Electronics Panel

Primary Power Receptacle

CAN BUS Port

Mains Switch

Figure 14: Spectrometer Rear View

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OVERVIEW External Components

EXTERNAL BEAM PORT The inlet port is used for connecting a light source (e.g. Hg-Source) or an emission sample. VENT OPENING / PURGE GAS INLET Depending on whether you evacuate or purge the spectrometer, these two ports serve different purposes. In case of evacuating the spectrometer these ports serve as vent openings, whereas, when purging the spectrometer the purge gas supply lines are connected to these ports. (For detailed information about installing the purge gas connection refer to chapter Installation.) ELECTRONICS PANEL On the electronics panel are a number of ports (e.g. Ethernet port), the reset button as well as LEDs indicating, for example, the status of the interferometer. For a detailed description of the electronics panel refer to appendix F. MAINS SWITCH AND PRIMARY POWER RECEPTACLE The mains switch is used to turn the spectrometer on and off. The power supply socket is used to connect the power cord to the spectrometer. CAN BUS PORT The CAN bus port is primarily used to connect external automated units to the spectrometer. For more information refer to appendix F. ATTACHMENT FLANGE FOR VACUUM PUMP The vacuum pump can be connected to this attachment flange (NW25) using the supplied sealing ring, flexible metal hose and hose clamp. (For detailed information about how to connect the vacuum pump to the spectrometer refer to chapter Installation.)

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INTERNAL COMPONENTS

.......................................................... The following figure identifies only the most important internal components and their location inside the spectrometer.

D

E

F

A

G H B

C I

Figure 15: Internal Spectrometer Components

Component A

RockSolid interferometer (permanently aligned)

B

DigiTect Detectors

C

Sample holder for transmission measurements (exchangeable for other optional accessories with QuickLock baseplate)

D

HeNe laser

E

Two beamsplitters storage positions (optional)

F

Beamsplitter (operation position)

G

Optional NIR source (operating position)

H

MIR source (operating position)

I

QuickLock mechanism for accessories (including connectors) VERTEX 70v User Manual

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OVERVIEW Internal Components

4 Light Source

The basic instrument is equipped with a MIR source (H in figure 15). The MIR light source is a globar (i.e. an U-shaped silicon carbide piece) that emits mid-infrared light. Apart from the standard air-cooled MIR source, the following optional sources are available:

• VIS/NIR source (tungsten halogen lamp), installed in the spectrometer (G in figure 15), air-cooled

• FIR source (mercury lamp), connected externally to the spectrometer, watercooled

• UV/VIS/NIR source (tungsten lamp), connected externally to the spectrometer, water-cooled

• UV source (deuterium lamp), connected externally to the spectrometer, air-cooled • High power MIR source (globar), connected externally to the spectrometer, watercooled All external sources can be connected to one of the two inlet ports (C in figure 12b or F in figure 12c). For the FIR source (mercury lamp), the preferred connection port is the inlet port at the spectrometer rear side, C in figure 12b.

Detector The basic spectrometer configuration is equipped with a DigiTect DLaTGS detector with integrated preamplifier. This detector package contains an analog-to-digital-converter that converts the analog signal from the detector directly into a digital signal. This digital signal is transmitted to the data processing electronics unit of the spectrometer. The standard detector is a pyroelectric DLaTGS detector which covers a spectral range from 12,000 to 250cm-1, operates at room temperature and has a sensitivity of D*>4x108 cm Hz1/2 W-1. Apart from the standard detector, there is a large number of optional detectors. All detectors are mounted on dovetail slides which allow an easy exchange. The following optional detectors are available: Detector

Spectral Range (cm-1)

Sensitivity

Operating Temperature

Mid-Infrared DLaTGS with KBr window

12,000 - 250

D*>4x108cm Hz1/2W-1

Temperature-stabilized

DLaTGS with CsI window

12,000 - 160

D*>4x108cm Hz1/2W-1

Room temperature

MCT narrow band, with BaF2 window

12,000 - 850

D*:>4x1010cm Hz1/2 W-1

Liquid N2 cooled

CAUTION - HARMFUL!

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Detector MCT mid band, with ZnSe window

Spectral Range (cm-1)

Sensitivity

Operating Temperature

12,000 - 600

D*:>2x1010cm Hz1/2 W-1

Liquid N2 cooled

12,000 - 420

D*:>5x109cm Hz1/2W-1

Liquid N2 cooled

12,000 - 850

D*:>2x1010cm Hz1/2 W-1

Liquid N2 cooled

10,000 - 600

D*:>2x1010 cm Hz1/2W-1 (MCT) D*:>1.5x1011cm Hz1/2W-1(InSb)

Liquid N2 cooled

InSb

10,000 - 1,850

D*:>1.5x1011cm Hz1/2 W-1

Liquid N2 cooled

InSb with cold filter

10,000 - 3,100

D*>5x1011cm Hz1/2 W-1

Liquid N2 cooled

Ge Detector (Raman)

11,750 - 5,900

NEP