Manual ALPHA 10055416th - Filosofia (2024)

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ALPHAUser Manual10055416th version 2017, publication date February 2017© 2017 BRUKER OPTIK GmbH, Rudolf-Plank-Straße 27D-76275 Ettlingen, www.bruker.comAll 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. with-out 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.This manual is the original documentation for the ALPHA spectrometer. The ALPHA spectrometer is covered by one or more of the following patents: DE 102004025448; DE 19940981; US 5923422; DE 19704598. Other US and international patents are pending.BrukerTable of Contents1 Introduction....................................................................................................91.1 About this manual .................................................................................................. 91.2 Terms....................................................................................................................... 91.3 Gender-neutral form............................................................................................... 91.4 Safety..................................................................................................................... 101.4.1 Warning labels........................................................................................................ 111.4.2 Waste disposal ....................................................................................................... 121.5 General information ............................................................................................. 131.5.1 Protective earthing ................................................................................................. 131.5.2 Qualified personnel ................................................................................................ 131.5.3 Intended use........................................................................................................... 131.6 Questions and concerns ..................................................................................... 142 ALPHA spectrometer ..................................................................................152.1 Basic module ........................................................................................................ 162.1.1 Connection ports and LEDs ................................................................................... 172.1.2 Stand-by mode ....................................................................................................... 192.2 Exchanging sampling module ............................................................................ 212.2.1 Procedure............................................................................................................... 212.2.2 After exchanging the sampling module .................................................................. 222.3 Spectrometer configuration ................................................................................ 232.3.1 ALPHA for transmission measurements ................................................................ 232.3.2 ALPHA for ATR measurements ............................................................................. 242.3.3 ALPHA for reflection measurements ...................................................................... 252.3.4 ALPHA for gas analysis.......................................................................................... 262.4 Design ................................................................................................................... 272.5 Applications.......................................................................................................... 272.6 Spectrometer housing ......................................................................................... 272.7 Optics .................................................................................................................... 272.8 Electronics ............................................................................................................ 282.9 Spectroscopy software........................................................................................ 283 ALPHA for transmission measurement.....................................................293.1 Overview on ALPHA spectrometer configurations for transmission.............. 293.2 ALPHA-T universal sampling module ................................................................ 303.2.1 Specifications ......................................................................................................... 303.2.2 Optical path ............................................................................................................ 313 Optik GmbH ALPHA User ManualTable of Contents3.2.3 Opening sample compartment ............................................................................... 323.2.4 Starting measurement ............................................................................................ 333.2.5 Potential operating errors ....................................................................................... 343.3 Measuring accessories ........................................................................................ 343.3.1 Sample holder (standard) ....................................................................................... 353.3.2 Foil holder (option).................................................................................................. 363.3.3 Liquid cell (option) .................................................................................................. 363.3.4 Gas cell (option) ..................................................................................................... 373.4 ALPHA-T 30° reflection accessory ..................................................................... 403.4.1 Specifications ......................................................................................................... 403.4.2 Displacing mounted sample holder ........................................................................ 413.4.3 Inserting 30° reflection accessory into the sample compartment ........................... 423.4.4 Performing measurement ....................................................................................... 434 ALPHA for ATR measurement....................................................................454.1 Overview on ALPHA spectrometer configurations for ATR............................. 454.2 ALPHA-E sampling module ................................................................................. 474.2.1 Optical path ............................................................................................................ 484.3 ALPHA-P sampling module ................................................................................. 494.3.1 Optical path ............................................................................................................ 504.3.2 High-pressure variant ............................................................................................. 504.3.3 With heatable ATR unit........................................................................................... 524.4 Crystal material..................................................................................................... 564.5 Replacing ATR crystal plate ................................................................................ 574.5.1 Procedure ............................................................................................................... 574.6 Working withsafety goggles.➣ Do not heat up a liquid above its boiling temperature.When using flow-through cells:During measurement, the flow-through cell and the sample can be heated up to 120°C.➣ Avoid any skin contact with hot objects and surfaces. Improper handling can cause burns!When heating flammable liquids:Heating up flammable liquids involves the risk of deflagration, explo-sion and fire.➣ Heat only liquids with a burning point above 200°C.➣ Consider that flammability is increased with heated liquids.➣ Keep heated liquids away from naked flames.When heating corrosive liquids or liquids that are hazardousto health:Heating corrosive liquids or liquids that are hazardous to health can produce toxic or corrosive gases and vapors.➣ Extract toxic or corrosive gases and vapors.Table 4.15: Safety instructions when heating sample material1 Fill the syringe with sample liquid.2 Insert the syringe into the injection port at the flow-through cap or filling hose.3 • Direct the drain hose into a bucket for collecting the sample liquid.• Inject the sample liquid.4 Set the temperature (chapter 4.9.2.1).Table 4.16: Positioning sample on ALPHA-P equipped with flow-through cell63 Optik GmbH ALPHA User ManualALPHA for ATR measurement 4In case of pressure applicator5 Measure sample (chapter 4.9.2).6 Clean flow-through cell (chapter 4.11).Table 4.16: Positioning sample on ALPHA-P equipped with flow-through cell1 Position sample in the middle of the sample plate.➣ The ATR crystal must completely be covered by the sample material. A small amount of sample material is sufficient.Improper use of heated corrosive substances and/or substances that are hazardous to health:Personal injury➣ Always wear safety googles.➣ Extract corrosive or hazardous gases or vapors.➣ Observe the safety instructions.2 Press anvil against the sample.➣ Make sure that the optimum contact pressure is used to press the sample against the ATR crystal.3 Measure sample (chapter 4.9).4 • Move pressure arm upwards.• Remove sample. i Sample material should not be left in contact with the crystal for an extended period of time, as chemically reactive sample material may degrade the crystal quality and discolor the metal plate. Therefore, once the measure-ment has finished, remove the sample from the crystal.5 Thoroughly clean the sample plate, ATR crystal and anvil, see chapter 4.10.Table 4.17: Positioning sample on ALPHA-P equipped with pressure applicatorCAUTION64 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.9 Performing measurementMeasurement is performed by the OPUS spectroscopy software. Before starting a sam-ple measurement you first have to perform a background measurement. Observe the steps described in the following chapters.4.9.1 Performing non-temperature controlled measurement4.9.1.1 Loading measurement experiment☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module and ATR crystal type used. Thus, the experiment file1 is automatically loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. Start the OPUS spectroscopy software and wait until the performance test has fin-ished.➣ The OPUS status light must be green after the performance test has finished.2. On the Measure menu, select the Setup Measurement Experiment command.3. On the dialog that opens, click the Basic tab.4. Click the Load button. Based on the ATR crystal material used, select the respective experiment file from the dialog that opens.5. Click the Accept & Exit button.4.9.1.2 Starting background measurement1. Flap the pressure arm upwards.2. On the OPUS Measure menu, select the Measurement command.3. On the dialog that opens, click the Start Background Measurement button.4. Wait until the background measurement has finished.1. Depending on the ATR crystal type used, the ATR sampling module is supplied with the following experi-ment file: ATR_Di.XPM, ATR_Ge.XPM, ATR_ZnSe.XPM. This experiment file contains the default parame-ters set by Bruker, to be used to perform ATR measurement.65 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.9.1.3 Starting sample measurement1. Flap the pressure arm upwards.2. Position sample onto the ATR crystal.3. Flap the pressure arm downwards.➣ The optimal contact pressure is given if the red spot is exactly in the middle of the round recess on the front of the pressure arm (chapter 4.6.2). The spectrom-eter status indicator and the OPUS status light must be green.4. On the Measure menu, select the Measurement command.5. On the dialog that opens, click the Start Sample Measurement button.6. Wait until the sample measurement has finished.4.9.2 Performing temperature-controlled measurement (only with heatable ALPHA-P)4.9.2.1 Setting temperaturei The temperature accuracy of the ATR crystal is ± 1°C. In case of a strongly heat-dissi-pating sample, wait a few minutes before starting the measurement to be able to ensure the stated temperature accuracy.Minimum temperature: 5°C above the current temperatureaa. The minimum temperature value specified must be at least 5°C above the current temperature. Otherwise, the sampling module does not start heating, and the Instrument ready status cannot be achieved, i.e. measurement cannot be performed. The status of the temperature control (chapter 4.3.3.1) is displayed by the temperature LED located on the sampling module. Maximum temperature: 120°Cbb. The sampling module is not equipped with a cooling device. The heatable sampling module al-lows temperature-controlled measurements up to a maximum temperature of 120°C. When en-tering a higher temperature value a warning message is displayed. Confirm the message and enter a temperature value ofopens, click the Start Background Measurement button.➣ The spectrometer starts heating. This is indicated by a quickly flashing LED (green). As soon as the desired temperature is reached (the LED is permanently green), OPUS automatically starts background measurement.4. Wait until the background measurement has finished.4.9.2.4 Measuring liquid sample1. Flap the pressure arm (if available) upwards and put the liquid sample onto the ATR crystal. If a flow-through cap is used, inject the liquid sample by a syringe.➣ Do not remove the syringe from the injection port during measurement, to avoid any dry run of the flow-through cap.2. Wait until the sample is heated.3. On the Measure menu, select the Measurement command.4. On the dialog that opens, click the Start Sample Measurement button.5. Wait until the sample measurement has finished.68 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.10 Cleaning ATR sampling moduleAfter each sample measurement performed, you thoroughly have to clean the sample plate, ATR crystal and anvil. Remaining sample material on any of these elements may cause falsified measurement results.4.10.1 Cleaning solventsNever use caustic, abrasive substances nor strong acids. These substances can dam-age the sample plate and the ATR unit.Possible cleaning solvents:• alcohol• acetone• ethanol• isopropanoli When using solvents read the materials safety data sheets supplied with the solvents and observe any recommended handling procedure.The solvent used for cleaning depends on the sample type that has been analyzed. In any case, it is best to try to clean the sample plate by the mildest solvent possible.4.10.2 ProcedureIf you use a heatable ALPHA-P sampling module, wait until the sample plate has cooled down sufficiently.1 Flap the pressure arm upwards and move it out of the measuring position.2 Clean the ATR crystal by a lint-free cloth or Q-tip. Apply only low pressure.i Never use filled paper tissue to rub on the surface. Due to the abrasive effect of the paper tissue you may scratch the crystal surface, especially in case of crystals made of germanium (Ge) and zinc selenide (ZnSe).3 Clean the anvil.4 Perform a cleanness test (chapter 4.7) to check whether the ATR crystal is free of sample residues.☞ If the cleanness test fails, repeat the cleaning procedure.Table 4.19: Cleaning ATR sampling module69 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.11 Cleaning flow-through cell1 Purge the flow-through cell thoroughly with an appropriate cleaning solvent and/or water.i It is recommended to purge the flow-though cell by using air.2 De-install the flow-through cell (chapter 4.3.3.4).3 Carefully clean the sampling surface and the ATR crystal surface.4 Perform a cleanness test (chapter 4.7) to check whether the ATR crystal is free of sample residues.☞ If the cleanness test fails, repeat the cleaning procedure.Table 4.20: Cleaning ATR sampling module70 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.12 ALPHA ATR multi reflection sampling module (A213/D-11)Measurement type: attenuated total reflectionUsable sample materiala:a. Especially suited for low-concentrated sample components. For more details refer to chapter 4.12.2.• pastes• liquidsAvailable crystal types: zinc selenide (ZnSe)bb. The ATR crystal is horizontally embedded into the working plate.Actual sampling surface on ATR crystal:5 x 48 mm ØMeasuring sensitivity: high light throughput due to 6 reflections on the sample surfaceSpectral range: 600 to 7,500 cm2pH value of sample: 4 to 8Definition1 Top cover made of stainless steel for volatile samples2 Crystal plateTable 4.21: ALPHA ATR multi reflection sampling module - ComponentsFigure 4.8: ALPHA ATR multi reflection sampling module2171 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.12.1 Optical path4.12.2 Usable sample materialTable shows the compatibility of certain chemical substances (sample material) in con-nection with the crystal material ZnSe and its fixing.Figure 4.9: ALPHA ATR multi reflection sampling module - Optical pathSample material Compatible with ZnSe1,1,1-trichloroethane Yes, short exposure only2-propanol Yes, permanentAcetone Yes, short exposure onlyBenzene Yes, permanentConcentrated acids and bases NoCutting oil Yes, permanentDiluted acids and bases (pH 4 to 8) Yes, short exposure onlyEthanol Yes, permanentMethyl ethyl ketone NoMethylene chloride NoUnleaded gasoline Yes, permanentWater Yes, permanentTable 4.22: Sample material and its compatibility with ZnSe72 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.12.3 Performing measurement4.12.3.1 Loading measurement experiment1. Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module and ATR crystal type used. Thus, the experiment file (ATR_ZnSe)1 is automatically loaded in OPUS. If the experiment file is not loaded automatically, perform the following steps.2. Start OPUS. On the Measure menu, select the Setup Measurement Experiment command.➣ The Setup Measurement Experiment dialog opens.3. Click the Basic tab.4. Click the Load button. Select the ATR_ZnSe experiment file from the dialog that opens.5. Click the Accept & Exit button.4.12.3.2 Starting background measurement1. The spectrometer status indicator and the OPUS status light must be green.2. Make sure that not any sample is available on the ATR crystal.3. On the OPUS Measure menu, select the Routine Measurement command.4. On the dialog that opens, click the Start Background Measurement button.5. Wait until the background measurement has finished.1. This experiment file contains the default parameters set by Bruker, to be used to perform ATR measure-ment.73 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.12.3.3 Starting sample measurement1. Use a pipette to drop the sample onto the ATR crystal.➣ The ATR crystal must completely be covered by the sample material. A small amount of sample material is sufficient.2. On the Measure menu, select the Routine Measurement command.3. On the dialog that opens, click the Start Sample Measurement button.4. Wait until the sample measurement has finished.4.12.4 Potential operating errorsFigure 4.10: Dropping sample onto ATR crystalCAUTIONImproper use of flammable and/or explosive substances:Personal injury➣ Always wear safety googles.➣ Only use small amounts of sample material.➣ Do not inhale the vapor of volatile substances.➣ Observe the safety instructions.Problem TroubleshootingPerformance or instrument test failed• Check whether there is any sample material or contamination on the ATR crystal.• Remove the sample, and clean the ATR crystal.• Restart the performance or instrument test.Crystal plate missing or not positioned properlyLift up the crystal plate again and carefully press it down until is snaps into position.Table 4.23: Potential operating errors74 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.12.5 Measuring accessoryTo be able to analyze volatile samples a top cover made of stainless steel is part of the delivery content, by default.4.12.6 Cleaning crystal plateAfter each sample measurement performed, you thoroughly have to clean the crystal plate (and the top cover for volatile samples if it had been used). Remaining sample material on any of these elements may cause falsified measurement results.4.12.6.1 Cleaning solventsNever use caustic, abrasive substances nor strong acids. These substances can cause sustainable damage to the crystal plate.Possible cleaning solvents:• alcohol• ethanol• isopropanoli When using solvents read the materials safety datasheets supplied with the solvents and observe any recommended handling procedure.The solvent used for cleaning depends on the sample type that has been analyzed. In any case, it is best to try to clean the sample plate by the mildest solvent possible.4.12.6.2 Procedure1. Lift up the sample compartment lid.2. Use a lint-free and soft cloth to clean the crystal. Apply only low pressure.➣ Never use filled paper tissue to rub on the surface. Due to the abrasive effect of the paper tissue you may scratch the crystal surface.Figure 4.11: Top cover for volatile samples75 Optik GmbH ALPHA User ManualALPHA for ATR measurement 43. Dry the crystal plate.4. Perform a cleanness test (chapter 4.7) to check whether the ATR crystal is free of sample residues.5. If the cleanness test fails, repeat the cleaning procedure.4.12.7 Replacing crystal plateThe crystal plate is flush mounted in a flat trough made of metal. Replace the crystal plate only if it is damaged.1 Lift up the sample compartment lid.2 Reach into the slot on the crystal plate (see arrow on the left figure), and carefully move up the crystal plate.3 Carefully insert the new crystal plate onto the trough, press it down until it snaps into position.Table 4.24: ALPHA ATR multi reflection sampling module - Replacing crystal plate76 ALPHA User Manual Bruker Optik GmbHBruker5 ALPHA for reflection measurement5.1 Overview on ALPHA spectrometer configurations for reflectionMeasurement type: • specular reflectiona• diffuse reflectionb a. When IR light falls on a surface, two types of reflection occur: specular reflection (i.e. the light reflects directly off the surface) and diffuse reflection (the IR light penetrates the sample surface is reflected in all directions). The amount of reflection type occurring on the sample depends on the roughness of the sample surface.b. The optics of a diffuse reflection accessory is designed in such a way that the detection of diffusely reflected light is optimized and the detection of specularly reflected light is minimized. DRIFTS (diffuse reflectance infrared fourier transform spectroscopy) is an analyzing technique in FT-IR spectroscopy that makes use of the phenomenon of the diffuse reflection.Usable sample material: sample surfacesALPHA spectrometer configurations for reflectionALPHA-R(A528/D drift module, diffuse reflection)ALPHA-R(A241/D module, contact-less reflection)ALPHA-R(A241/DL module, contact-less reflection)Table 5.1: Overview on ALPHA spectrometer configurations for reflection77 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.2 ALPHA-R sampling module (A528/D)ALPHA-R(A241/DV, contactless, video-based reflection)ALPHA-R(A240/DU, upward looking reflection)ALPHA spectrometer configurations for reflectionTable 5.1: Overview on ALPHA spectrometer configurations for reflectionMeasurement type: diffuse reflectionUsable sample material: • solids in a powdery or crystalline state• cloths, fibers and coatings that can be abraded• powders, paper, polymers, solid samples having a rough surface• gemstonesAdvantages of this kind of measuring technique:• no sample preparation required in case of powders and crystals• suited for strongly scattering and absorbing samples• high signal intensitya a. This measurement technique delivers comprehensive and extensive spectral informa-tion. As the scattered and diffusely reflected light of a large number of particles is de-tected, sample components with a weak signal intensity can be detected as well.Toolkit: included in delivery content, chapter 5.2.478 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.2.1 SpecificationsDefinition1 Reflection unit2 Slider for sample material and reference mirror3 Height adjustment screwTable 5.2: ALPHA-R (A528/D) sampling module - ComponentsFigure 5.1: ALPHA-R sampling module (A528/D)321Spectral range: 375 - 7,500 cm-1 Mirror material: GoldSampling spot: Ø 2 mm79 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.2.2 Optical path5.2.3 Software requirements in case of OPUS versionALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 53 If the instrument/performance test failed:• On the OPUS Measure menu, select the Setup Measurement Parameters command.• Click the Check Signal tab.• Check signal intensity (A).☞ Rotate the height adjustment screw (figure 5.1) until there is sufficient signal on the Check Signal tab.☞ Close the dialog.Table 5.5: Checking signal intensity, starting instrument/performance testA85 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.2.6.2 Loading measurement experiment☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (DRIFT.XPM) assigned to the sampling module is automatically loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. On the Measure menu, select the Setup Measurement Experiment command.2. On the dialog that opens, click the Basic tab.3. Click the Load button and select the DRIFT.XPM experiment file from the dialog that opens.4. Click the Accept & Exit button.5.2.6.3 Starting background measurement☞ The signal intensity is checked (chapter 5.2.6.1). The spectrometer status indicator and the OPUS status light must be green.1. On the OPUS Measure menu, select the Measurement command.2. On the dialog that opens, click the Start Background Measurement button.3. Wait until the background measurement has finished.5.2.6.4 Starting sample measurement1. Remove the reference mirror from the slider.2. Put the filled sample cup onto the slider, and move the slider to the measuring posi-tion, up to the mechanical stop.3. On the OPUS Measure menu, select the Setup Measurement Parameters com-mand.4. Click the Check Signal tab.5. Position the height adjustment screw (figure 5.1) such that the signal intensity, which can be achieved as maximum, is displayed. The maximum signal intensity depends very much on the sample properties (grain size, color).6. Close the dialog.7. On the OPUS Measure menu, select the Measurement command.➣ The Measure dialog opens.8. Click the Start sample Measurement button.9. Wait until the sample measurement has finished.1. The ALPHA-R sampling module is supplied with the DRIFT.XPM experiment file. This experiment file con-tains the default parameters set by Bruker, to be used to perform diffuse reflection measurement.86 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.2.7 Cleaning sampling moduleWhen cleaning the sampling module do not touch the mirrors. If dust or sample residues are on the sample, carefully wipe off the residues. Only use the brush supplied in the tool kit. Do by no means use any solvents or cleaning agents.5.2.8 Potential operating errorsNOTEMirror surface not properly cleanedProperty damage, gold coating destroyed➣ Remove dust or sample residues by means of the brush supplied.➣ Do not use any solvents or cleaning agents.Problem TroubleshootingNo or insufficient signal inten-sity, high spectral noiseCheck signal intensity (chapter 5.2.6.1).Reference mirror or the sam-ple are not correctly placed onto the measuring positionMove the slider into the sampling module, up to the mechanical stop.Sample cup not properly filled with powderFill in the sample cup properly (chapter 5.2.5).Table 5.6: Potential operating errors87 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.3 ALPHA-R (A241/D, A241/DV) sampling moduleThe ALPHA-R (A241/D, A241/DV) sampling module can be mounted on a tripod. Differ-ent types of tripods are available with Bruker.Measurement type: • contactless, non-destructive reflection (A241/D)• contactless, non-destructive reflection, visualization of exact measuring position (A241/D)Usable sample material: • large sample surfaces• mural paintings• coatings on metalsAdvantages of this kind of measuring technique:• non-destructive sampling• no sample preparation requiredApplication field: art conservation and restorationDefinition1 Reflection unit2 Port for video camera cableTable 5.7: ALPHA-R (A241/D, A241/DV) sampling module - ComponentsFigure 5.4: ALPHA-R sampling module (A241/D, A241/DV)A241/D A241/DV2188 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.3.1 SpecificationsFigure 5.5: ALPHA-R (A241/DV) sampling module mounted on a tripodSpectral range: 375 - 7,500 cm-1Mirror material: goldSampling spot: Ø 5 mm (optionally: 3 mm)Sampling spot distance from spectrometer front:15 mm89 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.3.2 Optical pathFigure 5.6: ALPHA-R (A241/D) - Optical path90 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 5Figure 5.7: ALPHA-R (A241/DV) - Optical path91 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.3.3 Software requirements in case of OPUS versiona logo test, click the Next button.☞ If the driver installation is completed, click the Finish button.Table 5.10: Installing driver for camera control software1 On the Windows Explorer, double click the Setup.exe file from the main path of the CD. ➣ The installation starts.2 Select Software Installation.3 Select Software for end users.Table 5.11: Installing camera control software96 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.3.4.5 Starting and configuring camera control software4 Select Capture.5 Continue installation. ☞ Click the Next button.☞ If the software installation is completed, click the Finish button.Table 5.11: Installing camera control software1 Double click the IC-Capture software shortcut, located on the desktop.2 Select the camera type connected and click OK to confirm.Table 5.12: Starting and configuring camera control software97 Optik GmbH ALPHA User ManualALPHA for reflection measurement 53 When the software starts, the video camera shows the live image of the sam-ple. If the live image is distorted, the settings made in the PAL/NTSC_M menu must be changed.☞ Check the correct orientation of the live image by means of a printed object.☞ If the view is rotated, select the Rotation command on the Device menu.4To change between live image and snapshots taken, use the icon or in the toolbar.i Further details on the camera control software are described in the Helpmenu.Table 5.12: Starting and configuring camera control software98 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.3.5 Performing measurementWhen performing a measurement observe the order of the chapters described in the fol-lowing.5.3.5.1 Mounting reference cap, starting instrument/performance testIf AAR accessory recognition is activated (which is the case by default), the instrument/performance test starts automatically. In case of the ALPHA-R (A241/D, A241/DV) sam-pling module, however, you first have to mount the supplied reference cap onto the front side of the sampling module. Otherwise, the tests will fail.Reference cap with built-in gold coated mirror:Spacer:Sample cap with sample spot diameter of 3 mm:Sample cap with sample spot diameter of 5 mm:Table 5.13: Measuring tools supplied99 Optik GmbH ALPHA User ManualALPHA for reflection measurement 5Procedure5.3.5.2 Loading measurement experiment☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (DRIFT.XPM) is automatically loaded in OPUS. If the experi-ment file is not loaded automatically, perform the steps 1 et seq.1. On the OPUS Measure menu, select the Setup Measurement Experiment com-mand.2. On the dialog that opens, click the Basic tab.3. Click the Load button and select the DRIFT.XPM experiment file from the dialog that opens.4. Click the Accept & Exit button.1 Mount the reference cap onto the front side of the sampling module.➣ The reference cap is kept in posi-tion by magnets.2 • Start the OPUS spectroscopy software.➣ The instrument/performance test starts.• Wait until the test has finished.➣ The spectrometer status indicator and the OPUS status light must be green.Table 5.14: Mounting reference cap1. The ALPHA-R sampling module is supplied with the DRIFT.XMP experiment file. This experiment file con-tains the default parameters set by Bruker, to be used to perform reflection measurement.100 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.3.5.3 Starting background measurement1. Keep the reference cap mounted. Make sure that the spectrometer status indicator and OPUS status light are green.2. On the OPUS Measure menu, select the Measurement command.3. On the dialog that opens, click the Start Background Measurement button.4. Wait until the background measurement has finished.5.3.5.4 Starting sample measurement1. Remove the reference cap and fix the spacer or sample cap with the particular sam-ple spot diameter onto the front side of the sampling module.➣ The spacer or holder is kept in position by magnets.2. Position the sample directly in front of the spacer or sample cap.➣ If the sample must not be touched, you can measure the sample without using the spacer. Position the sample in front of the sampling module. Keep a distance of about 15 mm from the reflection unit. 3. Illuminate the sample (optionally): turn the switch, located on top of the spectrome-ter housing, to the left.4. On the OPUS Measure menu select the Measurement command.5. On the dialog that opens, click the Start sample Measurement button.6. Wait until the sample measurement has finished.Figure 5.9: Spacer fixed on the front side of the sampling moduleFigure 5.10: Switch to illuminate sample101 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.3.6 Potential operating errorsProblem TroubleshootingInstrument/performance test failedCheck whether reference cap is mounted (chapter 5.3.5.1).No sample spectrum or bad spectrum quality• Keep a distance of at least 15 mm from the reflection unit to position the sample properly positioned when measuring without spacer.• If required, optimize signal:☞ On the OPUS Measure menu, select the Advanced Measurement command.☞ Click the Check Signal tab.• A different type of measuring technique may be required (e.g. ATR) if the sample consistency does not allow reflection measurement (e.g. in case of very dark, coarse or porous sample material). Table 5.15: Potential operating errors102 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.4 ALPHA-R (A241/DL) sampling moduleThe ALPHA-R (A241/DL) sampling module can be mounted on a tripod. Different types of tripods are available with Bruker.Measurement type: contactless, non-destructive reflec-tionUsable sample material: • large sample surfaces• shaped samplesAdvantages of this kind of measuring technique:• non-destructive sampling• no sample preparation requiredApplication field: surface analysis of shaped sam-ples, e.g. to control coatings or detect contaminationsDefinition1 Measuring adapterTable 5.16: ALPHA-R (A241/DL) sampling module - ComponentsFigure 5.11: ALPHA-R sampling module (A241/DL)1103 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.4.1 SpecificationsSpectral range: 375 - 7,500 cm-1Mirror material: goldSampling spot: Ø 7 mmSampling spot distance from spectrometer front:42 mmAngle of incidence: 11°104 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.4.2 Optical pathFigure 5.12: ALPHA-R (A241/DL) - Optical path105 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.4.3 Software requirements in case of OPUS versionthe case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (DRIFT.XPM) is automatically loaded in OPUS. If the experi-ment file is not loaded automatically, perform the steps 1 et seq.1. On the OPUS Measure menu, select the Setup Measurement Experiment com-mand.2. On the dialog that opens, click the Basic tab.3. Click the Load button and select the DRIFT.XPM experiment file from the dialog that opens.4. Click the Accept & Exit button.1. The ALPHA-R sampling module is supplied with the DRIFT.XMP experiment file. This experiment file con-tains the default parameters set by Bruker, to be used to perform reflection measurement.106 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.4.4.2 Starting background measurement1. Make sure that the spectrometer status indicator and OPUS status light are green.2. On the OPUS Measure menu, select the Measurement command.3. Put the reference mirror onto the measuring adapter.➣ The reference mirror is fixed by a magnet onto the measuring adapter.4. On the dialog that opens, click the Start Background Measurement button.5. Wait until the background measurement has finished.5.4.4.3 Starting sample measurement1. Remove the reference mirror from the measuring adapter.2. Position the sample directly in front of the measuring adapter.3. On the OPUS Measure menu select the Measurement command.4. On the dialog that opens, click the Start sample Measurement button.5. Wait until the sample measurement has finished.Figure 5.13: ALPHA-R (A241/DL) - Measuring adapter with reference mirror107 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.4.5 Potential operating errorsProblem TroubleshootingInstrument/performance test failedCheck whether the reference mirror is put onto the measuring adapter at all, or correctly (chapter 5.4.4.2).No sample spectrum or bad spectrum quality• Position the sample directly in front of the measuring adapter.• If required, optimize signal:☞ On the OPUS Measure menu, select the Advanced Measurement command.☞ Click the Check Signal tab.• A different type of measuring technique may be required (e.g. ATR) if the sample consistency does not allow reflection measurement (e.g. in case of very dark, coarse or porous sample material). Table 5.17: Potential operating errors108 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.5 ALPHA-R (A240/DU) sampling moduleMeasurement type: • specular reflection from bottom up• diffuse reflection from bottom upUsable sample material: • reflective materials• textilesApplication field: art conservation and restorationTwo sample holders included in delivery content:for solid samples with a diameter of 3 mm or 5 mmDefinition1 Reflection unit, closed with sample holder2 Sample holder3 Reflection unit, open with fixed sampling plate4 Gold mirror for reference measurementsTable 5.18: ALPHA-R (A240/DU) sampling module - ComponentsFigure 5.14: ALPHA-R sampling module (A240/DU)4321109 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.5.1 SpecificationsSpectral range: 375 - 7,500 cm-1 (with KBr win-dows)Sampling spot (depending on sample holder):• 5 mm• 3 mmSampling holder: • holder for flat samples• sample cup for granules (>3 mm, >5 mm)110 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for reflection measurement 55.5.2 Optical pathFigure 5.15: ALPHA-R (A240/DU) - Optical path111 Optik GmbH ALPHA User ManualALPHA for reflection measurement 55.5.3 Software requirements in case of OPUS versionmaterial). Table 5.21: Potential operating errors116 ALPHA User Manual Bruker Optik GmbHBruker6 ALPHA for gas analysis6.1 Overview on ALPHA spectrometer configurations for gas analysisMeasurement type: gas analysisUsable sample material: gaseous samplesApplication field: industrial research or process appli-cationsALPHA spectrometer configurations for ATRALPHA-G(A139, with long-path gas cell)ALPHA-G with A139-H1 option (heating jacket)ALPHA with A128D/T option (heatable 7 cm gas cell)Table 6.1: Overview on ALPHA spectrometer configurations for gas analysis117 Optik GmbH ALPHA User ManualALPHA for gas analysis 66.2 ALPHA-G sampling module (A139/D)Measurement type: gas analysisUsable sample material: gasesAccessory set: heating jacket for gas cell with a path length of 4.8 mDefinition1 Long-path gas cell2 Basic moduleTable 6.2: ALPHA-G (A139/D) sampling module - ComponentsFigure 6.1: ALPHA-G (A139/D) sampling module21118 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66.2.1 SpecificationsPath length: 4.8 mVolume: 0.5 lGas cell hardware: aluminium electroless nickelTemperature range: from ambient to 200°CPressure range: from vacuum to 3.5 barPower consumption: 300 WMaximum gas flow rate: 50 l/minProtection class: I, complies with IEC 61140Mirror: gold platedWindow material, standard: KBRspectral range: 7.500 - 380 cm-1Window material, optional: • BaF2spectral range: 7.500 - 900 cm-1• ZnSespectral range: 7.500 - 500 cm-1119 Optik GmbH ALPHA User ManualALPHA for gas analysis 66.2.2 Optical pathFigure 6.2: ALPHA-G (A139/D) sampling module - Optical path120 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66.2.3 Software requirements in case of OPUS version195 cm (w x d x h)Weight: 2.4 kgDimensions: 100 x 160 x 70 cm (w x d x h)Weight: 0.9 kg126 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66.3.3 Software requirements in case of OPUS versionthan the software, the following requirements must be met:• OVP database version 6.5.6The OVP database must be updated (chapter 6.2.3.1).6.4.3.1 Updating OVP data base1. Insert the USB stick, which contains the OVP database, into the USB port of the PC.2. Open the Windows explorer and browse to the directory of the USB stick.3. Double click the OVP_Database_Install.exe file to start the installation program.➣ The installation program first checks for previously installed components. This automatic search process may take a few seconds.4. Follow the on-screen instructions.6.4.4 Gas line connection portsThe gas cell is equipped with a gas inlet and outlet. The gas inlet and outlet are 1/8" Swagelok1 connections.To connect the gas supply lines you first have to remove the protective caps.1. American manufacturer of fluid system components: www.swagelok.comFigure 6.8: Sampling module ALPHA (A128D/T) - Gas line connection ports135 Optik GmbH ALPHA User Manualwww.swagelok.comALPHA for gas analysis 66.4.4.1 Safety instructions when operating the gas cellBefore being able to operate the gas cell you have to observe the following safety instructions:1. Define the gas flow volume. The maximum gas flow rate should not exceed 5 l/min. Use a mass flow rate controller.2. Limit the maximum allowed pressure within the cell to 4 bar in case of gas cell win-dows made of ZnSe.➣ The gas cell is NOT delivered with a safety valve. It is the operator’s duty to take safety measures which prevent the pressure inside the cell from exceeding the maximum.3. Set and check the temperature by means of the temperature control unit.4. Make sure that the gas cell reaches the appropriate operating temperature. Only after the operating temperature has been reached (nominal/ actual value compari-son) is a measurement reasonable. 6.4.5 Performing measurementWhen performing measurement observe the order of the chapters described in the fol-lowing.6.4.5.1 Starting instrument/performance testIf AAR accessory recognition is activated (which is the case by default), the instrument/performance test starts automatically. In case of the ALPHA (A128D/T) sampling mod-ule, however, you first have to fill in nitrogen into the gas cell. Otherwise, the tests will fail.CAUTIONImproper sampling techniquesPersonal injury➣ Never use oxidizing, corrosive or toxic samples in connection with the gas cell.1 • Start the OPUS spectroscopy software.• Follow the on-screen instructions.• Wait until the instrument/performance test has finished.➣ The spectrometer status indicator and the OPUS status light must begreen.Table 6.10: Starting instrument/performance test136 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66.4.5.2 Deactivating pre-defined measurement parameters1. On the Measure menu, select the Optic Setup and Service command.2. On the dialog that opens, click the Devices/Options tab.3. Delete the checkmark in front of the Enforce Predefined Measurement Parametersoption.4. Click the Save Settings button.6.4.5.3 Loading measurement experiment and set temperature☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (TRANS.XPM) assigned to the sampling module is automati-cally loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. On the Measure menu, select the Setup Measurement Experiment command.2. On the dialog that opens, click the Basic tab.3. Click the Load button and select the TRANS.XPM experiment file from the dialog that opens.4. On the Optic tab, define the temperature.➣ To switch off heating completely, enter -300°C.5. Click the Accept & Exit button.6.4.5.4 Starting background measurement1. Fill in reference gas (nitrogen) into the gas cell.2. On the OPUS Measure menu, select the Measurement command.3. On the dialog that opens, click the Start Background Measurement button.4. Wait until the background measurement has finished.6.4.5.5 Starting sample measurement1. Fill in sample gas into the gas cell.2. On the OPUS Measure menu, select the Measurement command.3. On the dialog that opens, click the Start sample Measurement button.4. Wait until the sample measurement has finished.1. The ALPHA sampling module is supplied with the TRANS.XPM experiment file. This experiment file con-tains the default parameters set by Bruker, to be used to perform gas analysis.137 Optik GmbH ALPHA User ManualALPHA for gas analysis 66.4.6 Potential operating errors6.4.7 Replacing windows of sampling moduleThe gas inlet and outlet ports of the ALPHA (A128D/T) sampling module are closed by means of exchangeable IR transparent windows.6.4.7.1 Window materialProblem TroubleshootingInstrument/performance test failedFill in the gas cell with nitrogen.Varying width and form of bands in the sample spectrumFill in the gas cell with constant pressure. In case of flow-through measurements ensure a constant flow rate (use a rotameter).Window opaque, corroded Replace windows (chapter 6.4.7 et seq.).Table 6.11: Potential operating errorsMaterial Chemical propertiesBarium fluoride (BaF2) Low water solubility; soluble in strong acid and NH4ClHarmful!➣ Observe the safety data sheet.➣ Do not inhale or ingest the dust of broken win-dow material. Avoid any skin contact.Calcium fluoride (CaF2) Insoluble in water; resistant to most acids and bases; soluble in NH4 saltsPotassium bromide (KBr)Soluble in water, alcohol, and glycerineHygroscopic!➣ Avoid any contact to humidity.Table 6.12: Window material available for ALPHA (A128D/T)CAUTIONNOTE138 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66.4.7.2 Replacing intervalThe windows of the sampling module ALPHA (A128D/T) must only be replaced, if they are opaque, cracked or completely damaged. This applies to all window material used with the sampling module ALPHA (A128D/T). 6.4.7.3 Replacing procedureZinc selenide (ZnSe) Soluble in acids (pH 4- 8), while generating hydrogen selenideToxic!➣ Observe the safety data sheet.➣ Do not inhale or ingest the dust of broken win-dow material. Avoid any skin contact.Material Chemical propertiesTable 6.12: Window material available for ALPHA (A128D/T)CAUTION1 Switch off spectrometer. ☞ Remove the power cable from the POWER port located on the rear spectrometer side.2 Press the lock on the basic module right down.➣ The sampling module is released from the basic module. The lock stops at half-height.Table 6.13: Replacing windows on ALPHA (A128D/T) sampling module139 Optik GmbH ALPHA User ManualALPHA for gas analysis 63 Pull the sampling module towards your direction to detach the sampling module from the basic module.4 On the rear side of the sampling module, loosen the 3 hexagon socket head cap screws (M3 x 10 mm).5 Tilt the blue hood slightly backwards and pull it out of the housing in upright posi-tion.Table 6.13: Replacing windows on ALPHA (A128D/T) sampling module140 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for gas analysis 66 Loosen the 3 slotted cheese head screws (M2.5 x 8 mm) of both windows.☞ Be careful that the Teflon rings do not get lost.7 • Check the Teflon rings for damage and insert them again.• Insert the new windows. • Slightly and equally fasten the 3 slotted cheese head screws (M2.5 x 8 mm), located on both windows.i To loosen stucked windows, use a pipette and carefully put a few droplets of isopropanol alcohol between window and O-ring. Do by NO means use a screwdriver to lever out the windows.8 Carefully press down the hood into the housing.9 On the rear side of the sampling module, fasten the 3 hexagon socket head cap screws (M3 x 10 mm).Table6.13: Replacing windows on ALPHA (A128D/T) sampling module141 Optik GmbH ALPHA User ManualALPHA for gas analysis 66.4.7.4 After replacing the windowsAfter replacing the windows you have to perform an instrument test. More details are described in chapter 9.5.4.1.6.4.8 Cleaning windowsTo clean KBr windows only use a dry, lint-free cloth. Do NOT use water or solvents as the window material is hygroscopic. To clean ZnSe windows use the cleaning solvents mentioned in chapter 4.10.1To clean BaF2 windows do NOT use acids.10 Push the sampling module towards the basic module.11 Press the lock on the basic module right down and release it.➣ The sampling module is attached tothe basic module.Table 6.13: Replacing windows on ALPHA (A128D/T) sampling module142 ALPHA User Manual Bruker Optik GmbHBruker7 Quick User GuideThis quick user guide gives an overview of the OPUS spectroscopy software, and allows to learn how to perform the most relevant analytical tasks on your own without long train-ing periods. This chapter describes the procedures for the solution of the following practical ques-tions:• Sample Measurement: How to perform a spectroscopic measurement? How to manipulate a sample spectrum? How to save and/or print a spectrum?• Quality Control: Are the delivered goods or the self-made products consistent with the specified quality criteria?• Identification of an unknown substance: What kind of substance is it?• Quantitative Analysis: How much of a certain component does the sample contain?i In OPUS, you can either use the default wizard or the distinctive menu to select the com-mands which allow to measure, manipulate and evaluate spectra. This chapter mainly uses the wizard variant in terms of the single operating process.7.1 Switching on spectrometer1 Connect one end of the data cable to the ETH/LAN port, located on the spectrome-ter rear side.Connect the other end of the data cable to the network/LAN port of the PC.2 • Connect the extra low-voltage connector of the power cord to the POWER port, located on the spectrometer rear side.• Use the clamp to secure the low-voltage connector against unintentional unplug-ging.3 Connect the safety plug of the power cord to the mains socket.Table 7.1: Switching on spectrometer143 Optik GmbH ALPHA User ManualIHO_QUICKGUIDEQuick User Guide 77.2 Starting the OPUS spectroscopy software1. Switch on PC.2. On the Windows Start menu, click the OPUS icon.➣ The ’OPUS Login’ dialog is displayed.3. Enter user ID and password.4. Select the ALPHA.ows workspace.5. Click the Login button.➣ The ’About OPUS’ dialog is displayed.6. Click the OK button.➣ The OPUS user interface is displayed.7.2.1 After starting the OPUS spectroscopy softwareThe performance test1 starts automatically, indicated by a yellow message bubble on the bottom right end of the software interface. Wait until the performance test has finished, and the OPUS status light is green.i If the OPUS status light does not become green, this can be the result of different rea-sons (see chapter 10.2.2). If the performance test fails, see chapter 10.5 et seq.4 Wait until the spectrometer status indica-tora is green.i The spectrometer status indicator becomes green if the IR source is warmed up (after about 7 minutes).a. Further details on the spectrometer status indicator are described in chapter 10.2.1.Table 7.1: Switching on spectrometer1. If the instrument test has expired, the instrument test starts immediately after the performance test has fin-ished. Both tests check whether the spectrometer achieves the specified performance. More information on both tests is given in chapter 10.5 et seq. and appendix D.144 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.3 Measuring7.3.1 Loading measurement experimentIf AAR accessory recognition is activated (which is the case by default), the OPUS spec-troscopy software recognizes the sampling module used. Thus, the experiment file1assigned to the sampling module is automatically loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. Start OPUS. On the Measure menu, select the Setup Measurement Experimentcommand.➣ The Setup Measurement Experiment dialog opens.2. Click the Basic tab.3. Click the Load button and select the distinctive experiment file from the dialog that opens.4. Click the Accept & Exit button.7.3.2 Editing measurement parametersIt is recommended to perform a measurement using the distinctive experiment file with the measurement parameters set by Bruker2.The OPUS spectroscopy software allows to adapt the measurement parameter settings (e.g. the Scan Time parameter value) to your special demands.1. The experiment file contains the default parameters for measurement, set by Bruker. The following experi-ment files are available for the ALPHA spectrometer: ATR_Di.XPM, ATR_Ge.XPM, ATR_ZnSe.XPM, DRIFT.XPM, TRANS.XPM.2. If you use the measurement parameters, the spectrum is stored by default in OPUS/MEAS. The file name is identical to the sample name you have entered in the Measurement dialog. If you do not change the sample name, the file name is incremented with any further measurement.1 • In the wizard, click the Measure level.• Click the arrow next to the Measure but-ton.Table 7.2: Setting up measurement parameters145 Optik GmbH ALPHA User ManualQuick User Guide 77.3.3 Starting background measurementBefore starting sample measurement you first have to perform a background measure-ment, i.e. a measurement without any sample. The measurement conditions must be identical for both the background and sample measurement.Depending on the type of sampling module used, you may have to position a reference mirror to perform the background measurement. Details are described in the different sampling module chapters.1. On the wizard, select the Acquire level and click the Advanced Measurement but-ton.➣ The Measure dialog opens.2. Click the Start Background Measurement button.3. Wait until the background measurement has finished.➣ The progress of the background measurement is shown in the OPUS status bar.7.3.4 Starting sample measurement1. On the wizard, select the Acquire level and click the Advanced Measurement but-ton.➣ The Measure dialog opens.2. Click the Start Sample Measurement button.3. Wait until the sample measurement has finished.➣ The progress of the sample measurement is shown in the OPUS status bar.i When the measurement has finished, the measured sample spectrum is displayed in the spectrum window. The wizard view changes to the Manipulate level.2 • On the pop-up menu, click the Setup Measurement Parameters command.• Change the specific measurement parameters and save the changes made.i Details on the measurement para-meters are described in the OPUS Ref-erence manual.Table 7.2: Setting up measurement parameters146 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.4 Manipulating spectrumAfter sample measurement has finished, a spectrum postprocessing may be required to ensure that the OPUS spectroscopy software yields acceptable evaluation results, for example when you intend to perform a substance identification or a quantitative analy-sis. For this purpose, OPUS provides a number of manipulation commands. In this context, manipulating means optimizing the measured sample spectrum. This chapter describes the following manipulation commands:• baseline correction• atmospheric compensationMore manipulation commands are described in the OPUS Reference manual.7.4.1 Baseline correctionA baseline correction is always highly advisable if the spectrum baseline deviates strongly from a theoretical horizontal line. This phenomenon may occur, for example, when you measure KBr pellets. Figure 7.1 illustrates the effect of a baseline correction.pressure applicator....................................................................... 584.6.1 With the ALPHA-E sampling module...................................................................... 584.6.2 With the ALPHA-P sampling module...................................................................... 594.7 Cleanness test ...................................................................................................... 614.8 Positioning sample on the ATR crystal.............................................................. 624.8.1 Procedure in case of ALPHA-E and ALPHA-P (non-heatable) .............................. 624.8.2 Procedure in case of ALPHA-P (heatable) ............................................................. 634.9 Performing measurement .................................................................................... 654.9.1 Performing non-temperature controlled measurement........................................... 654.9.2 Performing temperature-controlled measurement (only with heatable ALPHA-P) . 664.10 Cleaning ATR sampling module ......................................................................... 694.10.1 Cleaning solvents ................................................................................................... 694.10.2 Procedure ............................................................................................................... 694.11 Cleaning flow-through cell .................................................................................. 704.12 ALPHA ATR multi reflection sampling module (A213/D-11)............................. 714.12.1 Optical path ............................................................................................................ 724 ALPHA User Manual Bruker Optik GmbHBrukerTable of Contents4.12.2 Usable sample material.......................................................................................... 724.12.3 Performing measurement....................................................................................... 734.12.4 Potential operating errors ....................................................................................... 744.12.5 Measuring accessory ............................................................................................. 754.12.6 Cleaning crystal plate ............................................................................................. 754.12.7 Replacing crystal plate ........................................................................................... 765 ALPHA for reflection measurement...........................................................775.1 Overview on ALPHA spectrometer configurations for reflection.................... 775.2 ALPHA-R sampling module (A528/D) ................................................................. 785.2.1 Specifications ......................................................................................................... 795.2.2 Optical path ............................................................................................................ 805.2.3 Software requirements in case of OPUS versionMore details are described in the OPUS Reference manual.Figure 7.1: Baseline correctionSpectrum before a baseline correction has been per-formed.Spectrum after a baseline cor-rection has been performed.147 Optik GmbH ALPHA User ManualQuick User Guide 77.4.1.1 Performing baseline correction7.4.2 Atmospheric compensationAtmospheric compensation eliminates H2O and/or CO2 bands from a sample spectrum. These bands result from the ambient air and occur if there is a difference in the H2O and/or CO2 concentration between the background measurement and sample measurement.Figure 7.2 illustrates the effect of an atmospheric compensation. More details are described in the OPUS Reference manual.1 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 On the Manipulate button, click the Base-line Correction button.➣ The baseline correction is performed. The corrected spectrum is displayed in the spectrum window.i To undo baseline correction, select the Undo Changes command in the Filemenu.Table 7.3: Performing baseline correction148 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.4.2.1 Performing atmospheric compensationi Atmospheric compensation requires a spectrum file that contains an SSC (Sample Sin-gle Channel) and RSC (Reference Single Channel) data block. Otherwise, atmospheric compensation cannot be performed.Figure 7.2: Atmospheric compensationSpectrum before atmospheric com-pensation has been performedSpectrum after at-mospheric compen-sation has been per-formedFigure 7.3: Spectrum file with SSC and RSC data block149 Optik GmbH ALPHA User ManualQuick User Guide 71 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 On the Manipulate button, click the Atmospheric Compensation button.➣ The atmospheric compensation is performed. The manipulated spec-trum is displayed in the spectrum win-dow.i To undo atmospheric compensation, select the Undo Changes command in the File menu.Table 7.4: Performing atmospheric compensation150 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.4.3 Peak pickingPeak picking allows to determine the exact spectrum peak positions very quickly. The spectrum window shows the exact frequency values (x-values), at which maxima (in case of an absorption spectrum) or minima (in case of an transmission spectrum) occur.7.4.3.1 Performing peak picking1 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 Go to the Evaluate level, and click the Peak Picking button.➣ Peak picking is performed.Table 7.5: Performing peak picking151 Optik GmbH ALPHA User ManualIHO_EVAL_PEAKSEARCHQuick User Guide 73 The spectrum window shows the exact frequency values, at which maxima or minima occur.Table 7.5: Performing peak pickingPeak picking result in absorptionPeak picking result in transmission152 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.4.3.2 Performing interactive peak picking1 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 • Go to the Evaluate level, and click the arrow button next to the Peak Picking button.• On the pop-up menu displayed, click the Interactive Peak Picking command.➣ The spectrum window is displayed with an auxiliary line.3• Position the cursor onto the icon.• Press the left mouse button and move the auxiliary line upwards or down-wards.i In case of absorption spectra, the frequency values of all peaks above the auxiliary line are displayed. In case of transmission spectra, the frequency values of all peaks below the auxiliary line are displayed.• Click the button if you want to store the frequency values currently dis-played.➣ After storing the frequency values the PEAKS data block is added to the spectrum file in the OPUS browser.Table 7.6: Performing interactive peak picking153 Optik GmbH ALPHA User ManualQuick User Guide 77.4.3.3 Viewing peak picking result as reportWhen peak picking has finished, the result can be viewed in the form of a report.7.4.3.4 Selecting single peakThe frequency value can also be displayed for one particular peak only.1 • In the OPUS browser, right click the PEAKS data block of the respective spectrum file.• From the pop-up menu displayed, select the Show Peak List command.➣ The report view is displayed.Table 7.7: Viewing peak picking result as reportReport view of peak picking1 • Right click into the spectrum window.• From the pop-up menu displayed, select the Single Peak Pick command.➣ The cursor changes to .Table 7.8: Selecting single peak154 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.5 Evaluating spectrumAfter completing a spectrum manipulation, the wizard changes to the Evaluate level. Now, depending on your particular analytical task (quality control, substance identifica-tion, quantitative analysis etc.) you can evaluate the sample spectrum using the corre-sponding evaluation command from the OPUS spectroscopy software.The following chapters describe the most relevant evaluation commands:• quick compare• spectrum search• quantitative analysisThe remaining available evaluation commands are described in the OPUS Reference manual.7.5.1 Quick compareDuring quick compare, the correct identity of a substance or material is checked. The spectrum of the sample material to be verified is compared with the reference spectra being part of the quick compare method. In a quality control process quick compare allows to check whether the delivered goods or made products are in accordance with the quality criteria defined.Before starting quick compare, you first have to set up a method.2 • Position the cursor onto the desired position.• Press the left mouse button.➣ The frequency value is displayed above the peak desired.Table 7.8: Selecting single peak155 Optik GmbH ALPHA User ManualIHO_FUNCTION_QCOMPQuick User Guide 77.5.1.1 Setting up quick compare methodTo set up a quick compare method, you need to measure at least one reference spec-trum or several reference spectra. Reference spectra are spectra generated by samples which exactly meet the quality criteria defined. These samples are also called reference standards.Observe the following:• use only pure samples as reference standard, i.e. samples without any contami-nants and with unambiguous identity• prepare the reference standards carefully, e.g. homogenizing inhomogeneous samples before starting measurement• avoid errors during measurement, e.g. make sure that the ATR crystal has been carefully cleaned before starting background and sample measurement1 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 • Change to the Evaluate level and click the arrow button next to the Quick Com-pare button.• From the pop-up menu displayed, select the Setup Quick Compare method com-mand.3 In the dialog that opens on the Reference Spectra tab, click the Add Reference Spectra button.4 Select the reference spectra files to be added to the method from the particu-lar directory.➣ A table displays the fileand compound name of the reference spectra as well as information on the sample. The entries in the ’Compound name’ and ’Info column’ are editablea. A maximum of 5,000 reference spectra can be added to a method. The reference spectrum displayed in the first table line is the master spectrum.➣ More details are described in the OPUS Reference Manual.Table 7.9: Setting up quick compare method156 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 75 To select the spectral regions remove the checkmark in front of Use file limits to be able to interactively select the spectral regions.➣ If the checkmark is set, the wavenum-ber range is based on the first - and possibly only - reference spectrum.☞ Select the spectral region which includes the most relevant spectral information of the substance to be analyzed.☞ To define further regions, right click the window. ☞ From the pop-up menu displayed, select the Add Region button.☞ Position the cursor onto the boundary line of the newly added region.☞ While pressing the left mouse button, move the boundary line to the position desired. 6 If you activate the checkbox, spectral regions which contain CO2 bands are excluded during evaluation. This applies to spectral regions from 600 to 680 cm-1 and 2,275 to 2,400 cm-1. Optionally, you can select between different data pre-processing methods. If you check the First or Second Derivative option button, the Smoothing pointsselection box is enabled. The optimal number of smoothing points to be set for the specific pre-processing method has to be determined empirically.7 • On the Validate tab, define the thresh-oldb which determines how similar the reference and query spectrum must be so that the quick compare result is OK.• Click the Validatec button.➣ The reference spectra are validated and evaluated as follows:Table 7.9: Setting up quick compare method157 Optik GmbH ALPHA User ManualQuick User Guide 77.5.1.2 Performing quick compareWhen performing quick compare you have to observe the following with regard to the spectrum file(s):• The data blocks of sample and reference files have to be of the same spectrum type, i.e. AB (absorption) or TR (transmission).• The wavenumber range of the sample spectrum has to be at least as large as the range defined for the reference files.Green entry:• The correlation coefficient of all spectra compared is below the threshold defined. Clicking the plus sign in front of the entry shows the neighboring spectrum.• The reference spectra have the same substance name. The correlation value is identical for the particular references spectra, but may be above the threshold.Red entry:• The correlation coefficient of all spectra compared is above the threshold defined.• The reference spectrum cannot be distinguished from the others, as they are too similar. Clicking the plus sign in front of the entry shows the names of the reference spectra being too similar.8 • On the Method tab, click the Store Method button.• In the dialog that opens, enter a name for the method and click the Save but-ton.i Quick compare method files have the file extension *.qc.a. Equal or very similar compounds or material can be can be put together in one group, by entering the same compound name. This can be useful if spectra of the same material, but of different batches, are intended to be used in the method.b. The threshold can be between 90 and 100%. For quality control, enter a threshold between 96 and 99%.c. Validating reference spectra checks the similarity between the spectra to each other. Each reference spec-trum is compared with all other reference spectra. This kind of spectrum comparison is based on the cor-relation coefficient, which defines the correlation between at least two spectra.Table 7.9: Setting up quick compare method158 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.5.1.3 Quick compare resultThe quick compare result is immediately displayed in a separate view after quick com-pare has finished, and saved in the QC ( ) data block. This data block is attached to the spectrum file and displayed in the OPUS browser. The result view can also be opened by double clicking the QC data block.Table 7.11 contains the possible result for the Material verification and Material identifi-cation evaluation mode.1 • In the wizard, on the Acquire level click the Measurement button.• In the dialog that opens, click the Back-ground Single Channel button, then the Sample Single Channel button.➣ Details on measurement are described in chapter 7.3 et seq.2 After the measurement has finished, go to the Evaluate level in the wizard and click the Quick Comparea button.➣ The quick compare result is displayed in the spectrum window.a. Alternative: Click the arrow button next to the Quick Compare button. From the pop-up menu displayed, select the Select Quick Compare Method command. In the dialog that opens, you may select a different type of evaluation mode or load a different method, and click the Compare button. The Material verification evaluation mode checks the conformity between query spectrum and a particular user-defined reference substance. The substance is selected from the drop-down list, which contains the entries available in the method. In case of the Material identification evaluation mode, the query spectrum is compared to all reference spectra available in the method to identify the substance with the best confor-mity.Table 7.10: Performing quick compare159 Optik GmbH ALPHA User ManualQuick User Guide 7Result Material verification Material identificationMaterial is identical toaa. Only one reference spectrum is above the threshold.Material is identified asaMaterial is not identical tobb. The reference spectrum selected is below the threshold. It is possible, however, that the query spectrum is conform with a different reference substance.Material is not identifiedcc. No reference spectrum is above the threshold.No unique identification pos-sibledd. Several reference substances have been found which are above the threshold.No unique identification possi-bledTable 7.11: Quick compare result 160 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.5.1.4 Result viewThe structure of the result view is the same for both evaluation modes. Figure 7.4 exem-plifies the result view for the Material verification mode.Component Definition1 Spectrum window The query spectrum is displayed in red in the spectrum window. All the other spectra originate from the hit list (see 4 in this table).☞ Hiding crosshair: right click the spectrum window☞ Opening pop-up menu: right click the spec-trum window- Autoscale-mode: spectra are displayed in their original size ratio- Maximize-Y-mode: allows to maximize the spectra on the y-axis2 Result display Details are described in chapter 7.5.1.3.3 Query spectrum During quick compare, the query spectrum is compared with one or several reference spectra.Table 7.12: Setting options of quick compare321Figure 7.4: Quick compare result view4161 Optik GmbH ALPHA User ManualQuick User Guide 77.5.1.5 Viewing quick compare result as reportWhen quick compare has finished, the result can be viewed in the form of a report.4 Hit list The hit list contains the reference spectra which come close to the query spectrum, or are identical to it. By default, one hit is activated and displayed with the query spectrum in the spectrum window.Component DefinitionTable 7.12: Setting options of quick compare1 • In the OPUS browser, right click the QC data block of the respective spectrum file.• From the pop-up menu displayed, select the Show Report command.➣ The report view is displayed.Table 7.13: Viewing quick compare result as reportReport view of quick compare162 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.5.2 Spectrum searchIn case of spectrum search, an unknown spectrum is compared with spectra stored in a library. Those spectra from the library which show distinct similarities to the unknown spectrum are detected and displayed in a search report.The degree of consistency between query spectrum and library spectra is indicated as hit quality.Spectrum search is only possible if at least one spectra library is available. By default, the following spectra libraries are supplied:• DEMOLIB.SO1• SR.IDXThe spectra libraries are stored in the C:\Users\Public\Documents\Bruker\[OPUS_Ver-sion]\Data\Library directory and contain 350 or 200 entries. Both libraries contain numer-ous classes of substances (e.g. polymers, pharmaceuticals etc.).A decisive factor for a successful substance identification is the availability of spectra libraries, i.e. a spectrum search can only yield acceptable results if the selected library contains entries (i.e. spectra plus additional information) of the classes of substances that you actually analyze.7.5.2.1 Performing spectrum search1 • In the wizard, on the Acquire level click the Load File button.• Select the desired spectrum file from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.Table 7.14: Performing spectrum search163 Optik GmbH ALPHA User ManualIHO_EVAL_SPECSEARCHQuick User Guide 72 Change to the Evaluate level and click the Spectrum Search button.➣ Spectrum search is performed using the search parameters set by Bruker.➣ The SEARCH data block is added to the spectrum file in the OPUS browser.Table 7.14: Performing spectrum search164 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 7The result view consist of different windows which can be resized by dragging the split bars to the desired position.3 The search result is displayed in the spectrum window:A) Structural formula of the hits highlighted in Di The structural formula is only displayed if one is stored for the particular substance in the library.B) Compound information of the hit highlighted in DC) Spectrum window with query and/or hit spectrum:• the color of the query spectrum is always red (see E)• to hide the crosshair right click into the window• right clicking opens a pop-up menu which provides further setting options: the Autoscale-mode is set by default, which means that the spectra are displayed in their original size ratio; the Maximize-Y-mode allows to maximize the spectra on the y- axisD) List of hits found, sorted according to the hit quality:• by default, the first hit is activated; the hit highlighted determines the data provided in A and B• additional list entries are: compound name, entry number, molecular formula, molecular weight and CASa number• right clicking on a particular substance name allows to start info or internet search about the substanceE) Query spectruma. CAS: Chemical Abstracts Service; international unique numerical identifiers assigned by the Chemical Ab-stracts Service to every chemical described in the open scientific literatureTable 7.14: Performing spectrum searchABCDE165 Optik GmbH ALPHA User ManualQuick User Guide 77.5.2.2 Viewing spectrum search result as reportWhen spectrum search has finished, the result can be viewed in the form of a report.7.5.2.3 Generating user-specific libraryThe following commands are available in the OPUS spectroscopy software to generate a user-specific library:• Initialize Library• Edit Library• Library BrowserDetailed information about these commands are described in the OPUS Reference manual.When creating a user-specific spectra library, the following aspects are very important preconditions to be able to get acceptable search results when identifying unknown sub-stances.• When selecting the samples for the library, make sure that they cover the hole range of the class(es) of substances you want to analyze.• Use only pure substances, i.e. substance that are free of unwanted contami-nants.• Prepare the samples carefully (chapter 8).• Avoid measurement errors, e.g. the ATR crystal is not covered completely with the sample.• Before adding the measured sample spectra to the library, optimize them by using the available manipulation commands.1 • In the OPUS browser, right click the SEARCH data block of the respective spectrum file.• From the pop-up menu displayed, select the Show Report command.➣ The report view is displayed.Table 7.15: Viewing spectrum search result as reportReport view of spectrum search166 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 7• Preferably, add absorption spectra1 to the library.• Consider what kind of additional information (e.g. boiling point) you want to include into the library, and make sure that this kind of information is available.7.5.3 Quantitative analysisIf the sample is a mixture of several components, e.g. a tablet containing several active agents, the OPUS spectroscopy software allows to quantify one of these components. To realize quantitative analysis, the following commands are available in OPUS:• Quant Builder - to set up a quantitative (QUANT) method• Quantitative Analysis - to perform the actual quantitative analysisTo perform quantitative analysis observe the order described in the following chapters.7.5.3.1 Creating a set of calibration samples☞ Ideally, the set of calibration samples should contain at least 5 samples.☞ From these calibration samples, determine the exact concentration value of the component to be analyzed using a different technique (e.g. weighing).☞ When selecting the calibration samples for the set, make sure that the concentration value of the component to be analyzed is different with each calibration sample.i Before starting quantitative analysis, it is highly recommended to normalize all spectra, i.e. both the calibration spectra and the spectra of the sample(s). Spectra normalization is an OPUS manipulation command. Normalizing means that the spectra are scaled such that the minimum and/or maximum of the spectra assume the same value. There-fore, the spectra can be better compared with each other. Especially in case of ATR spectra, a normalization is highly recommended. Detailed information on normalization is given in the OPUS Reference manual.1. In case of an IR spectrum, the position and intensity of the absorption bands are very substance-specific. Therefore, the IR spectrum - similar to a human fingerprint - is well-suited to identify substances.167 Optik GmbH ALPHA User ManualQuick User Guide 77.5.3.2 Creating QUANT method1 • In the wizard, on the Acquire level click the Advanced Measurement button.• In the dialog that opens, click the Back-ground Single Channel button, then the Sample Single Channel button to measure one sample from the calibra-tion sample set.➣ Details on measurement are described in chapter 7.3 et seq.2 • After the measurement has finished, go to the Evaluate level in the wizard and select the Quant Builder command.• Click the GO button.➣ The Quant Builder New dialog is dis-played.3 Enter the name of the component to be analyzed.☞ Position the cursor into the entry field, delete the default name and enter the new name.Table 7.16: Creating QUANT method168 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 74 Specify the unit (mg, ml or %) of the con-centration value. i The unit to be specified depends on the unit which you have used to determine the concentration values of the calibra-tion samples. The result of the quantita-tive analysis is also indicated in this unit.5 Enter concentration valuea of the sample.➣ OPUS calculates a calibration straight lineb. This calibration straight line is further refined as soon as the data of all calibration samplesare entered.Calibration straight line:Table 7.16: Creating QUANT method169 Optik GmbH ALPHA User ManualQuick User Guide 76 Activate the New option button.i The New option button must only be activated when adding the very first calibration spectrum to a new QUANT method. When adding any further cali-bration spectrum, activate the Add spectrum option button.7 • Click the Save button.• Define the name and path of the method file.i The method file has the file extension *.q1.8 • In the wizard, on the Evaluate level click the Measure Next Sample button.• Repeat the steps 1 - 5 for all the other calibration spectra to be added to the method. The name and unit of the component are set by default.• With step 6, activate the Add spectrum option button.• Store all calibration spectra as described with step 7.i It is recommended to set the integration area not until at least 3 or 4 cali-bration spectra have been added to the QUANT method. At an earlier stage, it is probably not possible to clearly see which band results from the component to be analyzed.9 • Click the Change button.• Click the Load Method button and load the respective method.• Click the Set Integration Area button.Table 7.16: Creating QUANT method170 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 710 The dialog for setting integration areas is displayed:A) Band selected in the spectrum. This band can be assigned to the com-ponent to be analyzed, and should not be overlapped by other sample components. The spectral intensity of this band corresponds to the con-centration of the component to be analyzed with each single spectrum.☞ Define the integration method☞ Interactively define the limits of the integration area. Position the cursor onto a boundary and move the area while pressing the left mouse but-ton.☞ Click the Go to Quant button.11 Click the Save button.➣ Quant Builder is closed.a. The concentration value has to be determined first, by using a different analytical technique.b. The calibration straight line is the relation between the calibration spectra and the concentration values of the respective component. In case of a quantitative analysis of a sample, which contains an unknown con-centration value, OPUS can calculate the quantity of this component on the basis of the sample spectrum.Table 7.16: Creating QUANT methodA171 Optik GmbH ALPHA User ManualQuick User Guide 77.5.4 Performing quantitative analysis1 • In the wizard, on the Acquire level click the Load File button.• Select the spectrum file of a sample measured before, which contains an unknown concentration value of a com-ponent, from the dialog shown.➣ The spectrum is displayed in the spectrum window. The Manipulate level is shown on the wizard.2 • Change to the Evaluate level and click the Quantitative Analysis button.➣ The quantitative analysis is immedi-ately performed on the basis of the QUANT methoda recently generated or used.a. If a different kind of method is to be used, in the wizard on the Evaluate level click the arrow next to the Quant Analysis button. From the pop-up menu displayed, click the Select Quant Analysis method button. In the dialog that opens, click the Load Quant method button and select the desired method.Table 7.17: Performing quantitative analysis172 ALPHA User Manual Bruker Optik GmbHBrukerQuick User Guide 77.5.5 Viewing quantitative analysis result as reportWhen quantitative analysis has finished, the result can be viewed in the form of a report.1 • In the OPUS browser, right click the QUANT data block of the respective spectrum file.• From the pop-up menu displayed, select the Show Report command.➣ The report view is displayed.i The value indicated in the Sigma column is the standard deviation of the calculated concentration value. The sigma value is determined by the quality of the QUANT method set up. Ideally, the sigma value should be as small as possible.Table 7.18: Viewing quantitative analysis result as reportReport view of quantitative analysis173 Optik GmbH ALPHA User ManualQuick User Guide 7174 ALPHA User Manual Bruker Optik GmbHBruker8 Sample PreparationProper sample preparation is crucial to obtain good and meaningful spectra. This chap-ter describes the most important sample preparation methods1.Useful information helps you to select the most suitable sample preparation method for a given sample and the measuring technique selected.8.1 What is to be observed?1. For more detailed information about the different sample preparation methods refer to the relevant special-ist literature.How must the sample be like? homogeneous (constant concentration or com-position within the sample area to be analyzed)Disadvantages of a non-homo-geneous sample:• measuring data do not represent the sample• depending on the measuring technique used, spectral artefacts are possibleWhat has to be considered when selecting a sample preparation method?• aggregation state of the sample• absorptivity of the sampleWhat has to be considered in case of a highly absorbing sam-ple?• sample has to be very thin• sample has to be diluted by a solvent or pow-der that is not highly absorbing, otherwise the spectrum is not meaningfulWhat kind of solvents can be used?• carbon tetrachloride• carbon disulphide• chloroform• cyclohexane• acetonitrile• tetrachloroethyleneTable 8.1: Sample preparation - What is to be observed175 Optik GmbH MAGNETOM Sonata User ManualSample Preparation 88.2 Sample preparation methodsThe most common sample preparation methods are:• No sample preparation• KBr pellet (for solids)• Thin film between two transparent plates (for liquids)• Gaseous samplesi Most of the described sample preparation methods involve the use of hygroscopic ma-terial (such as NaCl or KBr). If this type of material comes in contact with water or alco-holic solvents, it begins to dissolve or becomes cloudy and thus, impairs the measure-ment results. Therefore, protect hygroscopic material from any sources of water, and even alcohol (ethanol and methanol).8.2.1 No sample preparationType of samples: films and polymers, with a thickness of less than approx. 100 µmTip: a large number of solid and liquid samples can also be analyzed by using an ATR unit; this measuring method does not require any sample preparation eitherAdvantage of this method: enables fast sample measurementsDisadvantage of this method: • ATR: an absolute quantification is not possible in case of solids• Transmission: sometimes samples are too thickTable 8.2: No sample preparation176 MAGNETOM Sonata User Manual Bruker Optik GmbHBrukerSample Preparation 88.2.2 KBr pelletType of samples: solidsWhat is to be observed during sample preparation?• grind the sample as fine as possible to mini-mize the infrared light scattering on the particle surface, and the portion of the reflected light• keep everything moisture free as the KBr material is hygroscopic, otherwise the pellets become cloudy• it would be best to keep the KBr material in a drying oven at a temperature of 50 to 60°CTip: a common mistake is to use too much sample material; the concentration of the sample in KBr should be between 0.2% and 1% (i.e. typically a mixing ratio of 300:1)Advantage of this method: • meaningful IR spectrum• KBr shows no absorption in the wavenumber area of 4000 cm-1 to 250 cm-1• this prevents the sample spectrum from con-taining any disturbing absorption bandsDisadvantage of this method: • time-consuming sample preparation method• interference of water bands (3,960 to 3,480 cm-1 and 1,950 to 1,300 cm-1 and below 500 cm-1)• in some cases there may be structural changes caused by high pressure applied to the KBr/sample mixtureTable 8.3: Sample preparation - KBr pellet177 Optik GmbH MAGNETOM Sonata User ManualSample Preparation 88.2.3 Thin film between two transparent plates8.2.4 Gaseous samplesType of samples: liquids (e.g. oils)What is to be observed during sample preparation?• pipette one drop of the sample on one of the plates• to avoid air bubbles the liquid sample between the two plates has to be a uniform film• to be able to perform a quantification you have to set a defined layer thickness, use cuvettesTip: • do not use the plates in case of samples that contain water as the plate material (NaCl or KBr) is extremely moisture-sensitive• keep the plates always dry (e.g. in an exicator)• clean the plates only by using chloroform or high purity acetone and polish them carefully after each useAdvantage of this method: • easy sample preparation method• small amount of sample material required• quantification is possibleDisadvantage of this method: • not suitable for samples which contain water• the material of the plates (NaCl or KBr) are extremely moisture-sensitive• very often there are air bubbles between the platesTable 8.4: Sample preparation - Thin film between two transparent platesWhere to inject the sample? into an evacuated gas cellThe intensity of the peak measured is influenced by:• thickness of gas cell• pressure of gas inside the gas cell (pressure is proportional to the concentration)• absorption coefficients of the bandsTable 8.5: Sample preparation - Gaseous samples178 MAGNETOM Sonata User Manual Bruker Optik GmbHBruker9 MaintenanceThe ALPHA spectrometer is a low-maintenance instrument, i.e. the operator can replace components with a limited service life (e.g. IR source). The following maintenance pro-cedures are described in this chapter: • Replacing IR source• Replacing desiccant bags• Replacing windows9.1 General maintenance considerationsPerform only the maintenance procedures described in this chapter. Strictly observe the relevant safety precautions. Any failure to do so may cause property damage or per-sonal injury. In this particular case Bruker does not assume any liability. Maintenance procedures not described in this manual should only be performed by a Bruker service engineer. For service addresses, see the appropriate appendix.The following precautions must be observed to ensure user and property safety:• Disconnect power supply before performing any maintenance procedures. • Be careful if the spectrometer covers are removed and the spectrometer is switched on to avoid contact with potentially harmful voltages.9.2 Performing OQ1 test by using OVP2If you have exchanged a defective optical component, e.g. light source or laser, we rec-ommend running the OQ test using the OPUS validation software (OVP). This test checks whether the spectrometer achieves the specified performance parameter values.Perform the OQ test only if you have replaced a defective component. Do not perform the OQ test if you have replaced a component for the purpose of spectral range exten-sion.More details on how to perform an OQ test are described in the OPUS Reference man-ual. If the OQ test fails, read about possible causes and solutions in the Troubleshootingchapter.1. OQ test - Operational Qualification Test: This test is to be performed once a year, or after the replacement of any kind of defective optical component. During the OQ test, the following parameters are tested: resolution, sensitivity, energy distri-bution, wavenumber accuracy and photometric accuracy.2. OVP (OPUS Validation Program) is a program used to perform validation tests (e.g. OQ and PQ).179 Optik GmbH ALPHA User ManualMaintenance 99.3 Replacing IR sourceThe ALPHA spectrometer uses a highly efficient, low power, air-cooled IR source. The IR source is accessible from the spectrometer rear side and is located behind the cover plate. The light source is pre-aligned. The average IR source lifetime is specified with about 44.000 operating hours.9.3.1 Display in the OPUS spectroscopy software9.3.2 ProcedureStatus of IR source Display in OPUS Message in OPUS MeasurementLifetime of spectrometer nearly reachedOPUS status lighta is yellowEnd of average life-time is nearly reached, spare part will be required.still possiblebDefective OPUS status light is redSource is broken. not possibleTable 9.1: Display in OPUS the spectroscopy softwarea. The OPUS status light is located in the lower right end of the OPUS interface.b. To retrieve the status information click the yellow OPUS status light. Then, click the Ignore button. The status light turns green again. After intervals which always become shorter, the IR source operating hour meter will remind you again to re-place the IR source.1 Switch off spectrometer. ☞ Remove the power cable from the POWER port located on the rear spectrometer side.2 Loosen the 4 TORX screws of the rear cover plate. ☞ Use the TORX TX20 screw driver supplied.Table 9.2: Replacing IR source180 ALPHA User Manual Bruker Optik GmbHIHO_INSTR_SOURCEIHO_MOVIETAG#Movie: #repsource.mpg#Replacing IR source#BrukerMaintenance 93 Remove the cover plate. IR source very hotRisk of skin burn.➣ Have the IR source cooled down, before replacing it.4 Loosen the two fixing screws of the IR source.☞ Use the TORX TX20 screw driver supplied5 Strip off the green IR source plug from the SRC female connector.6 • Remove the used IR source.• Insert the new IR source.☞ The alignment pin (arrow in figure) must correctly fit in the alignment groove.7 Fasten the two TORX screws.Table 9.2: Replacing IR sourceCAUTION181 Optik GmbH ALPHA User ManualMaintenance 98 Insert the green IR source plug into the SRC female connector.9 Attach the cover plate and fasten the 4 TORX screws.10 Switch on spectrometer.☞ Insert the power cable into the POWER port located on the rear spectrometer side.Table 9.2: Replacing IR source182 ALPHA User Manual Bruker Optik GmbHBrukerMaintenance 99.3.3 After replacing the IR sourceAfter replacing the IR source, you have to perform an instrument test.9.3.3.1 Performing instrument test9.4 Replacing desiccant bagsToo high a humidity inside the spectrometer can be recognized by H2O bands in the spectrum. To minimize this undesirable spectral effect as far as possible, the desiccant bags inside the spectrometer bind humidity.The air inside the complete spectrometer optics unit (measuring and optics compart-ment) is convectively kept dry using a desiccant which is enclosed in removable small bags.1 On the wizarda, click the Instrument Test button.➣ The test starts and takes about 5 min-utes.a. Alternatively, you can click the OPUS status light. On the dialog shown, click the icon displayed for the cur-rent measurement channel. The instrument test starts.2 Wait until the test has finished.➣ If the test has passed, the OPUS status light must be green.Table 9.3: Performing instrument test183 Optik GmbH ALPHA User ManualMaintenance 99.4.1 Replacing intervalIf the desiccant is saturated and cannot further absorb any humidity, it has to be replaced. In this case, the Humidity out of range message is displayed in the OPUS spectroscopy software.Besides, the OPUS status light ( ) becomes yellow. Order new desiccant bags. Measuring is still possible even if the status light is yellow. As soon as you have received the new desiccant bags, replace the old ones.9.4.2 Replacing procedure1 Switch off spectrometer. ☞ Remove the power cable from the POWER port located on the rear spectrometer side.2 Loosen the 4 TORX screws of the rear cover plate. ☞ Use the TORX TX20 screw driver supplied.3 Remove the used desiccant bags.☞ A pair of tweezers may be helpful.i Do not cut or tear off the bags into sin-gle pieces, nor ingest the desiccant.4 The replacement desiccant bags are protected by an extra packaging. ☞ Open this packaging and take out the desiccantbags. Alternatively, place the used bags into an oven at 130°C for at least 10 minutes.☞ Completely insert the new desiccant bags properly.5 Attach the cover plate and fasten the 4 TORX screws.Table 9.4: Replacing desiccant184 ALPHA User Manual Bruker Optik GmbHIHO_MOVIETAG#Film: #repdesiccant.mpg#Trockenmittel austauschen#BrukerMaintenance 99.5 Replacing windowsThe ALPHA basic module has one beam output and one beam input port. The beam enters the sampling module by the output port, and is then directed to the basic module again via the IR input port. The ports are closed by means of exchangeable IR transpar-ent windows.9.5.1 Window materialThe serial number, which is located on the rear spectrometer side, indicates what type of window material is used for the IR transparent windows.6 Switch on spectrometer.☞ Insert the power cable into the POWER port located on the rear spectrometer side.Table 9.4: Replacing desiccantMaterial Chemical propertiesPotassium bromide (KBr)Soluble in water, alcohol, and glycer-ineHygroscopic!➣ Avoid any contact to humidity.Zinc selenide (ZnSe) Soluble in strong acids and HNO3Toxic!➣ Observe the safety data sheet.➣ Do not inhale or ingest the dust of broken window material. Avoid any skin contact.Table 9.5: ALPHA - Window materialNOTECAUTION185 Optik GmbH ALPHA User ManualMaintenance 99.5.2 Replacing interval9.5.3 Replacing procedureSpectrometer type Serial number Window materialALPHA Basic 1003271 KBr (hygroscopic)1005151ZnSe ( toxic)ALPHA Basic HR 1010948 KBr (hygroscopic)1010951ZnSe ( toxic)Table 9.6: Window material identified by serial numberKBr window material ZnSe window materialReplacing inter-valwhen opaqueOpaque windows substan-tially reduce infrared trans-mittance which can be indicated by a failed perfor-mance or instrument test.only when brokenTable 9.7: Replacing interval1 Switch off spectrometer. ☞ Remove the power cable from the POWER port located on the rear spectrometer side.Table 9.8: Replacing windows186 ALPHA User Manual Bruker Optik GmbHBrukerMaintenance 92 Press the lock on the basic module right down.➣ The sampling module is released from the basic module. The lock stops at half-height.3 Pull the sampling module towards your direction to detach the sampling module from the basic module.The windows are located on the inner side of the basic module. 4 ☞ To remove the windows use the assembly tool supplied.• Insert the two pins of the assembly tool into the respective holes on the basic module window frame.• Rotate the tool several turns counter-clockwise and pull out the tool including the window assembly (i.e. window and assembly frame).• Remove the used window from the assembly tool.5 • Insert the two pins of the assembly tool into the respective holes of the assembly frame of the NEW window.• Put the window assembly into the holes on the basic module window frame.• Rotate the tool several turns clockwise to fasten the window.• Carefully remove the assemble tool.Table 9.8: Replacing windows187 Optik GmbH ALPHA User ManualMaintenance 99.5.4 After replacing the windowsAfter replacing the windows you have to perform an instrument test.9.5.4.1 Performing instrument test6 Push the sampling module towards the basic module.7 Press the lock on the basic module right down and release it.➣ The sampling module is attached to the basic module.Table 9.8: Replacing windows1 On the a wizard, click the Instrument Test button.➣ The test starts and takes about 5 min-utes.a. Alternatively, you can click the OPUS status light. On the dialog shown, click the icon displayed for the cur-rent measurement channel. The instrument test starts.2 Wait until the test has finished.➣ If the test has passed, the OPUS status light must be green.Table 9.9: Performing instrument test188 ALPHA User Manual Bruker Optik GmbHBrukerMaintenance 99.5.5 Cleaning windowsTo clean the KBr windows only use a dry, lint-free cloth. Do NOT use water or solvents as the window material is hygroscopic. To clean the ZnSe windows use the cleaning sol-vents mentioned in chapter 4.10.1.9.6 Cleaning spectrometer housingThe outer spectrometer surface can be cleaned only by using a dry or damp cloth. Do not use detergents with organic solvents, acid or base!189 Optik GmbH ALPHA User ManualMaintenance 9190 ALPHA User Manual Bruker Optik GmbHBruker10 TroubleshootingThis chapter describes possible spectrometer problems1, their potential causes and rec-ommended solutions.Spectrometer problems can be indicated by: • spectrometer status indicator and OPUS status light• diagnostics LEDs on the rear spectrometer side• error messages in OPUS • instrument/performance test10.1 General information on fault diagnosticsA problem caused by a spectrometer component, that is either defective or not properly installed or not in operating condition, becomes apparent in several different ways. For example:• You have started a measurement, but not any measurement result is displayed in OPUS.➣ Reason: OPUS did not start any measurement at all.• No signal detected in OPUS.➣ Reason: Wrong OPUS parameters selected.• You have started a validation test but OVP does not display a PQ or OQ test pro-tocol. ➣ Reason: OVP did not start the validation test at all.To find out the concrete cause of a spectrometer problem, it is advisable to narrow down the problem in a systematic way. We recommend the following fault diagnostics proce-dure:• First, check the status LEDs on the spectrometer and the OPUS status light (chapter 10.2.1 and 10.2.2). If the OPUS status light is red, click the status light. The diagnostics view opens.• Check whether one hardware component has the status WARNING or ERROR. If yes, whether an error message is displayed for the respective component.Check the firmware diagnostics page (chapter 10.4.1) of the respective hardware com-ponent. Check whether there is any kind of reference to the possible cause of the prob-lem.1. Not all failures and causes can be outlined in this chapter. If the recommended solutions do not solve the problem, contact Bruker Service (chapter 1.6).191 Optik GmbH ALPHA User ManualTroubleshooting 1010.1.1 Remote fault diagnosticsRemote fault diagnostics means that you send a complete spectrometer status report (also called Full Report) to Bruker via e-mail. This report enables a Bruker service tech-nician to perform a first remote fault diagnostics.The procedure for sending the report is different and depends on whether your spec-trometer is connected to a network, network PC or a stand-alone PC.10.1.1.1 If your spectrometer is connected to a network/network computer,...With the OPUS spectroscopy software version 6 or higher, it is possible to send the full report to Bruker via e-mail. Proceed as follows:1. Click the OPUS status light (chapter 10.2.2). The Instrument Status dialog opens.2. Click the Send Report button. Clicking this button sends the report to the ser-vice.bopt.de@bruker.com e-mail address.i To be able to use this feature an e-mail program must be installed on the network com-puter, and an e-mail account set up.10.1.1.2 If your spectrometer is connected to a stand-alone computer,...☞ Generate a full report:1 • Open the Web browser.• Enter the spectrometer IP address into the address entry field.• On the configuration page, click Ser-vice.2 Click the Full Report option. The cur-rent full report is displayed.3 • On the File menu of the Web browser, click the Save as command.• Use the file extension *.htm.• Send the original htm file to Bruker. Do not generate any screenshots or text files.Table 10.1: Generating full report192 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 10i Save the full report immediately after a problem or failurehas occurred. Otherwise, important information will be overwritten by newer entries.☞ Transfer the full report file to a network computer.➣ Make sure that an e-mail program is installed on this network computer, and an e-mail account set up.☞ Send the full report to service.bopt.de@bruker.com as an attached file.i Save the full report immediately after a problem or failure has occurred. Otherwise, important information will be overwritten by newer entries.10.2 Retrieving spectrometer statusThe spectrometer status can be retrieved by means of:• status indicator on the spectrometer housing1• status light in the OPUS spectroscopy software1• diagnostics LEDs on the spectrometer1 • Open the Web browser.• Enter the spectrometer IP address into the address entry field.• On the configuration page, click Ser-vice.2 Click the Full Report option. The cur-rent full report is displayed.3 • On the File menu of the Web browser, click the Save as command.• Use the file extension *.htm.• Send the original htm file to Bruker. Do not generate any screenshots or text files.Table 10.2: Generating full report1. In most cases, the color of the status indicator located on the spectrometer housing corresponds to the OPUS status light. Exception: if the performance or instrument test has failed, the OPUS status light is red whereas the status indicator is yellow.193 Optik GmbH ALPHA User ManualTroubleshooting 1010.2.1 Status indicator on the spectrometer housingFor each spectrometer configuration the status LED is located on the front spectrometer side.The status indicator can indicate different types of operating states:Status indicator DefinitionGreen (permanent) Spectrometer operates properlyGreen (flashing) Spectrometer is in stand-by modeYellow • Spectrometer is in the initialization phase• Warning is indicated (e.g. IR source has not yet reached its operating temperature, the air humidity content inside the spectrometer is too high etc.)Red • Spectrometer is not able to operate• Malfunction• Defective hardware componentTable 10.4: Status indicator on the spectrometer housingTable 10.3: Status indicator on the spectrometer housing194 ALPHA User Manual Bruker Optik GmbHBrukeTroubleshooting 1010.2.1.1 Troubleshooting in case of problems indicated by the spectrometer status indicatorPossible cause TroubleshootingSpectrometer status indicator is offSpectrometer not connected properly to mains supplyConnect spectrometer to mains sup-ply.No voltage applied Check whether the proper voltage is applied at the mains outlet.Short circuit in the mains adapter i A short circuit is accompanied by a "ticking" sound in the mains adapter.☞ Disconnect power supply imme-diately and contact Bruker Ser-vice.Non of the possible causes applyContact Bruker Service (chapter 1.6).Spectrometer status indicator is yellowSpectrometer still initializes Wait until initialization has been completed (about 5 minutes).IR source has not yet reached operating temperature➣ In this case, the following message is displayed: Device not readyWait until the IR source is ready to operate.i The IR source warm-up takes about 7 minutes. As soon as the IR source has reached its operat-ing temperature the spectrometer status indicator becomes green.Specified lifetime of the IR source nearly reached ➣ In this case, the following message is displayed: End of average lifetime is nearly reached, spare will be required.• Order new IR source with Bruker.• After receipt replace the used IR source (chapter 9.3).i As long as the lifetime is not expired, measuring is still possi-ble. To turn the OPUS status light green again, click the Ignore but-ton on the Instrument Status Mes-sage dialog (table 10.16 on page 213).Performance or instrument test failedDetails are described in chapter 10.5 et seq.Table 10.5: Troubleshooting in case of problems indicated by the spectrometer status indicator195 r Optik GmbH ALPHA User ManualTroubleshooting 10Instrument test validity period is expired. ➣ In this case, the following message is displayed in the yellow information bubble (table 10.16 on page 213): An instru-ment test is required or one of the instrument components does not meet its specifications☞ Click the OPUS status light.➣ The Instrument Status dialog opens. The measurement channel must read EXPIRED.Close the dialog and start a new instrument test:☞ On the wizard, click the Instru-ment Test button.Air humidity inside the spec-trometer is too high ➣ In this case, the following message is displayed: Humidity out of range.Replace desiccant (chapter 9.4).Laser wavenumber must be recalibrated ➣ In this case, a respective message is displayed in a yellow information bub-ble (table 10.16 on page 213).In the information bubble, click the Calibrate button.Too high a temperature inside the spectrometer due to too high an ambient temperature➣ In this case, the following message is displayed: Temperature out of range.Operate the spectrometer only within the specified temperature range between 18 and 35°CNon of the possible causes applyContact Bruker Service.Possible cause TroubleshootingTable 10.5: Troubleshooting in case of problems indicated by the spectrometer status indicator196 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 10Spectrometer status indicator is redDefective hardware compo-nentDetect the defective component:☞ Click the OPUS status light.➣ The Instrument Status dialog opens.i If the laser or the interferometer, electronics, automation or the detector is defective, contact Bruker Service. If the IR source is defective, replace the IR source (chapter 9.3).The sampling module is not properly attached to the basic module.Attach the sampling module properly (chapter 2.2).ATR module: ATR-crystal plate not installed properly Install the ATR-crystal plate properly (chapter 4.5).Non of the possible causes applyContact Bruker Service.Possible cause TroubleshootingTable 10.5: Troubleshooting in case of problems indicated by the spectrometer status indicator197 Optik GmbH ALPHA User ManualTroubleshooting 1010.2.2 Status light in the OPUS spectroscopy softwareThe status light in the OPUS spectroscopy software is located on the lower right end of the interface. It indicates the status based on the currently active channel or measure-ment experiment loaded.The OPUS status light can indicate different types of operating states.LED DefinitionGray:no spectrometer connectedGreen:spectrometer is connected and works properlyYellow:warning (e.g. service life of a spectrometer com-ponent comes to an end, instrument test has expired etc.)i Measuring is still possible.Red:error (e.g. spectrometer malfunction, defective spectrometer component, instrument test failed etc.)i Measuring is not possible.Table 10.6: OPUS status light198 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.2.2.1 Troubleshooting in case of problems indicated by the OPUS status lightPossible cause TroubleshootingSpectrometer status indicator is yellowIR source has not yet reached operating temperature➣ In this case, the following message is displayed: Device not readyWait until the IR source is ready to operate.i The IR source warm-up takes about 7 minutes. As soon as the IR source has reached its operat-ing temperature the spectrometer status indicator becomes green.Specified lifetime of the IR source nearly reached➣ In this case, the following message is displayed: End of average lifetime is nearly reached, spare will be required.• Order new IR source with Bruker.• After receipt replace the used IR source (chapter 9.3).i As long as the lifetime is not expired, measuring is still possi-ble. To turn the OPUS status light greenagain, click the Ignore but-ton on the Instrument Status Mes-sage dialog (table 10.16 on page 213).Instrument test validity period is expired➣ In this case, the following message is displayed in the yellow information bubble (table 10.16 on page 213): An instru-ment test is required or one of the instrument components does not meet its specifications.☞ Click the OPUS status light.➣ The Instrument Status dialog opens. The measurement channel must read EXPIRED.Close the dialog and start a new instrument test:☞ On the wizard, click the Instru-ment Test button.Air humidity inside the spec-trometer is too high ➣ In this case, the following message is displayed: Humidity out of range.Replace desiccant (chapter 9.4).Table 10.7: Troubleshooting in case of problems indicated by the OPUS status light199 Optik GmbH ALPHA User ManualTroubleshooting 10Laser wavenumber must be recalibrated ➣ In this case, a respective message is displayed in a yellow information bub-ble (table 10.16 on page 213).In the information bubble, click the Calibrate button.Non of the possible causes applyContact Bruker Service.Spectrometer status indicator is redPerformance or instrument test failedDetails are described in chapter 10.5 et seq.Defective hardware compo-nentDetect the defective component:☞ Click the OPUS status light.➣ The Instrument Status dialog opens.i If the laser or the interferometer, electronics, automation or the detector is defective, contact Bruker Service. If the IR source is defective, replace the IR source (chapter 9.3).Non of the possible causes applyContact Bruker Service.Spectrometer status indicator is graySpectrometer not connected to PCConnect spectrometer to PC (see Installation Instructions).Wrong cable type used to connect spectrometer to PCOnly use the cross-over, Cat5-cable supplied.RJ45-plug(s) of the data cable not properly connected to PC and/or spectrometer.Check the data cable cord connec-tion at spectrometer and PC.Possible cause TroubleshootingTable 10.7: Troubleshooting in case of problems indicated by the OPUS status light200 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 10Not any or wrong spectrome-ter IP address specified in OPUS Specify correct spectrometer IP address in OPUS:☞ On the OPUS Validation menu, select the Optic Setup and Ser-vice command.➣ The Optic Setup and Service dialog opens.☞ In the Configuration drop-down list, select the ALPHA spec-trometer.☞ In the Optical Bench URL entry field, enter the spectrometer standard IP address (10.10. 0.1).The factory-set standard IP address of the spectrometer (10.10.0.1) has been changedReassign the standard IP address to the spectrometer:☞ Set the DIP-switch on the spec-trometer rear side. See Installa-tion Instructions.Reset spectrometer:☞ Press the SBY/RES key, located on the spectrometer rear side, more than 6 seconds.Spectrometer is in stand-by mode. ➣ The spectrometer status indicator flashes green.Deactivate stand-by mode:☞ Press the SBY/RES key, located on the spectrometer rear side.Possible cause TroubleshootingTable 10.7: Troubleshooting in case of problems indicated by the OPUS status light201 Optik GmbH ALPHA User ManualTroubleshooting 1010.2.3 Diagnostics LEDs on the spectrometerThe diagnostics LEDs are located on the rear spectrometer side.LED Definition1 TKD Green:➣ interferometer mirror is within the data acquisition rangeLight green:➣ data acquisition runsBlack:➣ no data acquisitionThe TKD abbreviation means Take Data.2 ACC Yellow:➣ the optics is accessed by the networkLight yellow:➣ data transfer runsThe ACC abbreviation means Access.3 DIR/ERR Slightly red flashing:➣ normal operation mode, scanner movesPermanent bright red:➣ interferometer problem, e.g. missing laser signal; no data acquisition possibleThe DIR abbreviation means Direction, ERR means Error.Table 10.8: Definition of diagnostics LEDs on spectrometerFigure 10.1: Diagnostics LEDs on spectrometer321202 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.2.3.1 Possible error causes and troubleshootingPossible cause TroubleshootingAll LEDs off Spectrometer not connected properly to mains supplyConnect spectrometer to mains sup-ply.No voltage applied Check whether the proper voltage is applied at the mains outlet.Short circuit in the mains adapter i A short circuit is accompanied by a "ticking" sound in the mains adapter.☞ Disconnect power supply imme-diately and contact Bruker Ser-vice.Yellow ACC LED does not lightSpectrometer not connected PCConnect spectrometer to PC.Wrong cable type used to connect spectrometer to PCOnly use the cross-over, Cat5-cable supplied.RJ45-plug(s) of the data cable not properly connected to PC and/or spectrometer.Check the data cable cord connec-tion at spectrometer and PC.Not any or wrong spectrome-ter IP address specified in OPUS Specify correct spectrometer IP address in OPUS:☞ On the OPUS Validation menu, select the Optic Setup and Ser-vice command.➣ The Optic Setup and Service dialog opens.☞ In the Configuration drop-down list, select the ALPHA spec-trometer.☞ In the Optical Bench URL entry field, enter the spectrometer standard IP address (10.10. 0.1).Table 10.9: Troubleshooting - LEDs on spectrometer rear side203 Optik GmbH ALPHA User ManualTroubleshooting 1010.3 Spectrometer status reportWith OPUS version 6 or higher, it is possible to save a complete report about the current spectrometer status. This report can be sent to Bruker service for remote fault diagnos-tics. Proceed as follows:1. Click the OPUS status light ( ).➣ The ’Instrument Status’ dialog opens.2. To send the report click the Send Report button. ➣ The report is sent by e-mail to opusreports@bruker.com.i This function requires an e-mail program installed on your PC and an e-mail account to be set up. In addition, your spectrometer needs to be connected to a network PC.Factory-set standard IP address of the spectrometer (10.10.0.1) has been changedReassign the standard IP address to the spectrometer:☞ Set the DIP-switch on the spec-trometer rear side. See Installa-tion Instructions.Reset spectrometer:☞ Press the SBY/RES key, located on the spectrometer rear side, more than 6 seconds.Spectrometer is in stand-by mode ➣ The spectrometer status indicator flashes green.Deactivate stand-by mode:☞ Press the SBY/RES key, located on the spectrometer rear side.DIR ERR LED is per-manently redSpectrometer problem caused by the laser and/or interferometerContact Bruker Service.Strong vibrations or other strong mechanical impacts on the spectrometer, which impair the spectrometer oper-ationPut the spectrometer on a vibration-free surface. If the problem still per-sists:☞ Contact Bruker Service.Possible cause TroubleshootingTable 10.9: Troubleshooting - LEDs on spectrometer rear side204 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.4 Instrument Status dialog in OPUSThe Instrument Status dialog in OPUS shows the status of each hardware component, and the status of the instrument test for the measurement channel currently used.1. Status of hardware components, e.g. IR source, laser etc. is displayed. The status can be as follows:Status DefinitionOK (green):component is okWarning (yellow):the exact meaning depends on the specific component; in case of the source a warning means:• source lifetime nearly reached (measuring is still possible)• source warms up (measuring not possible) Table 10.10: Hardware statusFigure 10.2: OPUS Instrument Status dialog21205 Optik GmbH ALPHA User ManualTroubleshooting 102. The second row of icons refers to the current measurement channel1 used, and indicates the result ofthe last instrument test performed. The results can be as fol-lows:Error (red):Component is defective (measuring not possi-ble)1. The measurement channel shown in table 10.11 is an example. The icon can vary and depends on the spectrometer type connected.Status DefinitionINACTIVE (yellow):the single tests of the particular test category are disabledPASSED (green): instrument test configured or passed, test is still validEXPIRED (light blue): instrument test validity period has expiredFAILED (red): last instrument test has failedTable 10.11: Status of measuring channelStatus DefinitionTable 10.10: Hardware status206 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.4.1 Diagnostics of hardware componentsTo perform a fault diagnostics for a particular hardware component proceed as follows:1. On the Instrument Status dialog, click the icon which indicates an error or warning.➣The Instrument Status Message dialog opens.2. Click the Service Info button.➣The firmware diagnostics page of the respective spectrometer hardware compo-nent opens. This page contains all relevant information about the current operat-ing state of the respective hardware component.i You can send the diagnostics pages of all hardware spectrometer components as full report to Bruker service for remote fault diagnostics (see chapter 10.1.1).207 Optik GmbH ALPHA User ManualTroubleshooting 1010.5 Diagnostics via instrument or performance testThe instrument or performance test checks whether the spectrometer achieves the per-formance specified. The difference of these two types of test procedures are as follows:Instrument test Performance testThe test procedure includes the fol-lowing single tests:• signal-to-noise test• deviation from 100% line• wavenumber accuracy test• signal-to-noise test• deviation from 100% lineNumber of test measurements:11 1Test duration: about 5 minutes about 1 minuteWhen is the test performed?• automatically when the PC and ALPHA communicate with each other for the very first time• automatically when you use a sampling module or an ATR crystal plate for the very first time• manually, i.e. you have to start the instrument test yourself after the defined instrument test validity period has expiredi The factory-set validity period is 7 days.• automatically after OPUS has been opened again• automatically after ALPHA has been accessed again• automatically after the sam-pling module or the ATR crystal plate has been sub-stituted by another sampling module or another ATR crystal plateTable 10.12: Instrument or performance test features208 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.5.1 Performance test does not start automatically10.5.2 Performance test failedThe performance test procedure includes the following tests:• Signal-to-noise test• 100% line testIf the performance test failed, an OVP - PQ Test Protocol (as pdf file) is displayed. The PDF files with the PQ test protocol are saved in the direc-tory.Possible cause TroubleshootingThe sampling module is not properly attached to the basic module.Attach the sampling module properly to the basic module (chapter 2.2).The ATR-crystal plate is not installed properly.Install the ATR-crystal plate properly (chapter 4.5).Table 10.13: Performance test does not start automaticallyFigure 10.3: Test protocol of a failed performance test209 Optik GmbH ALPHA User ManualTroubleshooting 1010.5.2.1 Possible causes and troubleshootingPossible cause TroubleshootingAs the performance test per-forms only one single measurement, this test may fail under certain circum-stances. This is not a spec-trometer problem or malfunction.In this case, we recommend to perform an instru-ment test which is going to be passed. • Click the OPUS status light.• On the dialog that opens, click the icon dis-played for the current measurement channel.• Wait until the test is completed (duration: about 5 minutes). If the problem still persists and the instrument test fails as well, see chapter 10.5.3.During the performance test, the spectrometer was exposed to strong vibrations.The spectrometer must not be exposed to strong vibrations. Perform an instrument test as follows:• Click the OPUS status light.• On the dialog that opens, click the icon dis-played for the current measurement channel.• Wait until the test is completed (duration: about 5 minutes). The spectrometer operates in too low an ambient tempera-ture, so that the IR source warm-up phase of 7 minutes is not sufficient.Wait until the IR source has reached its operating temperature. Then, perform an instrument test as follows:• Click the OPUS status light.• On the dialog that opens, click the icon dis-played for the current measurement channel.• Wait until the test is completed (duration: about 5 minutes). Transmission module: there is a sample or another object in the sample compartment.Remove the sample or object. Then, perform an instrument test as follows:• Click the OPUS status light.• On the dialog that opens, click the icon dis-played for the current measurement channel.• Wait until the test is completed (duration: about 5 minutes).ATR module: ATR crystal is dirty or there is a sample on the ATR crystal.Remove the sample or clean the ATR crystal (chapter 4.10). Then, perform an instrument test as follows:• Click the OPUS status light.• On the dialog that opens, click the icon dis-played for the current measurement channel.• Wait until the test is completed (duration: about 5 minutes).Table 10.14: Performance test failed210 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.5.3 Instrument test failedThe instrument test procedure includes the following tests:• Signal-to-noise test• 100% line test• Wavenumber accuracy testIf the performance test failed, an OVP - PQ Test Protocol (as pdf file) is displayed. The PDF files with the PQ test protocol are saved in the direc-tory.Figure 10.4: Test protocol of a failed instrument test211 Optik GmbH ALPHA User ManualTroubleshooting 1010.5.3.1 Possible causes and troubleshootingPossible cause TroubleshootingAll three tests failed Defective hardware compo-nentDetect the defective component:☞ Click the OPUS status light.➣ The Instrument Status dialog opens.i If the laser or the interferometer, electronics, automation or the detector is defective, contact Bruker Service. If the IR source is defective, replace the IR source (chapter 9.3).• All three tests failed• Only the S/N or 100% line test failedTransmission module: an object (e.g. sample) in the spectrometer sample com-partment obstructs the IR beamRemove the object and repeat the instrument test:• Click the OPUS status light.• On the dialog that opens, click the icon displayed for the current measurement channel.ATR module: ATR-crystal plate not installed properly Install the ATR-crystal plate prop-erly (chapter 4.5).Dirty ATR crystal, or sample material on crystalClean the crystal (chapter 4.10).Damaged ATR crystal • Order a new crystal plate with Bruker.• After receipt, replace the dam-aged crystal plate (chapter 4.5).Opaque KBr windows, which causes the infrared transpar-ency to be substantially reduced• Order new KBr windows with Bruker.• After receipt, replace the opaque windows (chapter 9.5).Non of the possible causes applyContact Bruker Service (chapter 1.6).Only the wavenumber accuracy test failedLaser wavenumber must be recalibrated• On the Validation menu, select the Setup Instrument Test command.• On the Setup OVP dialog, click the Measure LWN button.Table 10.15: Instrument test failed212 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 1010.6 Spectrometerproblem indicated by an error message in OPUSError messages which refer to the spectrometer can be displayed in OPUS as follows:i In case of a spectrometer problem indicated by an error message, the OPUS status light is yellow or red.Non of the possible causes applyContact Bruker Service (chapter 1.6).Possible cause TroubleshootingTable 10.15: Instrument test failedInstrument Status Message dialoga:a. The dialog opens if you have clicked a hardware component icon in the Instrument Status dialog (chapter 10.4).Yellow information bubbleb:b. The information bubble is displayed on the lower right end of the OPUS interface.Message window:Table 10.16: Display options in case of OPUS error messages213 Optik GmbH ALPHA User ManualTroubleshooting 1010.6.1 Troubleshooting in case of problems indicated by OPUS error messagesError message in OPUSPossible cause TroubleshootingAn instrument calibra-tion is required.Factory setting, displayed every 6 months in the form of a yellow information bubbleOn the information bubble, click the Calibrate button.i The purpose of a regular recalibra-tion is to ensure that the measure-ments performed are based on a correct laser wavenumber.Device not ready. IR source has not yet reached operating tempera-tureWait until the IR source is ready to operate.i The IR source warm-up takes about 7 minutes. As soon as the IR source has reached its operating tempera-ture the spectrometer status indica-tor becomes green.End of average life-time is nearly reached, spare part will be required.Specified lifetime of the IR source nearly reached • Order new IR source with Bruker.• After receipt replace the used IR source (chapter 9.5).i As long as the lifetime is not expired, measuring is still possible. To turn the OPUS status light green again, click the Ignore button on the Instru-ment Status Message dialog (table 10.16 on page 213)Front sample not con-nected.ATR crystal plate not or not properly installedInstall ATR crystal plate properly (chapter 4.5).Humidity out of range. Air humidity inside the spec-trometer is too highReplace desiccant (chapter 9.4).No accessory con-nected.Sampling module not prop-erly attached to basic moduleProperly attach the sampling module to the basic module (chapter 2.2).Source is broken. Defective IR source • Order new IR source with Bruker.• After receipt replace the defective IR source (chapter 9.3).Table 10.17: Error messages in OPUS214 ALPHA User Manual Bruker Optik GmbHBrukerTroubleshooting 10Source is not con-nected.Plug of the IR source not or not connected properly to the female connectorCheck whether the plug is connected properly (chapter 9.3).Standby mode acti-vated.Spectrometer is in stand-by mode➣ Spectrometer status indicator is green.Deactivate stand-by mode:☞ Press the SBY/RES key on the spectrometer rear side.Temperature out of range.Too high a temperature inside the spectrometer due to too high an ambient tem-peratureOperate the spectrometer only within the specified temperature range between 18 and 35°CWrong accessory inserted, unable to run OVP tests.Cannot run OVP tests, please check OVP Setup.The instrument test is started by the OPUS planer com-mand. But the type of sam-pling module defined in the OPUS planer is not identical to the one currently attached to the basic module.The sampling module defined in the OPUS planer must be identical to the one currently attached to the basic module.The instrument test is started via the OPUS Validation menu. But the test channel defined in OPUS is not identi-cal to the currently attached sampling module.Select the correct test channel:☞ On the Validation menu, select the Setup Instrument Test command.☞ In the dialog displayed, select the correct test channel.If an error message is displayed which is not listed above:Contact Bruker Service.Error message in OPUSPossible cause TroubleshootingTable 10.17: Error messages in OPUS215 Optik GmbH ALPHA User ManualTroubleshooting 1010.7 Checking communication between spectrometer and PC1. Switch on spectrometer.2. Wait about 1 minute to allow the spectrometer to boot. ➣ The spectrometer is ready to operate when the spectrometer status indicator is green.3. Start the internet browser.➣ The internet browser must not be off-line. In case of the Microsoft Internet Explorer the off-line mode is activated if the Offline Mode command on the File menu of the browser is checked.➣ Ensure that the internet browser does not use a proxy server, or at least not in case of addresses of direct access in the 10.10.x.x.-range. If you use the Micro-soft Internet Explorer, you can check this by selecting the Internet Options com-mand on the Extra browser menu. Click the Connections tab and click the Settings button in the LAN-Settings group field.4. Enter the spectrometer IP address into the browser address field as follows: http://10.10.0.1/diag.htm.5. Click the Enter button.➣ Now, the Internet Explorer should display the firmware diagnostics page for the ALPHA spectrometer (figure 10.5). If the Internet Explorer shows a blank page, this indicates that the PC cannot access the spectrometer. A wrong spectrometer IP address may be the cause of the problem.6. Close the Internet Explorer.Figure 10.5: Firmware diagnostics page for the ALPHA spectrometer216 ALPHA User Manual Bruker Optik GmbHBrukerA SpecificationsA.1 GeneralParameter SpecificationDimension Transmission module: 22 x 33 x 26 cm (w x d x h)ATR module: 22 x 31 x 14 cm (w x d x h)EMC regulations Complies with EN/IEC 61326/01.2006 (Electrical equip-ment for measurement, control and laboratory use - EMC requirements)Environmental conditionsaa. The values indicated are target values which have an effect on the performance of the entire configuration. In case of non-observance the functioning and safety of the configuration may be affected adversely.• Operational temperature range: 5 - 35°C• Temperature variation: max. 1°C/ per hour and max. 2°C per day• Humidity (non-condensing): less than 80% (relative humidity)• Installation site: in a closed room, max. 2000m above sea level• Pollution degree: 2, complies with 61010-1 or IEC 60664-1Overvoltage categorya II, complies with 61010-1 or IEC 60664-1Power consumption of spectrometerStandard configuration (with external power supply unit):Maximum: 48 WPower supply Standard configuration (with external power sup-ply):• AC Input: 100 - 240 V, 2,5 A; 50 - 60 Hz• DC Output: 24V DC ± 10%, 3,75 A• safety extra low voltage circuit (i.e. either double or reinforced isolated from primary supply circuits) with functional earthing at the negative terminal in the external power supplySafety regulations • Complies with EN/IEC 61010-1/08.2002 (Safety requirements for electrical equipment for measure-ment, control and laboratory use)• Complies with EN 60825-1/10.2003 (Safety require-ments for laser equipment)Weight 7 kgTable 11.1: Specifications - General217 Optik GmbH ALPHA User ManualSpecifications AA.2 PerformanceA.3 OpticsParameter SpecificationPhotometric accuracy 0.1% TResolution better than 2 cm-1; optionally better than 0.8 cm-1 Spectral range • 375 - 7,500 cm-1, with standard KBr beam splitter• 500 - 6,000 cm-1, with optional high-humidity ZnSe opticsWavenumber accuracy Better than 0.05 cm-1 @ 1,576 cm-1Wavenumber reproduci-bilityBetter than 0.01 cm-1Table 11.2: Specifications - PerformanceParameter SpecificationBeamsplitter • Standard: KBr• Optional: ZnSeDesign Sealed optics housing, convective desiccatingDetector High resolution DTGS detectorInterferometer Mechanical ROCKSOLID interferometer, permanently alignedScanner Mechanical frictionless bearing (no compressed air required)IR source Air-cooled, 12V, 20WTableunit ...................................................................................... 1296.3.8 Performing measurement ..................................................................................... 1306.3.9 Potential operating errors ..................................................................................... 1316.4 ALPHA sampling module with A128D/T option (heatable 7 cm gas cell)...... 1326.4.1 Specifications ....................................................................................................... 1336.4.2 Optical path .......................................................................................................... 1346.4.3 Software requirements in case of OPUS version11.3: Specifications - Optics218 ALPHA User Manual Bruker Optik GmbHBrukerSpecifications AA.4 ElectronicsA.5 ATR crystal typesParameter SpecificationA/D converter 100 kHz with 24 bit dynamic range Connectors EthernetLaser diode The spectrometer is a CLASS 1 LASER PRODUCT and contains a laser diode (850 nm).Table 11.4: Specifications - ElectronicsCrystal type To be used for Spectral range [cm-1]Refraction indexDiamond • all kinds of sam-ple material• hard and sharp-edged samples7500 - 350 n = 2.43Germanium (Ge) samples with a high absorptivity, especially carbon-filled samples (e.g. O-rings, polymer)5500 - 550 n = 4.01Zinc selenide (ZnSe)• all kinds of sam-ple material• exceptions: acids (pH -value 8) and sharp-edged samples>500 n = 2.43Table 11.5: Specifications - Crystal types219 Optik GmbH ALPHA User ManualSpecifications AA.6 Window materialSize Material Chemical propertiesStandard 25 x 4 mm Potassium bromide (KBr)Soluble in water, alcohol, and glycer-ineHygroscopic!➣ Avoid any contact to humidity.Option 25 x 4 mm Zinc selenide (ZnSe) Soluble in strong acids and HNO3Toxic!➣ Observe the safety data sheet.Table 11.6: ALPHA - Window materialNOTECAUTION220 ALPHA User Manual Bruker Optik GmbHBrukerB Spare PartsPart No. Description1005855 IR source with housing, pre-adjusted1011885 Desiccant bags1005847 2x replacement window (KBr), frame-mounted1006041 2x replacement window (ZnSe), frame-mountedTable B.1: Spare parts221 Optik GmbH ALPHA User ManualSpare Parts B222 ALPHA User Manual Bruker Optik GmbHBrukerC Firmware UpdateThe spectrometer firmware needs to be updated in order to make new features avail-able. The update is performed by using the FCONF program (Firmware Configuration Tool). This program performs all the necessary actions automatically.The FCONF program allows:• updating the firmware• restoring a previous firmware version• backing up the current firmware version• initializing the firmware (for service purposes only!)• running a custom script (for service purposes only!)Typically, firmware updates are delivered on CD or by e-mail. The delivered firmware update performs all the actions required to properly substitute the existing firmware ver-sion. i Before the firmware update, restoration or initialization starts, backup copies of the pre-vious firmware version are generated automatically, and stored in the Backup program folder.C.1 Firmware update on CD1. Start the FCONF program directly from CD.2. Double click the fconf.exe file.3. Proceed as described in chapter C.3.C.2 Firmware update via E-mail1. Store the delivered files into a temporary directory.2. Start the FCONF program by double-clicking the fconf.exe file3. Proceed as described in chapter C.3.The following dialog opens:223 Optik GmbH ALPHA User ManualFirmware Update CC.3 Performing firmware updateFigure E.1: Program FCONF - Firmware Update1 • Activate the Enter custom address option button.• Enter the IP address in dotted nota-tion.i In case of a stand-alone spectrome-ter configuration, the default IP address is 10.10.0.1. If the spec-trometer is directly integrated into a network, it must have a different IP address. In this case, use the IP address labeled on the spectrome-ter rear side. The operating com-pany is obliged to write the IP address on the label provided on the spectrometer rear side.2 • Check whether the spectrometer desired is recognized by the firmware.☞ Click the Beep button. If the spectrometer beeps three times in rapid suc-cession (once in case of ALPHA), it has been recognized by the firmware.• Click the Next button.Table C.1: Updating firmware224 ALPHA User Manual Bruker Optik GmbHBrukerFirmware Update C3 • Activate Update firmware option but-ton.• Click the Next button.4 i In case of firmware-versions = 1.3 the firmware type is selected automati-cally.• Click the Next button6 • Either accept the default directory setting or define a different path by clicking the Browse button.• Click the Next button.7Click the Finish button to start the update.i The update procedure may take sev-eral minutes, depending on the available bandwidth and the amount of files to be updated.Table C.1: Updating firmware225 Optik GmbH ALPHA User ManualFirmware Update CDuring firmware update• During firmware update, a log window is displayed showing all actions performed by the FCONF program. • The log-file is stored in the same directory as the backup files.• If an error occurs during the update procedure, the FCONF program terminates the procedure and recommends to restore the previous firmware version.After firmware update has finished• If the firmware update has finished, the FCONF program resets the spectrome-ter. The log window reads: Resetting the spectrometer... done.• After a successful spectrometer initialization, the firmware version is displayed in the log window.C.4 Restoring a previous firmware versionRestoring a previous firmware version is only possible if a firmware update has been performed first.1 • Activate the Restore previous firm-ware option button.• Click the Next button.Table C.2: Restoring previous firmware version226 ALPHA User Manual Bruker Optik GmbHBrukerFirmware Update CC.5 Backing up the current firmware version2 • Select the directory containing the backup information of the last firm-ware version (Previous run folder). By default, this directory is displayed automatically.i If you click the View Log button, a log window is displayed. The window contains detailed information about the last update including errors, warnings or other irregularities.• Click the Next button.3 Specify a directory for the backup files generated.i It is recommended to accept the directory set by the FCONF pro-gram.• Click the Next button.4 In the next dialog, click the Finish button.➣ The previous firmware version is going to be restored.Table C.2: Restoring previous firmware version1 • Activate the Backup current firmware option button.• Click the Next button.Table C.3: Backup current firmware version227 Optik GmbH ALPHA User ManualFirmware Update C2 • Specify a directory for the backup files generated.i It is recommended to accept the directory set by the FCONF pro-gram.• Click the Next button.3 In the next dialog, click the Finish button.➣ The backup starts.Table C.3: Backup current firmware version228 ALPHA User Manual Bruker Optik GmbHBrukerD GlossaryAperture The aperture wheel contains accurately etched holes to admit light into the spectrometer.ATR measuring ATR is the abbreviation of Attenuated Total Reflection and is also known as Internal Reflection Spectroscopy (IRS).Principle:• IR light is directed through an internal reflection element (ATR crystal) which requires a high refraction index.• Due to the internal reflection in the ATR crystal the IR light is repeatedly reflected on the crystal surface. The number of reflections depends on the refraction index as well as on the crystal length and thickness, as well as on the incidence angle of the IR light.• If a sample gets in contact with the crystal, it absorbs IR light at each reflection point of the crystal. Therefore, a good con-tact between sample and crystal has to be ensured.• The IR light absorbed by the sample is missing in the reflected beam. Thus, the reflected beam changes its inten-sity, which is recorded as absorption spectrum, depending on the wavenumber.The sample needs to have a lower refraction index than the crystal to achieve total internal reflection.Advantages of ATR measuringmethod:• Non-destructive analysis method, i.e. the sample has not to be destructed for analysis• No sample preparation required• Only a small number of sample quantity required• Suited for samples which are actually too thick or highly absorbing for transmission measurement• Due to the multiple reflection of the IR light, the sample absorbs more light than in case of transmission measure-mentDisadvantages of ATR measuring method:• Falsified measurement result due to possible contaminations caused by previous sample material, solvents or fingerprints.• In case of multi-layer materials only the first layer will be spectroscopically analyzed.• The quality of the measurement result substantially depends on the contact pressure between sample and ATR crystal during measurement.229 Optik GmbH ALPHA User ManualGlossary DATR spectra In case of ATR spectra the intensities of the spectral features are of lower absorbance than the corresponding features in a transmission spectrum, especially, in the high wavenumber (short wavelength) region of the spectrum.The intensity is related to the penetration depth of the evanes-cent wave into the sample. This depth depends on the refrac-tive index of the crystal and sample, and on the wavelength of the IR radiation. The relatively thin depth of penetration of the IR beam into the sample creates the main benefit of ATR sam-pling. This is in contrast to traditional FT-IR sampling by trans-mission where the sample must be diluted with IR transparent salt, pressed into a pellet or pressed to a thin film, prior to anal-ysis to prevent totally absorbing IR bands.Beamsplitter The beamsplitter splits the incident beam into two separate ligth waves. Generally, the beamslitter is a half-mirrored sub-strate that reflects and transmits approximately equal portions of the incident radiation.Calibration Calibration comprises the entirety of working steps to define the relation between analyte concentrations and the corre-sponding standard measurement values. Under specified con-ditions the analyte concentrations are indicated by an instrument, measuring system, or values which have been evaluated when measuring substances or reference material.Collimated light Light for which all flux lines are parallel.Cross-over cable The cross-over cable includes a RJ45 plug on each cable end. In one plug, however, the pairs leading the signal are swapped (crossed). That means, one plug swaps the transmission data with the received data to enable data exchange when one ter-minal device is directly connected to another. If the transmis-sion and received data were not swapped at one cable end, a connection could not be accomplished.Detector A detector converts incoming light into an electrical signal.Diffuse reflection In case of diffuse reflection the light scatters evenly at all angles, from one particular point of reflection. Diffuse reflection techniques are used to analyze rough-surfaced solid samples.DRIFTS Diffuse reflectance infrared fourier transform spectroscopy is an analyzing technique where infrared light hits on a rough or mat surface. The infrared light penetrates the sample surface, and part of the light is reflected over all angles (diffusely reflected) due to the rough sample surface.230 ALPHA User Manual Bruker Optik GmbHBrukerGlossary DEthernet Ethernet is the most widely installed Local Area Network (LAN). A LAN is a network of interconnected workstations sharing the resources of a single processor or server within a relatively small geographic area (i.e. an office building). Ethernet is a set of hardware and signaling standards used for LANs. The most commonly installed systems are 10/100/1000 BaseT.FIR Far InfraRed; covers the spectral range from 400 to about 5cm-1 wave numbers. It is about vibrational frequencies of both backbone vibrations of large molecules, as well as funda-mental vibrations of molecules that include heavy atoms (e.g. inorganic or organometallic compounds) and pure rotational vibrations.Fourier Transform Fourier Transform (FR) spectroscopy is a mathematical trans-formation method used to convert an interferogram into an infrared spectrum. Essentially, Fourier Transform decomposes or separates a waveform or function into sinusoids of different frequencies. All these different frequencies together sum to the original waveform. Fourier Transform identifies or distinguishes the dif-ferent frequency sinusoids and their respective amplitudes.Frequency Frequency is the number of occurrences of a repeating event per unit time. In equations, frequency is denoted by the Greek letter . The following equation applies to the frequency of a wave : , with c being the phase velocity of the wave in the respective medium, and (lambda) being the wave-length. The wavelength is no timely but local parameter.Any kind of time-restricted vibration process, even in the form of a sinusoid, always represents an overlapping of several fre-quencies.FT-IR The Fourier Transform InfraRed Spectroscopy is a method to obtain infrared spectra of a sample using an interferometer. A Fourier transform is performed on the resulting interferogram to calculate the spectrum.In case of an FT-IR spectrometer infrared light emitted from a source is directed to an interferometer which modulates the light. Leaving the interferometer the light passes through the sample compartment (and also the sample) and is focused onto the detector. The signal measured by the detector is called the interferogram.  c---=231 Optik GmbH ALPHA User ManualGlossary DFuse Fuses and circuit protectors protect electrical devices and components from overcurrents and short circuits. This is achieved automatically by the melting of an internal melting element through which a fault current flows. Both components are rated so as to reliably interrupt current flow when it reaches a predictable magnitude for a fixed time period. For all practical purposes, a fuse or protector is invisible to a properly operating circuit.A fuse switches or blows when a high short-circuit or fault cur-rent causes an irreversible, physical separation of the melting element. As the weakest element in a circuit, the fuse/protec-tor resistivity increases, eventually causing the melting point of the melting element to be reached. The element then changes state from a solid to a liquid (or even gas) within a defined time period.Gateway address A gateway is a kind of connecting point between different net-works, which controls data traffic of the respective network. A gateway address is the address of a particular gateway within a network.Instrument test The instrument test checks whether the spectrometer achieves the specified performance. The instrument test con-tains the following single tests: signal-to-noise, deviation from 100% line and wavenumber accuracy. The instrument test is performed when:• a communication connection between spectrometer and computer has been established• the sampling module or ATR crystal plate has been exchanged• the test validity period has been expired (manual start required)The instrument test lasts about 5 minutes. Exactly 11 mea-surements are performed during the instrument test, which has a validity period of 7 days (factory-set).232 ALPHA User Manual Bruker Optik GmbHBrukerGlossary DInterferogram The interferogram is a plot of detector signal as a function of optical path length difference. Spectrometers are equipped with a broadband light source, which yields a continuous infi-nite number of wavelengths. The interferogram is the continu-ous sum, i.e. the integral of all the interference patterns produced by each wavelength. This results in the intensity curve as function of the optical retardation. At the zero path difference of the interferometer ( x=0) all wavelengths undergo constructive interference andsum to a maximum signal. As the optical retardation increases different wavelengths undergo constructive and destructive interfer-ence at different points, and the intensity therefore changes with retardation. For a broadband source, however, all the interference patterns will never be simultaneously in phase except at the point of zero path difference, and the maximum signal occurs only at this point. This maximum in the signal is referred to as the centerburst. Dispersive elements detected in the optical path can cause chirping in the centerburst.Interferometer An interferometer detects interferences, that means overlap-pings of light waves. Inside the interferometer a light beam is splitted into two light waves (beams) by the beam splitter. These two light waves pass through optical paths of different lengths, are reflected by additional mirros, and finally recom-bined.If you change the optical path of one of the two light waves, e.g. by moving one mirror, the phases of the two light waves displace against each other. When recombining the light waves, interferences occur.The result is an interference pattern (stripes or rings) which has been written by the light waves. This pattern is determined by the difference of the optical path lengths which the single light waves have passed before being recombined.IP address An IP address is the network address of a workstation or net-work. IP addresses consist of 4 number fields separated by dots. Each number field represents 1 byte. Values can be between 0 and 255. The numbers on the left of the string define the network, the numbers on the right define the individ-ual workstation or Network Interface Card (NIC).IR source In the mid and near infrared an IR source is used which emits infrared light.KBr pellet The pellet is prepared by grinding the sample, diluting it in KBr and pressing it into a transparent disc. The KBr pellet is directly placed into the infrared beam for analysis.233 Optik GmbH ALPHA User ManualGlossary DLaser The laser is a coherent source of monochromatic radiation. It is an essential part of the interferometer system. Due to laser light interference the position of the movable mirror, and the data sampling positions are determined.Micrometer (µm) Micrometer is a length unit of 10-6 meter, which is equal to a thousandth of a millimeter.Optical path The optical path is the distance of the light passing through the spectrometer. The distance between two points in the light beam is calculated in longitudinal direction, and multiplied by the refraction index of the medium.OQ test The OQ (Operational Qualification) is a test category used to validate the spectrometer. This test checks the current instru-ment performance and compares it to the one specified. The OQ test consists of several single tests and is performed within a defined time interval.Generally, the OQ test protocol runs during final testing before an instrument is delivered to the customer, after each major repair, exchange of optical components which may influence the instrument performance, and on a regular yearly or semi-yearly basis after maintenance.Performance test The performance test checks whether the spectrometer achieves the specified performance. The performance test contains the following single tests: signal-to-noise and devia-tion from 100% line. In case of the ALPHA spectrometer the performance test starts when:• the OPUS spectroscopy software has been started• the sampling module has been exchanged• the ATR crystal plate has been exchangedThe performance test lasts about 1 minute. Exactly 1 mea-surement is performed during the performance test.PQ test The PQ (Performance Qualification) is a test category used to validate the spectrometer. The test evaluates the performance and proper function of the spectrometer. The PQ test consists of several single tests and is performed within a defined time interval. Generally, the test is intended to be performed once a day.Reflectance Reflectance describes the ratio of the radiation energy reflected from a surface to the radiation energy incident on the surface. It is the percentage or part of the incident light (= 100%), which an object reflects again.Reflection In case of reflection light incidents on a sample and is con-verted to radiation energy. This kind of energy is subsequently reflected by the sample surface at a defined wavelength.234 ALPHA User Manual Bruker Optik GmbHBrukerGlossary DRelative humidity Relative humidity is the amount of water vapor in the air, which can be between 0 and 100%.Resolution Resolution in FT-IR is determined by the maximum optical path difference reached in the measurement of an interfero-gram. The spectral resolution corresponds to the minimum possible spectral distance between 2 adjacent spectral lines which can be resolved by the spectrometer. It is produced by the instrumental spectral line shape and the line width of the sample’s absorption.The instrumental line shape is reciprocally related to the travel distance of the movable mirror in the interferometer, and also influenced by the apodization function and divergence in the interferometer. The higher the spectral resolution (smaller val-ues), the higher the noise in the spectrum.Sample A sample is a special kind of substance which is put into the spectrometer sample position, and measured.Signal-to-noise ratioThe signal-to-noise ratio describes the quality of a wanted sig-nal which has been superimposed by noise. It outlines the ratio between the average performance of a wanted signal emitted by a signal source, and the average performance of noise.Spectrometer Spectrometer derives from the Latin word specere meaning image, and the Greek word metron meaning to measure. A spectrometer uses some sort of mechanical or electrical detec-tion device to obtain the infrared spectrum of a sample. It con-tains a source of infrared radiation, a sample compartment to allow the radiation to interact with a sample, a detector for radi-ation, and units to determine and display the intensity of radia-tion.Spectrum A spectrum is an image of radiation energy dispersed into its wavelength constituents or a two-dimensional plot of radiation energy, or radiation energy ratio versus wavelength. It includes a set of absorption, reflection or transmission values which have been measured by an IR spectrometer based on defined wavelengths. The features in an infrared spectrum correlate with the pres-ence of functional groups of molecules of a sample.Subnet mask The subnet mask is a network mask used to partition network addresses for efficiency and security. Subnet masks work by ’masking’ less significant address bits on all workstations in the sub-network.235 Optik GmbH ALPHA User ManualGlossary DTransmission Transmission describes the portion of transmitted infrared light. One part of the incidented light directly passes through the sample without any interactions with electrons or mole-cules in the sample. Another part of light is absorbed and con-tinuously re-emitted to the same direction from which the incident light comes.Transmission measurementIn IR spectroscopy, transmission is the classical analysis method for samples. Depending on the sample material, sam-ple preparation can be very complex in case of transmission measurement.Principle:• IR light transmits a sample. The sample absorbs specific wavelengths of the IR light. This kind of absorption of certain wavelengths enables to identify the sample.• If samples are evaluated for quantitative analysis, the inten-sity ratio of the IR light before and after passing the sample is measured within a specific wavelength. Advantages:• Almost all kinds of samples can be analyzed.• Measurement represents the entire sample.Disadvantages:• Depending on the sample material a complex and some-timesdifficult sample preparation is required. A successful transmission measurement substantially depends on how carefully the sample has been prepared.• Depending on the sample preparation method required, measuring in transmission may sometimes destroy the sam-ple.• Too much a sample quantity can cause total absorption.• Additional accessories (e.g. liquid and gas cells) are required.Transmittance Transmittance is the ratio between the beam energy transmit-ted through a sample and the beam energy incident on the surface of the sample.USB The Universal Serial Bus (USB) is a serial bus system which allows to connect peripherals to a host computer. Devices or storage media equipped with USB can be hot plugged, and the properties of peripherals can be automatically detected.236 ALPHA User Manual Bruker Optik GmbHBrukerGlossary DValidation In general, validation evidently documents that, by the use of specific laboratory investigation methods, a process or system (spectrometer) meets the previously defined requirements (acceptance criteria) in reproducible manner and for its intended analytical use.During spectroscopic validation the x-axis (frequency) and y-axis (transmission, reflection) are verified by transmission or reflectance standards which may be included in the internal spectrometer validation unit. Validation can be performed at individual time intervals by the application software.Wavelength The wavelength is the distance between two maxima on a sinusoidal wave, i.e. the distance traversed by one period of an electromagnetic wave. The wavelength depends on the refractive index of the medium which the electromagnetic wave travels through.Wavenumber The wavenumber is the reciprocal of the wavelength . The wavenumber is defined as with the unit of cm-1, that means the number of waves per each centimeter.̃ ̃ 10-----=237 Optik GmbH ALPHA User ManualGlossary D238 ALPHA User Manual Bruker Optik GmbHBruker OptikIndexAA241/D ......................................................88A241/DV ...................................................88AccessoryWrong a. inserted ...................................215ALPHAP- Anvil tip ...............................................49ALPHA (A128D/T) ........................... 26, 132Gas cell ................................................132Gas cell hardware ..................................133Gas line ................................................135Maximum gas flow rate ...........................133Measurement ........................................136Optical path ...........................................134Path length ............................................133Pressure range ......................................133Replacing windows ....................... 138, 139Sealing ring ...........................................133Temperature range ................................133Volume .................................................133Window material ....................................133ALPHA-E ........................................... 24, 45Anvil .......................................................47Crystal type ...................................... 47, 71Optical path .............................................48Pressure applicator ..................................58Sampling surface .............................. 47, 71ALPHA-G (A128D/T)After replacing windows ..........................142Cleaning windows ..................................142ALPHA-G (A139/D) .......................... 26, 118Gas cell hardware ..................................119Maximum gas flow rate ...........................119Mirror ....................................................119Path length ............................................119Pressure range ......................................119Temperature range ................................119Volume .................................................119Window material ....................................119ALPHA-G (A139-H1) ....................... 26, 125Heating jacket ....................... 125, 126, 127Mounting heating jacket ..........................127Temperature control unit .........................126ALPHA-P ........................................... 24, 45Anvil .......................................................50Crystal type ...................................... 49, 50Heatable .......................................... 52, 54Optical path .............................................50Pressure applicator ..................................59Pressure arm ...........................................49Sampling surface .............................. 49, 50ALPHA-R ................................................. 25ALPHA-R (A240/DU) ................. 25, 78, 109Measuring ............................................ 113Optical path .......................................... 111Positioning sample ................................ 115Reference mirror ................................... 113Sampling holder .................................... 110Sampling spot ....................................... 110Specifications ........................................ 109Spectral range ...................................... 110ALPHA-R (A241/D) ............................ 25, 77Optical path ............................................ 90Sampling spot ................................. 89, 104Specifications .................................. 89, 104Spectral range ................................ 89, 104ALPHA-R (A241/DL) ........................ 77, 103Measurement experiment ....................... 106Measuring ............................................ 106Optical path .......................................... 105ALPHA-R (A241/DV) ....................25, 78, 93Camera software ...................94, 95, 96, 97Installing video converter .......................... 93Optical path ............................................ 91Sampling spot ................................. 89, 104Specifications .......................................... 89Spectral range ................................ 89, 104ALPHA-R (A528/D) ............................ 77, 78Auxiliary device ....................................... 82Checking signal intensity .......................... 84Filling sample cup .................................... 82Measurement experiment ......................... 86Measuring .............................................. 84Optical path ............................................ 80Reference mirror ..................................... 81Sampling spot ......................................... 79Specifications .......................................... 79Spectral range ........................................ 79Starting background measurement ............ 86Starting sample measurement .................. 86Tool kit ................................................... 81ALPHA-R A241/DLStarting background measurement .......... 107Starting sample measurement ................ 107ALPHA-T ...................................... 23, 29, 30Displacing sample holder ......................... 38Foil holder .............................................. 36Inserting gas cell ..................................... 39Measuring accessories ............................ 34Opening sample compartment .................. 32Optical path ............................................ 31239 GmbH ALPHA User ManualIndexReflection accessory ......................... 40, 42Spectral range ........................................ 30Spectral resolution ................................... 30Aperture ................................................. 229Applications .............................................. 27Atmospheric compensation ............ 147, 148Performing ............................................ 149ATR crystalPositioning sample ..................................62ATR crystal plate ...................................... 56Replacing ............................................... 57ATR measurement ............................. 45, 65ATR sampling moduleCleaning ................................................. 69ATR spectra ........................................... 230BBackground measurement ..................... 146Baseline correction ................................ 147Performing ............................................ 148Basic module ..................................... 15, 16Connection ports ..................................... 17Beamsplitter ..................................... 16, 230CCalibration .............................................. 230Camera softwareFunctions ............................................... 94Installing ................................................. 96Installing driver ........................................ 95Starting .................................................. 97CFG ......................................................... 18Cleaning ................................................. 189Cleanness test ......................................... 61Collimated light ...................................... 230Compound information ........................... 165Connection port ........................................ 17Connector .............................................. 219Cross-over cable .................................... 230CrystalMaterial ................................................ 219Refraction index .................................... 219DDesiccant bagsReplacing ............................................. 184Design ...................................................... 27Detector ................................... 16, 218, 230DiagnosticsHardware component .................... 205, 207In OPUS ............................................... 205Instrument test ...................................... 208LED ..................................................... 202Performance test ................................... 208Diagnostics LEDs ...................................202Diffuse reflection .............................. 77, 230Dimension ...............................................217DRIFTS ...................................................230DTGS ........................................................16EElectronics ....................................... 28, 219Environmental conditions ........................217Error message ............................... 213, 214Ethernet ..................................................231Experiment file ........................................145FFault diagnostics .....................................191Remote .................................................192FIR ..........................................................231FirmwareBacking up version .................................227Restoring version ...................................226Update ..................................................223Flow-through cell ............................... 55, 63Cleaning .................................................70De-installing ............................................56Installing .................................................55Fourier transform ....................................231Frequency ...............................................231FT-IR spectroscopy ................................231Full report ................................................192Generating ................................... 192, 193Fuse ........................................................232GGas analysis ...........................................117Pressure range ............................. 119, 133Temperature range ....................... 119, 133Gateway address ....................................232HHardware componentDiagnostics ...........................................191Error .....................................................205OK .......................................................205Warning ................................................205Hardware component diagnostics ..........207Heating jacket .........................................125Danger ..................................................129Functionality ..........................................127Mounting ...............................................127Safety ...................................................129Hit spectrum ............................................165Humidity ......................................... 196, 217Too high ................................................214240 ALPHA User Manual Bruker Optik GmbHBrukerIndexIIEC/EN ......................................................10Installation site ........................................217Instrument status dialog ..........................205Instrument test ....................... 144, 208, 232Disabled ................................................206Expired ........................................ 196, 206Failed .......................................... 206, 211Passed .................................................206Problems ...................................... 211, 212Protocol ................................................211Test duration .........................................208Validity ..................................................208Intended use .............................................13Interferogram ..........................................233Interferometer .................... 16, 27, 218, 233IP address ...............................................233Defining ................................................201IR source ................................. 16, 218, 221Lifetime .................................................195Not ready ..............................................195Replacing ..................................... 180, 183Warm-up ...............................................195KKBr pellet ................................................233Kensington lock ........................................19LLaser .......................................................234Laser diode .............................................219Laser wavenumberCalibrate ...............................................196LEDACC .............................................. 17, 202ACC is yellow ........................................203All off ....................................................203DIR ERR is red ......................................204DIR/ERR ........................................ 18, 202TKD ............................................... 17, 202Liquid sampleMeasuring ...............................................68MMaterial identification ..............................159Material verification .................................159Measurement experiment .......................145Measurement parameters .......................145Editing ..................................................145Micrometer ..............................................234OOperational temperature .........................217Optical path ............................................234Optics ...............................................27, 218OPUS ...............................................28, 143OQ test ...................................................234Overvoltage category .............................217OVP ........................................................179PPeak picking ...........................................151Interactive .............................................153Performing ............................................151Report ..................................................154Single peak ...........................................154Performance ...........................................218Performance test ................... 144, 208, 234Failed ...................................................209Problems ......................................209, 210Protocol ................................................209Test duration .........................................208Photometric accuracy .............................218Pollution degree ......................................217PortETH/LAN ................................................17Ext. Accessory .........................................18Power .....................................................18SBY/RES ................................................18TAP ........................................................18USB .......................................................17Positioning sampleALPHA-P ................................................64ALPHA-P heatable ...................................63In case of flow-through cell ........................63Power consumption ................................217Power supply ..........................................217PQ test ....................................................234Pressure applicator ...................................59Adjusting height .......................................61Working with ............................................58Protective earthing ....................................13QQualified personnel ...................................13Quantitative analysis ..............................167Calibration samples ................................167Calibration straight line ...................169, 171Concentration value .......................169, 171Integration area .....................................171Method .................................................168Performing ............................................172Report ..................................................173Sigma ...................................................173Query spectrum ......................................165Quick compare .......................................155Method .................................................156Performing ............................................158241 Optik GmbH ALPHA User ManualIndexQuery spectrum .................................... 161Report .................................................. 162Result .................................................. 159Result view ........................................... 159RReflectance ............................................ 234Reflection ............................................... 234Spectrometer configuration ....................... 77Relative humidity .................................... 235Remote fault diagnostics ........................ 192Replacement window ............................. 221Reset ........................................................ 18Resolution ...................................... 218, 235SSafety ....................................................... 10Sample ................................................... 235Sample preparation ................................ 175Condition of sample ............................... 175Methods ............................................... 176Solvents ............................................... 175Sampling module ..................................... 15Exchanging ............................................ 21Scanner .................................................. 218Signal-to-noise ....................................... 235SoftwareStarting ................................................ 144Source .................................................... 233Spectra library ........................................ 163Spectral range ........................................ 218Spectrometer ......................................... 235Housing ................................................. 27Status .................................................. 193Switching on ......................................... 143Spectrometer configuration ...................... 23ATR ....................................................... 24Design ................................................... 27Gas analysis ........................................... 26Reflection ............................................... 25Transmission .......................................... 23Spectroscopy software ............................. 28Spectrum ................................................ 235Manipulating ......................................... 147Spectrum searchPerforming ............................................ 163Report .................................................. 166Specular reflection ................................... 77Stand-by mode ................................... 18, 19Activating ............................................... 19Deactivating ............................................ 20Status indicatorColor definition ...................................... 193On spectrometer ................................... 194Problems .............................................. 195Status lightOPUS ...................................................198Problems ...............................................199Status report .................................. 192, 204Structural formula ...................................165Subnet mask ...........................................235TTemperatureOut of range ..........................................215Specified ...............................................196Variation ...............................................217Temperature control unit .........................129Transmission ..........................................236Spectrometer configuration .......................29Transmission measurement ...... 33, 43, 236Transmittance .........................................236UUSB ........................................................236VValidation ................................................237WWarning labels ..........................................11Waste disposal .........................................12Wavelength .............................................237Wavenumber ..........................................237Accuracy ...............................................218Reproducibility .......................................218Weight .....................................................217WindowChemical properties ...............................220Cleaning ...............................................189Material .......................... 16, 138, 185, 220Replacing ............................. 185, 186, 188Replacing interval ..................................186242 ALPHA User Manual Bruker Optik GmbHALPHALegal ClauseTable of Contents1 Introduction1.1 About this manual1.2 Terms1.3 Gender-neutral form1.4 Safety1.4.1 Warning labels1.4.2 Waste disposal1.5 General information1.5.1 Protective earthing1.5.2 Qualified personnel1.5.3 Intended use1.6 Questions and concerns2 ALPHA spectrometer2.1 Basic module2.1.1 Connection ports and LEDs2.1.2 Stand-by mode2.2 Exchanging sampling module2.2.1 Procedure2.2.2 After exchanging the sampling module2.3 Spectrometer configuration2.3.1 ALPHA for transmission measurements2.3.2 ALPHA for ATR measurements2.3.3 ALPHA for reflection measurements2.3.4 ALPHA for gas analysis2.4 Design2.5 Applications2.6 Spectrometer housing2.7 Optics2.8 Electronics2.9 Spectroscopy software3 ALPHA for transmission measurement3.1 Overview on ALPHA spectrometer configurations for transmission3.2 ALPHA-T universal sampling module3.2.1 Specifications3.2.2 Optical path3.2.3 Opening sample compartment3.2.4 Starting measurement3.2.5 Potential operating errors3.3 Measuring accessories3.3.1 Sample holder (standard)3.3.2 Foil holder (option)3.3.3 Liquid cell (option)3.3.4 Gas cell (option)3.4 ALPHA-T 30° reflection accessory3.4.1 Specifications3.4.2 Displacing mounted sample holder3.4.3 Inserting 30°reflection accessory into the sample compartment3.4.4 Performing measurement4 ALPHA for ATR measurement4.1 Overview on ALPHA spectrometer configurations for ATR4.2 ALPHA-E sampling module4.2.1 Optical path4.3 ALPHA-P sampling module4.3.1 Optical path4.3.2 High-pressure variant4.3.3 With heatable ATR unit4.4 Crystal material4.5 Replacing ATR crystal plate4.5.1 Procedure4.6 Working with pressure applicator4.6.1 With the ALPHA-E sampling module4.6.2 With the ALPHA-P sampling module4.7 Cleanness test4.8 Positioning sample on the ATR crystal4.8.1 Procedure in case of ALPHA-E and ALPHA-P (non-heatable)4.8.2 Procedure in case of ALPHA-P (heatable)4.9 Performing measurement4.9.1 Performing non-temperature controlled measurement4.9.2 Performing temperature-controlled measurement (only with heatable ALPHA-P)4.10 Cleaning ATR sampling module4.10.1 Cleaning solvents4.10.2 Procedure4.11 Cleaning flow-through cell4.12 ALPHA ATR multi reflection sampling module (A213/D-11)4.12.1 Optical path4.12.2 Usable sample material4.12.3 Performing measurement4.12.4 Potential operating errors4.12.5 Measuring accessory4.12.6 Cleaning crystal plate4.12.7 Replacing crystal plate5 ALPHA for reflection measurement5.1 Overview on ALPHA spectrometer configurations for reflection5.2 ALPHA-R sampling module (A528/D)5.2.1 Specifications5.2.2 Optical path5.2.3 Software requirements in case of OPUS version > /ColorImageDict > /JPEG2000ColorACSImageDict > /JPEG2000ColorImageDict > /AntiAliasGrayImages false /CropGrayImages true /GrayImageMinResolution 300 /GrayImageMinResolutionPolicy /OK /DownsampleGrayImagestrue /GrayImageDownsampleType /Bicubic /GrayImageResolution 300 /GrayImageDepth -1 /GrayImageMinDownsampleDepth 2 /GrayImageDownsampleThreshold 1.50000 /EncodeGrayImages true /GrayImageFilter /DCTEncode /AutoFilterGrayImages true /GrayImageAutoFilterStrategy /JPEG /GrayACSImageDict > /GrayImageDict > /JPEG2000GrayACSImageDict > /JPEG2000GrayImageDict > /AntiAliasMonoImages false /CropMonoImages true /MonoImageMinResolution 1200 /MonoImageMinResolutionPolicy /OK /DownsampleMonoImages true /MonoImageDownsampleType /Bicubic /MonoImageResolution 1200 /MonoImageDepth -1 /MonoImageDownsampleThreshold 1.50000 /EncodeMonoImages true /MonoImageFilter /CCITTFaxEncode /MonoImageDict > /AllowPSXObjects false /CheckCompliance [ /None ] /PDFX1aCheck false /PDFX3Check false /PDFXCompliantPDFOnly false /PDFXNoTrimBoxError true /PDFXTrimBoxToMediaBoxOffset [ 0.00000 0.00000 0.00000 0.00000 ] /PDFXSetBleedBoxToMediaBox true /PDFXBleedBoxToTrimBoxOffset [ 0.00000 0.00000 0.00000 0.00000 ] /PDFXOutputIntentProfile () /PDFXOutputConditionIdentifier () /PDFXOutputCondition () /PDFXRegistryName () /PDFXTrapped /False /CreateJDFFile false /Description /BGR /CHS /CHT /CZE /DAN /DEU /ESP /ETI/FRA /GRE /HEB /HRV (Za stvaranje Adobe PDF dokumenata najpogodnijih za visokokvalitetni ispis prije tiskanja koristite ove postavke. Stvoreni PDF dokumenti mogu se otvoriti Acrobat i Adobe Reader 5.0 i kasnijim verzijama.) /HUN /ITA /JPN /KOR /LTH /LVI/NLD (Gebruik deze instellingen om Adobe PDF-documenten te maken die zijn geoptimaliseerd voor prepress-afdrukken van hoge kwaliteit. De gemaakte PDF-documenten kunnen worden geopend met Acrobat en Adobe Reader 5.0 en hoger.) /NOR /POL /PTB /RUM /RUS /SKY /SLV /SUO /SVE /TUR20910.5.3 Instrument test failed ............................................................................................ 21110.6 Spectrometer problem indicated by an error message in OPUS................... 21310.6.1 Troubleshooting in case of problems indicated by OPUS error messages .......... 21410.7 Checking communication between spectrometer and PC ............................. 216A Specifications ............................................................................................217A.1 General ................................................................................................................ 217A.2 Performance........................................................................................................ 218A.3 Optics .................................................................................................................. 218A.4 Electronics .......................................................................................................... 219A.5 ATR crystal types ............................................................................................... 219A.6 Window material ................................................................................................. 220B Spare Parts.................................................................................................221C Firmware Update .......................................................................................223C.1 Firmware update on CD ..................................................................................... 223C.2 Firmware update via E-mail ............................................................................... 223C.3 Performing firmware update.............................................................................. 224C.4 Restoring a previous firmware version ............................................................ 226C.5 Backing up the current firmware version......................................................... 227D Glossary .....................................................................................................229Index ...........................................................................................................2398 ALPHA User Manual Bruker Optik GmbHBruker1 Introduction1.1 About this manualThis manual is a complete documentation about the ALPHA spectrometer.Depending on the degree of hazard important safety information and safety instructions are classified as follows:i The i provides information given to the user to facilitate spectrometer operation, and make the best possible use of the spectrometer.1.2 TermsThis manual uses both the term spectrometer or ALPHA when the spectrometer is described.1.3 Gender-neutral formThe manual uses the male form in a neutral sense and does not differentiate between male and female users. We would kindly ask all female users to have understanding for this simplified form.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.9 Optik GmbH ALPHA User ManualIntroduction 11.4 SafetyAlways observe the instructions described in this manual to ensure user safety and to avoid property damage. Keep this manual for further reference available at any time. Improper use or failure to follow the safety instructions can result in serious injuries and/or property damage. Any non-observance infringes the intended use (i.e. spectroscopic measurements) of the spectrometer. In this case Bruker Optik GmbH does 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 condition and fully functioning. A safe and faultless operation can only be guar-anteed if the spectrometer is transported, stored, installed, operated and maintained properly according to the procedures and instructions described in this manual.Never remove or deactivate any supporting safety systems during spectrometer opera-tion. Objects and/or material not required for operation must not be kept near the spec-trometer operating area.The spectrometer has been developed according to the EN 61010-1:2010 (IEC 61010-1:2010+Cor.:2011) safety regulations for electrical measuring, control and laboratory devices.10 ALPHA User Manual Bruker Optik GmbHBrukerIntroduction 11.4.1 Warning labelsWhen operating the spectrometer you have to observe a number of safety instructions which are highlighted by the appropriate warning label. The warning labels and their meaning are described in the following. All warning labels on the spectrometer must always be kept legible. Immediately replace worn or damaged labels.Label DefinitionGeneral Hazard:This warning symbol indicates general hazard. Observe the safety instructions and follow the precautions described to avoid personal injury.Hot Surface:This warning symbol refers to 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 operat-ing near hot components and/or surfaces.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 look into the beam as this may cause permanent eye damage.Table 1.1: Warning labels11 Optik GmbH ALPHA User ManualIntroduction 11.4.1.1 In case of hazardous sample materialBesides the dangers described above, there can also be hazards caused by the sample material. Depending on the type of hazardous substances used, you have to observe the specific substance-relevant safety instructions. Put on the specific warning label on the corresponding module position. The label must be legible and permanently discern-ible. The following list exemplifies types of hazardous sample material:1.4.2 Waste disposalDispose all waste produced (chemicals, infectious and radioactively contaminated sub-stances etc.) according to the prevailing laboratory regulations. Detergents and cleaning agents must be disposed according to the special waste regulations.Label DefinitionInfectious MaterialThis warning symbol indicates the possible existence of biologically dangerous and infectious material. When working with this kind of material always observe the prevailing laboratory safety regulations and take necessary precautions and disinfection measures (e.g. wear-ing protective clothing, masks, gloves etc.). Non-observance 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: 2004 by WHO - World Health Organization.Radioactive MaterialThis warning symbol indicates the possible existence of radioactivity. When working with radioactive material always observe the safety reg-ulations and take necessary protective measures. Wear protective clothing, e.g. masks and gloves. Non-observance may cause severe personal injury or even death.Corrosive SubstancesThis warning symbol indicates the possible existence of corrosive sub-stances. When working with corrosive substances always observe the laboratory safety regulations, and take protective measures (e.g. wear protective masks and gloves). Non-observance may cause severe personal injury or even death.Table 1.2: Warning labels in case of hazardous sample material12 ALPHA User Manual Bruker Optik GmbHBrukerIntroduction 11.5 General information1.5.1 Protective earthingTo avoid personal injuries and/or damage caused by electrical power, the supplied spec-trometer power cord is equipped with a safety plug./UKR /ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.) >> /Namespace [ (Adobe) (Common) (1.0) ] /OtherNamespaces [ > > /FormElements false /GenerateStructure false /IncludeBookmarks false /IncludeHyperlinks false /IncludeInteractive false /IncludeLayers false /IncludeProfiles false /MultimediaHandling /UseObjectSettings /Namespace [ (Adobe) (CreativeSuite) (2.0) ] /PDFXOutputIntentProfileSelector /DocumentCMYK /PreserveEditing true /UntaggedCMYKHandling /LeaveUntagged /UntaggedRGBHandling /UseDocumentProfile /UseDocumentBleed false >> ]>> setdistillerparams> setpagedeviceConnect this safety plug only to an earthed power socket. Make sure that the earthed power socket used complies with IEC (International Electrotechnical Commission1).1.5.2 Qualified personnelInitial installation and all maintenance and repair work not described in this manual should only be performed by Bruker service personnel. Make sure that the spectrometer is only operated and maintained (i.e. only maintenance work that is described in this manual) by authorized operating personnel trained in the spectrometer operation and all relevant safety aspects.All repairs, adjustments and alignments on any spectrometer component must be per-formed in accordance with the safety regulations and standards applied in the country where the instrument will be installed.1.5.3 Intended useThe 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 con-nection with the spectrometer, Bruker Optik GmbH does not assume any liability for safe operation and proper functioning.1. International standards organization for electrical and electronic-related technologies. 13 Optik GmbH ALPHA User ManualIntroduction 11.6 Questions and concernsIf you have questions or concerns about safety, operating the spectrometer, or if you need assistance with software problems or replacement parts, contact Bruker at the numbers listed below:• 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.comservice.bopt.us@bruker.com• Internet: www.bruker.com/optics• International service: www.bruker.com/about-us/offices/offices/bruker-optics14 ALPHA User Manual Bruker Optik GmbHBruker2 ALPHA spectrometerThe ALPHA spectrometer is a compact FT-IR spectrometer, with modular design for rou-tine applications in the laboratory.ALPHA consists of a basic module and an exchangeable sampling module.Definition1 Basic module2 Sampling moduleTable 2.1: Spectrometer modulesFigure 2.1: Modular spectrometer design2115 Optik GmbH ALPHA ALPHA spectrometer 22.1 Basic moduleThe basic module is equipped with the following optical components:Optical component SpecificationIR source • air cooled• low voltage• lifetime: 44.000 operating hoursInterferometer • Rocksolid• permanently adjustedBeamsplitter • KBr (standard)• ZnSe (optional High Humidity variant)Window material • KBr (standard)• ZnSe (optional High Humidity variant)Detector DTGSa, room temperaturea. DTGS: deuterated triglycine sulphateTable 2.2: ALPHA - Optical componentsFigure 2.2: ALPHA - Basic module16 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.1.1 Connection ports and LEDsThe following are located on the rear side of the basic module:• connection ports for power supply and Ethernet• system diagnostics LEDsType Definition/Function1 USB port 5 V power supply, e.g. for WLAN adapter2 ETH/LAN port ➣ Port to connect the spectrometer to the PCi Use the supplied cross-over data cable, 100Base-T with RJ45 ports. See also the ALPHA installation instructions.3 TKD LED ➣ If the TKD LED is green, the interferometer mirror is within the data acquisition range.➣ During data acquisition the light intensity changes to bright green.i The TKD abbreviation means Take Data.4 ACC LED ➣ If the ACC LED is yellow, the network accesses the optics.➣ During data transfer the LED will be light yellow.i The ACC abbreviation means Access.Table 2.3: Basic module - Connection ports and LEDs and their functionsFigure 2.3: Basic module- Connection ports and LEDs111098765432117 Optik GmbH ALPHA ALPHA spectrometer 25 DIR/ERR LED ➣ If the DIR/ERR LED flashes slightly red in normal operation, the scanner moves.➣ If the LED is permanently bright red, there must be an interferometer problem, e.g. missing laser signal.i As long as this LED is permanently red no data acquisition is possible. The DIR abbreviation means Direction, ERR means Error.6 Ext. Accessory port Port to connect spectrometer to external optional accessories, e.g. detector, remote trigger etc.7 TAP port Male connector with 10 socket contacts for service and diagnosticsi The TAP abbreviation means Test Access Port.8 CFG switch Fourfold DIP switch, the following lever positions are possible:• #1 ON and #2 OFF: DHCP mode - use last DHCP address• #1 OFF and #2 ON: use ON-IP address 10.10.0.1• #3: stay in boot loader, do not load the application program• #4: reservedi The CFG abbreviation means Configuration.9 SBY/RES button ➣ Pressing this button about 2 seconds, activates/deactivates the stand-by mode. ➣ Pressing this button more than 6 seconds, resets the spectrometer.i The abbreviation SBY means Standby, RES means Reset.10 POWER port Port to connect the spectrometer to power supply i Use the supplied power cord with mains adapter. The POWER port is suited for extra low-voltage connectors. Only use power cords which have been approved by Bruker. See also the ALPHA installa-tion instructions.Type Definition/FunctionTable 2.3: Basic module - Connection ports and LEDs and their functions18 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.1.2 Stand-by modeThe spectrometer can be set into stand-by mode by pressing the SBY/RES button. The button is located on the rear spectrometer side (chapter 2.1.1).i If the spectrometer is in stand-by mode, it is not switched off completely. There is still some power consumption which is, however, significantly lower than in operation mode as the IR source, laser and detector are switched off.2.1.2.1 Activating11 Kensington lock Optional safety (anti-theft) lock for mobile hardwareType Definition/FunctionTable 2.3: Basic module - Connection ports and LEDs and their functions1 Press the SBY/RES button for a short time (about 1 to 2 seconds).➣ The button is located at the spectrom-eter rear side.2 • The spectrometer beeps.• The green status indicator on the spec-trometer top side (marking in figure) begins to flash in short intervals.• The status light on the OPUS spectros-copy software interface becomes gray.Table 2.4: Activating stand-by mode19 Optik GmbH ALPHA ALPHA spectrometer 22.1.2.2 Deactivating1 Press the SBY/RES button for a short time (about 1 to 2 seconds).➣ The button is located at the spectrom-eter rear side.2 • The spectrometer beeps.➣ Laser, IR source and detector are switched on again.• The status indicator on the spectrometer top side (marking in figure) and on the software interface are yellow.➣ Reason: The IR source needs about 7 minutes to reach its operating tem-perature.i As soon as the IR source has reached its operating temperature, the status indicator on the spectrometer top side and on the spectroscopy software interface is permanently green.Table 2.5: Deactivating stand-by mode20 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.2 Exchanging sampling moduleThe different types of ALPHA sampling modules can be attached and detached from the basic module. The procedure is the same for all types of sampling modules.2.2.1 ProcedureFigure 2.4: Different ALPHA sampling modules1 Press the lock, located on the basic mod-ule, right down.➣ The sampling module is released from the basic module. The lock stops at half-height.2 Detach the sampling module from the basic module.Table 2.6: Exchanging sampling module21 Optik GmbH ALPHA ALPHA spectrometer 22.2.2 After exchanging the sampling moduleAfter exchanging the sampling module, a calibration is performed. The calibration is indi-cated by a yellow message bubble on the bottom right end of the software interface.If the calibration has finished, the performance test starts(chapter 7.2.1). A yellow bub-ble appears on the bottom right of the OPUS graphical interface, and contains an appro-priate message.3 Push the new sampling module right towards the basic module.4 Press the lock on the basic module once again right down.➣ The sampling module engages into the basic module. The lock snaps right up.Table 2.6: Exchanging sampling module22 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.3 Spectrometer configuration2.3.1 ALPHA for transmission measurementsALPHA Sample typeALPHA-T(Universal Sampling Module)• Solids• Liquids• GasesALPHA-T with liquid cellsLiquidsALPHA-Twith gas cells (different types of path lengths possible)GasesALPHA-Twith 30° reflection accessorySolidsTable 2.7: ALPHA for transmission measurements23 Optik GmbH ALPHA ALPHA spectrometer 22.3.2 ALPHA for ATR measurementsALPHA Sample typeALPHA-E (Eco ATR module)• Solids• LiquidsALPHA-P(Platinum ATR module)• Solids• LiquidsALPHA-P(Platinum ATR module, high pressure variant)• Solids• LiquidsALPHA-P(Platinum ATR module, heat-able, without pressure applica-tor)LiquidsALPHA-P(Platinum ATR module, heat-able, with pressure applicator)• Solids• LiquidsALPHAATR multi reflection sampling module (A213/D-11)• Solids• LiquidsTable 2.8: ALPHA for ATR measurements24 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.3.3 ALPHA for reflection measurementsALPHA Sample typeALPHA-R (Drift module, for diffuse reflection)SolidsALPHA-R (A241/D, contact-less reflection)SolidsALPHA-R (A241/DL, contact-less reflection)SolidsALPHA-R (A241/DV, contact-less, video-assisted reflection)SolidsALPHA-R (A240/DU, diffuse and specular reflection from the bottom upwards)SolidsTable 2.9: ALPHA for reflection measurements25 Optik GmbH ALPHA ALPHA spectrometer 22.3.4 ALPHA for gas analysisALPHA Sample typeALPHA-G (A139/D, with long-path gas cell)GasesALPHA-G(A139-H1 with long-path gas cell and heating jacket)GasesALPHA(A128D/T with heatable 7 cm gas cell)GasesTable 2.10: ALPHA for gas analysis26 ALPHA Bruker Optik GmbHBrukerALPHA spectrometer 22.4 DesignDue to its modular design many maintenance tasks, e.g. replacing IR source are easy to perform and can be achieved without any re-alignment of the optics. The consumables and electronic components are located in separate compartments and can therefore be replaced without interfering with the sealed, desiccated optics area. For further details on maintenance refer to chapter 9.Full support of industry standard communication protocols makes the integration simple. A permanent on-line diagnostics of each spectrometer component facilitates trouble-shooting and maintenance.i Depending on the spectrometer configuration ordered, the spectrometer may not include all options that are described in this manual.2.5 Applications• Analysis of liquids and solids• Analysis of gases• Contactless and non-destructive analysis2.6 Spectrometer housingUnder no circumstances is the operator allowed to open the sealed spectrometer hous-ing.2.7 OpticsThe spectrometer incorporates state-of-the-art optics for outstanding sensitivity and sta-bility, which enables• high quality measurement results• less down-time• direct method transferThe spectrometer uses a permanently aligned ROCKSOLID interferometer which ensures a high energy throughput and low polarization effects.In the standard configuration the spectrometer is equipped with a room-temperature DTGS1 detector.1. DTGS: deuterated triglycine sulphate27 Optik GmbH ALPHA ALPHA spectrometer 22.8 ElectronicsThe electronics are based on a high speed 24 bit data sampling unit that guarantees experimental results with an outstanding accuracy. Any modern data system (PC work-station, laptop etc.) with the OPUS spectroscopy software installed can be used to con-trol the instrument and perform data processing. The spectrometer is linked to the data system by a standard 100Base-T Ethernet connection, which allows the spectrometer to be integrated into an existing data network.The spectrometer is completely software controlled. All components can be operated using the OPUS spectroscopic software. Diagnostic routines help to maintain optimum status and maximum instrument performance which is validated by the OPUS Validation Program (OVP) using the internal validation unit (IVU) which is also called aperture or fil-ter wheel.2.9 Spectroscopy softwareThe spectrometer is operated by the OPUS spectroscopy software. More detailed infor-mation on the OPUS software is described in the OPUS Reference manual.28 ALPHA Bruker Optik GmbHBruker3 ALPHA for transmission measurement3.1 Overview on ALPHA spectrometer configurations for transmissionMeasurement type: transmissionUsable sample material: • solids (films, KBr pellets)• liquids• gasesOptional measuring tools: • liquid cell• gas cell• 30° reflection accessoryALPHA spectrometer configurations for transmissionALPHA-Tuniversal sampling moduleALPHA-T with liquid cellsALPHA-Twith gas cells (different types of path lengths possible)ALPHA-Twith 30° reflection accessoryTable 3.1: ALPHA spectrometer configurations for transmission29 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.2 ALPHA-T universal sampling module3.2.1 SpecificationsMeasurement type: transmissionUsable sample material: • solids (films, KBr pellets)• liquids• gasesDefinition1 Lock/release2 Sample compartment lidTable 3.2: ALPHA-T sampling module - ComponentsFigure 3.1: ALPHA-T universal sampling module21Spectral range: • 375 – 7,500 cm-1, with standard KBr beamsplitter• 500 – 6,000 cm-1, optionally with high humidity ZnSe opticsSpectral resolution: • better than 2 cm-1• optionally better than 0.8 cm-1 Wavenumber accuracy: better than 0.05 cm-1 @ 1,576 cm-130 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.2.2 Optical pathFigure 3.2: ALPHA-T - Optical path31 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.2.3 Opening sample compartmentOpening the sample compartment is identical with all ALPHA-T spectrometer configura-tions.1 Reach under the bottom edge of the sample compartment lid.2 Lift up the sample compartment lid.Table 3.3: ALPHA-T sampling module - Opening sample compartment32 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.2.4 Starting measurement3.2.4.1 Loading measurement experiment☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (TRANS.XPM) assigned to the sampling module is automati-cally loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. Start the OPUS spectroscopy software and wait until the performance test (chapter 10.5 et seq.) has finished.➣ The spectrometer status indicator and the OPUS status light must be green.2. On the Measure menu, select the Setup Measurement Experiment command.3. On the dialog that opens, click the Basic tab.4. Click the Load button and select the TRANS.XPM experiment file from the dialog that opens.5. Click the Accept & Exit button.3.2.4.2 Starting background measurement1. Make sure that the OPUS status light is green.2. Make sure that not any sample is available in the sample compartment.3. Turn down the sample compartment lid.4. On the OPUS Measure menu, select the Measurement command.5. On the dialog that opens, click the Start Background Measurement button.6. Wait until the background measurement has finished.3.2.4.3 Starting sample measurement1. Lift up the sample compartment lid.2. Insert the sample.3. Turn down the samplecompartment lid.4. On the OPUS Measure menu, select the Measurement command.5. On the dialog that opens, click the Start sample Measurement button.6. Wait until the sample measurement has finished.1. The universal ALPHA-T sampling module is supplied with the TRANS.XPM experiment file. This experi-ment file contains the default parameters set by Bruker, to be used to perform transmission measurement.33 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.2.5 Potential operating errors3.3 Measuring accessoriesDepending on the type of sample used (solid, liquid or gas) different types of measuring accessories are available to position the sample into the sample compartment of the sampling module:Possible problems TroubleshootingInstrument/performance test not passed• Check whether there is a sample or any other kind of object inside the sample compartment.• Remove sample or object from the sample com-partment.• Start instrument/performance test again.Table 3.4: Potential operating errorsIncluded in delivery content: 2 x 3" sample holder for KBr pellets (13 mm)Optional measuring acces-sory:• foil holder• liquid cell• gas cell• 30° reflection accessoryTable 3.5: ALPHA-T sampling module - Measuring accessory34 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.3.1 Sample holder (standard)By default, the sample holder is mounted in the middle of the sample compartment. On the left side of the sample holder there is a fixture to insert the sample.Definition1 Sample holder2 FixtureTable 3.6: Sample holder - ComponentsFigure 3.3: ALPHA-T sampling module with sample holder21235 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.3.2 Foil holder (option)To perform spectroscopic analysis of foils you can fix the foils in a foil holder. To measure the sample is inserted into the foil holder. The foil holder is mounted in the sample com-partment, by default.3.3.3 Liquid cell (option)To perform spectroscopic analysis of liquid samples, liquid cells are inserted into the sample holder. The sample holder is mounted in the sample compartment, by default.Figure 3.4: Foil holder for ALPHA-TDefinition1 Liquid cell2 Sample holderTable 3.7: Liquid cell - ComponentsFigure 3.5: ALPHA-T sampling module with liquid cell2136 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 3When analyzing the sample in a liquid cell observe the following:• Avoid any air bubbles when filling in the sample into the liquid cell.• Thoroughly empty and clean the liquid cell after each measurement.• Clean the liquid cell using an appropriate solvent.i The solvent to be used for cleaning depends on the window material of the cell. Do not use water for cleaning in case of KBr windows. Do not use acidic solvents for cleaning in case of ZnSe windows.3.3.4 Gas cell (option)To perform spectroscopic analysis of gaseous samples the gas cell is inserted into the sample compartment together with a special gas cell holder. The following gas cell types can be inserted into the sample compartment:Gas cell Path length Position of gas cell holder Spectral rangeA131: 10 cm Right Depending on the win-dow material:• CaF2: >1.200 cm-1• NaCl: >700 cm-1• KBr: >380 cm-1• KRS-5: >200 cm-1• PE: 600-10 cm-1A132: 5 cm Right >500 cm-1A133/D-3: 30 mm Middle >1200 cm-1Table 3.8: Gas cell types to be inserted into the sample compartment37 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.3.4.1 Displacing mounted sample holderi To insert the gas cell into the ALPHA-T sample compartment you may first have to dis-place the sample holder in the sample compartment. This, however, does not apply to each gas cell type. In case of doubt, contact Bruker Service (chapter 1.6).Procedure1 Lift up the sample compartment lid.2 Remove the blue casing at the front side of the sample compartment.3 Use the TX20 screw driver supplied to loosen the two TORX screws which fix the sample holder.Table 3.9: Displacing sample holder when using ALPHA-T with gas cell38 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.3.4.2 Inserting gas cell into the sample compartment4 Mount the sample holder to the most right position.5 Attach the blue casing onto the front side of the sample compartment.Table 3.9: Displacing sample holder when using ALPHA-T with gas cell1 Insert the gas cell holder into the fixture of the sample holder.Table 3.10: ALPHA-T sampling module - Inserting gas cell into the sample compartment39 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.4 ALPHA-T 30° reflection accessoryTo perform fast surface spectroscopic analysis of solid samples by specular reflection, the 30° reflection accessory is inserted into the sample compartment.3.4.1 Specifications2 Position the gas cell onto the gas cell holder as shown in the left figure.Table 3.10: ALPHA-T sampling module - Inserting gas cell into the sample compartmentFigure 3.6: ALPHA-T 30° reflection accessorySpectral range: 375 to 7,500 cm-1Angle of incidence: 30°Sample spot: 8 mm ØAdditional components: reference mirror (gold)Special features: horizontal face-down sample posi-tion, to fix into sample holder40 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.4.2 Displacing mounted sample holderTo insert the 30° reflection accessory into the ALPHA-T sample compartment you first have to displace the sample holder located in the sample compartment, into the outer right position.Procedure1 Lift up the sample compartment lid.2 Remove the blue casing at the front side of the sample compartment.3 Use the TX20 screw driver supplied to loosen the two TORX screws which fix the sample holder.Table 3.11: Displacing sample holder when using ALPHA-T with 30° reflection accessory41 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.4.3 Inserting 30° reflection accessory into the sample compartment4 Mount the sample holder to the most right position.5 Attach the blue casing onto the front side of the sample compartment.Table 3.11: Displacing sample holder when using ALPHA-T with 30° reflection accessory1 Insert the 30° accessory reflection into the fixture of the sample holder.2 Position the 30° reflection accessory as shown in the left figure.Table 3.12: ALPHA -T sampling module - Inserting 30° reflection accessory into the sample compartment42 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for transmission measurement 33.4.4 Performing measurementMeasurement is performed by the OPUS spectroscopy software. Before starting a sam-ple measurement you first have to perform a background measurement. Observe the steps described in chapter 3.4.4.1 to 3.4.4.3.3.4.4.1 Loading measurement experiment☞ Measurement experiment file is loaded.➣ If AAR accessory recognition is activated (which is the case by default), the OPUS spectroscopy software recognizes the sampling module used. Thus, the experiment file1 (TRANS.XPM) assigned to the sampling module is automati-cally loaded in OPUS. If the experiment file is not loaded automatically, perform the steps 1 et seq.1. Start the OPUS spectroscopy software and wait until the performance test (chapter 10.5) has finished.➣ The spectrometer status indicator and the OPUS status light must be green.2. On the Measure menu, select the Setup Measurement Experiment command.3. On the dialog that opens, click the Basic tab.4. Click the Load button and select the TRANS.XPM experiment file from the dialog that opens.5. Click the Accept & Exit button.1. The universal ALPHA-T sampling module is supplied with the TRANS.XPM experiment file. This experi-ment file contains the default parameters set by Bruker, to be used to perform transmissionmeasurement.43 Optik GmbH ALPHA User ManualALPHA for transmission measurement 33.4.4.2 Starting background measurement1. Put the reference mirror onto the reflection unit and push it completely to the right.2. Turn down the sample compartment lid.3. On the OPUS Measure menu select the Measure command.4. On the dialog that opens, click the Start Background Measurement button.5. Wait until the background measurement has finished.3.4.4.3 Starting sample measurement1. Lift up the sample compartment lid.2. Remove the reference mirror.3. Position the sample exactly onto the reflection unit.4. Turn down the sample compartment lid.5. On the Measure menu, select the Measure command.6. On the dialog that opens, click the Start Sample Measurement button.7. Wait until the sample measurement has finished.Figure 3.7: Putting reflection mirror onto reflection unit44 ALPHA User Manual Bruker Optik GmbHBruker4 ALPHA for ATR measurement4.1 Overview on ALPHA spectrometer configurations for ATRMeasurement type: attenuated total reflectionUsable sample material: • solids (paste, powder, gel, granu-lar material, work pieces)• liquids• polymer film• surface coatingAvailable crystal types: • diamond• germanium (Ge)• zinc selenide (ZnSe)ALPHA spectrometer configurations for ATRALPHA-E (Eco ATR module)ALPHA-P(Platinum ATR module)ALPHA-P(Platinum ATR module, high pressure variant)Table 4.1: Overview on ALPHA spectrometer configurations for ATR45 Optik GmbH ALPHA User ManualALPHA for ATR measurement 4ALPHA-P(Platinum ATR module, heat-able, without pressure appli-cator)ALPHA-P(Platinum ATR module, heat-able, with pressure applica-tor)ALPHA ATR multi reflection sampling moduleALPHA spectrometer configurations for ATRTable 4.1: Overview on ALPHA spectrometer configurations for ATR46 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.2 ALPHA-E sampling moduleMeasurement type: attenuated total reflectionUsable sample material: • solids (paste, powder)• liquids• foilsAvailable crystal types: • germanium (Ge)• zinc selenide (ZnSe)Actual sampling surface on ATR crystal:5 mm ØDefinition1 Knob to press and release the anvil2 Anvil3 Crystal plate with integrated ATR crystalTable 4.2: ALPHA-E sampling module - ComponentsFigure 4.1: ALPHA-E sampling module12347 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.2.1 Optical path11. With the ATR crystal plate being fixed, the edge of the ATR crystal is turned by about 10° to the perpendicular line of the IR-beam, which becomes visible in case of ZnSe crystal types. This does by no means affect the light throughput.Figure 4.2: ALPHA-E - Optical path48 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.3 ALPHA-P sampling moduleMeasurement type: attenuated total reflectionUsable sample material: • solids (paste, powder)• liquidsAvailable crystal types: • diamond• germanium (Ge)Actual sampling surface on ATR crystal:• diamond: 2 x 2 mm• germanium: 5 mm ØAnvil tip types: • Standard tip type for powder, foils, work pieces• Special tip type for granular mate-rialDefinition1 Lever to move the anvil up and down2 Pressure arm3 Pressure control spot (red spot)Table 4.3: ALPHA-P sampling module - ComponentsFigure 4.3: ALPHA-P sampling module65432149 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.3.1 Optical path4.3.2 High-pressure variant4 Anvil5 Knob to adjust height adjustment of pressure arm6 Crystal plate with integrated ATR crystalDefinitionTable 4.3: ALPHA-P sampling module - ComponentsFigure 4.4: ALPHA-P - Optical pathMeasurement type: attenuated total reflectionUsable sample material: • solids (paste, powder)• liquidsAvailable crystal types: • diamondActual sampling surface on ATR crystal:2 x 2 mm Anvil tip types: • Standard tip type for powder, foils, work pieces• Special tip type for granular mate-rial50 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 4Definition1 Knob to press and release the anvil2 Anvil3 Pressure arm4 Crystal plate with integrated ATR crystalTable 4.4: ALPHA-P sampling module - Components of high-pressure variantFigure 4.5: ALPHA-P sampling module - High-pressure variant432151 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.3.3 With heatable ATR unitThe desired temperature value is set by using the OPUS spectroscopy software. The temperature controller (chapter 4.3.3.1) integrated into the ALPHA-P sampling module heats the sample position up to the temperature set in the software.The ALPHA-P sampling module with heatable ATR unit is available in different variants:Measurement type: attenuated total reflection up to a temperature of 120°CUsable sample materiala:a. In case of ALPHA-P with pressure applicator only.• solids (paste, powder)• liquidsAvailable crystal types: diamondActual sampling surface on ATR crystal:2 x 2 mm Maximum sample tempera-ture:120°CVariant IllustrationWithout pressure applicator:• 1: crystal plate with integrated ATR crystal• 2: temperature LEDTable 4.5: ALPHA-P sampling module with heatable ATR unit - Variants2152 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 4With pressure applicator:• 1: pressure arm• 2: crystal plate with integrated ATR crystal• 3: temperature LEDWith flow-through cell:• 1: temperature LED• 2: clamping bracket• 3: flow-through cellVariant IllustrationTable 4.5: ALPHA-P sampling module with heatable ATR unit - Variants32132153 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.3.3.1 Temperature controller status indicated by temperature LEDThe temperature LED indicates the temperature controller status as follows:4.3.3.2 Software requirements in case of OPUS versionfor col-lecting the sample liquid.i Alternatively, you can connect the drain and filling hoses to a pump to ensure a continuous liquid flow-through.Table 4.7: Installing flow-through cell55 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.3.3.4 De-installing flow-through cell4.4 Crystal materialDepending on the sampling module used, the ATR crystal plate is available with the fol-lowing types of crystal material: • diamond• germanium (Ge)• zinc selenide (ZnSe)Due to the accessory recognition (AAR), which is activated by default, the crystal mate-rial is automatically recognized with ALPHA. The color of the crystal indicates which type of crystal material is used for the crystal plate.The specifications of the crystal material are described in appendix A.5.1 Rotate fastening screw upwards.2 Pull out the two locking pins.3 Lift up the retaining clip.4 Remove the flow-through cell from the ATR crystal.Table 4.8: De-installing flow-through cellCrystal material Crystal colorDiamond TransparentGermanium Silver grayZinc selenide YellowTable 4.9: Crystal colors56 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.5 Replacing ATR crystal platei As it is not easy to rotate the ATR crystal plate manually, it is recommended to use the pin supplied. The leverage effect of the pin facilitates rotating the crystal plate.4.5.1 ProcedureCAUTIONImproper use of the ZnSe crystal material, broken crystalHealth damage, risk of poisoning➣ Carefully handle broken crystal fragments.➣ Avoid material abrasion or dust.➣ Do not inhale nor ingest material abrasion or dust.1 Insert the pin supplied into the borehole of the crystal plate.2 Use the pin and rotate the crystal plate counterclockwise up to the stop (about 20°).3 Remove the crystal plate.4 Position the new crystal plate onto the ATR sampling module and insert the pin into the borehole of the crystal plate.5 • Use the pin and rotate the crystal plate counterclockwise up to the stop (about 20°). • Pull out the pin from the borehole of the crystal plate.Table 4.10: Replacing ATR crystal plate57 Optik GmbH ALPHA User ManualIHO_MOVIETAG#Film: #excrysttool.mpg#Kristallplatte austauschen#ALPHA for ATR measurement 44.6 Working with pressure applicatorHow to work with the pressure applicator depends on the sampling module used.4.6.1 With the ALPHA-E sampling module Definition Function1 Knob Moving pressure arm (B) upwards: ☞ Rotate the knob counterclockwiseMoving pressure arm (B) downwards:☞ Rotate the knob clockwise2 Pressure arm • Rotatable by 360°• Can be swivelled out of measuring positioni If you swivel the pressure arm into the measuring position again, the pressure arm snaps into place exactly above the ATR crystal.Table 4.11: ALPHA-E sampling module - Components of pressure applicatorFigure 4.6: Pressure applicator with the ALPHA-E sampling module32158 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.6.2 With the ALPHA-P sampling module3 Anvil Pressing sample against the ATR crystal• Increasing contact pressure:☞ rotate knob (A) further downwards• Decreasing contact pressure:☞ rotate knob (A) further upwardsi The inner part of the pressure arm (B) is equipped with a slip-clutch mechanism which is activated as soon as the optimal contact pressure between sam-ple and anvil has been applied. Further rotating the knob, which is only possible by substantial force, would not have any effect on the contact pressure already applied.Definition FunctionTable 4.11: ALPHA-E sampling module - Components of pressure applicatorFigure 4.7: Pressure applicator with ALPHA-P sampling module 542159 Optik GmbH ALPHA User ManualALPHA for ATR measurement 4Definition Function1 Lever • Moving anvil (E) upwards:☞ turn up the lever• Moving anvil (E) downwards:☞ turn down the lever2 Knob Adjusting height of pressure arm (C)• Moving pressure arm (C) upwards:☞ Rotate knob counterclockwise• Moving pressure arm (C) downwards:☞ Rotate knob clockwise3 Pressure arm • Rotatable by 360°• Can be swivelled out of measuring positioni If you swivel the pressure arm into the measuring position again, the pressure arm snaps into place exactly above the ATR crystal.4 Pressure control (red spot)Indicating contact pressure i The red spot must be exactly in the middle of the round recess on the front of the pressure arm to ensure optimal contact pressure (see figure 4.7).5 Anvil Pressing sample against the ATR crystalTable 4.12: ALPHA-P sampling module - Pressure applicator60 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.6.2.1 Adjusting height of pressure armTo adjust the height of the complete pressure arm (C in figure 4.7) is required if:4.7 Cleanness testBefore you start measuring, a cleanness test can be performed. This kind of test is a ref-erence measurement of the ATR crystal. Based on the maximum contamination limit allowed, the test verifies whether the crystal is clean. The tested wavenumber range is between 2800 and 3030 cm-1 (absorption).The cleanness test is performed by the OPUS spectroscopy software. Details on the cleanness test are described in the OPUS Reference manual.Problem Setting• Lever (A in figure 4.7) turned to the outermost front position• Anvil (E) has not yet any contact with the sample• Red spot below round recessMove pressure arm (C) downwards:☞ rotate knob (B) clockwise☞ rotate knob (B) until the red spot (D) is exactly in the middle of the round recess• Lever (A in figure 4.7) cannot be turned to the outermost front posi-tion as the sample is too thick• Red spot above round recessMove pressure arm (C) upwards:☞ rotate knob (B) counterclockwise☞ rotate knob (B) until the red spot (D) is exactly in the middle of the round recessTable 4.13: When must the height of the pressure arm be adjusted?61 Optik GmbH ALPHA User ManualALPHA for ATR measurement 44.8 Positioning sample on the ATR crystalBefore positioning the sample on the ATR crystal make sure that the sample plate, ATR crystal and the anvil are clean.i If the sample cannot be placed onto the ATR crystal as the distance between the ATR crystal and anvil is too small, you first have to move the pressure arm upwards.4.8.1 Procedure in case of ALPHA-E and ALPHA-P (non-heatable)1 Position sample in the middle of the sample plate.➣ The ATR crystal must completely be covered by the sample material. A small amount of sample material is sufficient.Improper use of flammable and/or explosive substances:Personal injury➣ Always wear safety googles.➣ Only use small amounts of sample material.➣ Do not inhale the vapor of volatile substances.➣ Observe the safety instructions.2 Press anvil against the sample.➣ Make sure that the optimum contact pressure is used to press the sample against the ATR crystal.3 Measure sample (chapter 4.9).4 • Move pressure arm upwards.• Remove sample. i Sample material should not be left in contact with the crystal for an extended period of time, as chemically reactive sample material may degrade the crystal quality and discolor the metal plate. Therefore, once the measure-ment has finished, remove the sample from the crystal.5 Thoroughly clean the sample plate, ATR crystal and anvil, see chapter 4.10.Table 4.14: Positioning sample on ATR crystal in case of ALPHA-E and ALPHA-P (non-heatable)CAUTION62 ALPHA User Manual Bruker Optik GmbHBrukerALPHA for ATR measurement 44.8.2 Procedure in case of ALPHA-P (heatable)Observe the following safety instructions when heating sample material:In case of flow-through cellLabel DefinitionHot liquids directly on the ATR crystal:When putting hot liquids onto the ATR crystal without using a flow-through cell, be careful as some hot liquids may splash around.➣ Always wear