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ALPHA

User Manual

1005541

2nd edition, publication date May 2011


2011 BRUKER OPTIK GmbH, Rudolf-Plank-Strae 27, D-76275 Ettlingen, www.brukeroptics.com
All rights reserved. No part of this manual may be reproduced or transmitted in any form or by
any means including printing, photocopying, microfilm, electronic systems etc. without our
prior written permission. Brand names, registered trademarks etc. used in this manual, even if
not explicitly marked as such, are not to be considered unprotected by trademarks law. They
are the property of their respective owner.
This manual is the original documentation for the ALPHA spectrometer. The ALPHA spectrometer is covered by one or more of the following patents: US 5,499,095; US 5,923,422; DE
19940981. Other US and international patents are pending.

<Number>1

Ta b l e o f C o n t e n ts
1

About this Manual . . . . . . . . . . . . . . . . . . . . . . . . 1

ALPHA & Measurement Modules . . . . . . . . . . . . . 3


2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8

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11
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M easurement . . . . . . . . . . . . . . . . . .
Q uali ty Contro l . . . . . . . . . . . . . . . . .
I dentification of an unknown Substance
Q u a n t i t a t i o n o f a S ample Component .

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No Sa mpl e P repa ration . . . . . . . . . . . . . . . . . . . . . . 4 2


KB r P e l l e t . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 2
Th i n fi l m be tw ee n two plates . . . . . . . . . . . . . . . . . . 4 3

Transmission Measuring . . . . . . . . . . . . . . . . . . 45
5.1
5.2
5.3
5.4

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Sample Preparation . . . . . . . . . . . . . . . . . . . . . . 41
4.1
4.2
4.3

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Quick User Guide . . . . . . . . . . . . . . . . . . . . . . . 13


3.1
3.2
3.3
3.4

G eneral Technical Feat ures . . . . . .


Basic Module . . . . . . . . . . . . . . . .
AL P H A -T Mea s u re m e n t M o d u l e . . . .
AL P H A - P M e a s u r e m e n t M o d u l e . . .
AL P H A - E M e a s u r e m e n t M o d u l e . . .
Exchanging Measurement
Mo d u l e
O perating Spectrometer . . . . . . . . .
Ac t i v a t i n g S t a n d - b y M o d e . . . . . . .

G eneral Information . . . .
AL P H A -T . . . . . . . . . . .
Positioning sample in the
ment . . . . . . . . . . . . . .
M easuring Sample . . . . .

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ALPHA-T
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sample compart. . . . . . . . . . . . .
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. 45
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. 47
. 50

ATR Measuring . . . . . . . . . . . . . . . . . . . . . . . . . 51
6.1
6.2
6.3
6.4
6.5
6.6
6.7

G eneral Information . . . . . . . . .
AT R Measurement Module . . . .
Pe r f o r m i n g C l e a n n e s s T e s t . . .
Placing Sample on AT R Crystal
M easuring Sample . . . . . . . . . .
Cleaning ATR Module . . . . . . .
AT R S pectra . . . . . . . . . . . . . .

Bruker Optik GmbH

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ALPHA User Manual

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51
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57
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iii

Table of Contents

Ma i n t e n a n c e & R e p a i r . . . . . . . . . . . . . . . . . . . . 6 1
7.1
7.2
7.3
7.4
7.5

Replacing IR Source . . . . . . . .
Replacing Desiccant Bags . . . .
Re p l aci ng Wi n d o ws . . . . . . . . .
Cl e a n i n g W i n d o w s . . . . . . . . . .
Cl e a n i ng S pe ctrom eter Housing

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62
65
67
70
70

Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . 71
8.1
8.2
8.3

G eneral Information . . . . . . . . . . . . . . . . . . . . . . . . . 7 1
Available Diagnostic M eans . . . . . . . . . . . . . . . . . . . 7 2
Problem - Possible Causes - Sol u t i o n s . . . . . . . . . . . 7 9

Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . 93

Consumables . . . . . . . . . . . . . . . . . . . . . . . . . . 95

Dimensional Drawings . . . . . . . . . . . . . . . . . . . . 97

Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

Service Addresses . . . . . . . . . . . . . . . . . . . . . 111

iv

ALPHA User Manual

Bruker Optik GmbH

Chapt. 1

About this Manual


The ALPHA user manual contains detailed information on the single
spectrometer measurement modules in chapter 2.
On the basis of different examples the Quick User Guide in chapter 3
provides a step-by-step introduction into the OPUS software, and gives
answers to analytical problems.
For sample preparation refer to chapter 4 which contains a short
summary of the most important sample preparation methods.
Chapter 5 describes in detail the measuring in transmission mode
and gives information on how to properly position the sample in the
sample compartment of the transmission module.
Detailed information on what has to be considered in case of ATR
measuring, what crystal types are available and how to position the
sample on the ATR crystal is given in chapter 6.
Maintenance instructions and a description of the steps required when
replacing the IR source, the desiccant bag as well as the KBr-window
are included in chapter 7.
Chapter 8 describes possible spectrometer problems, their diagnosis as
well as troubleshooting by means of the OPUS software.
The specifications of the ALPHA spectrometer are listed in
appendix A, the most important customer drawings are included in
appendix B.
The glossary in appendix D describes single relevant spectroscopic
terms in more detail. For the worldwide Bruker service addresses refer
to appendix E.

Bruker Optik GmbH

ALPHA User Manual

Chapt. 1

About this Manual

ALPHA User Manual

Bruker Optik GmbH

Chapt. 2

ALPHA & Measurement Modules


2.1

General Te chnical Features

The ALPHA spectrometer is a small compact FT-IR spectrometer


designed for routine applications in the laboratory. Due to its modular
design ALPHA ensures highest possible flexibility during measurement.
ALPHA consists of a basic module and an exchangeable measurement
module. The following measurement modules are available.
Module available

Type of measurement

To be used for the following


sample types

ALPHA-T
Transmission
(Universal Sampling Module)

Solids (e.g. plasic films, KBr


pellets) liquids, gases

ALPHA-P
Attenuated total reflection
(Platinum ATR Module; avail- (ATR)
able as high pressure module
as well)

Solids, liquids

ALPHA-E
(Economic ATR Module)

Solids, liquids

Attenuated total reflection


(ATR)

The different modules are described in the following. For further


information on the single measurement modules refer to chapter 5 and
6.

Basic module

Exchangeable
measurement
module

Figure 1: Modular spectrometer design

Bruker Optik GmbH

ALPHA User Manual

Chapt. 2

ALPHA & Measurement Modules

2.2

B asic Module

The basic module contains the following optical components:

IR source

low voltage, air cooled


lifetime: 44,000 operating hours

Interferometer

Rocksolid, permanently adjusted

Beam splitter
(material)

KBr (standard)
ZnSe (in case of high humidity option)

Window

KBr (standard)
ZnSe (in case of high humidity option)

Detector

DTGS detector (room temperature)

A permanent online diagnosis of the single components (e.g. IR source,


laser, detector and interferometer) facilitates troubleshooting and
maintenance.
The connecting ports (e.g. power, Ethernet) and the system diagnosis
LEDs are at the rear side of the basic module, see figure 2.

CDE

H I

Figure 2: ALPHA rear side - Connecting ports and LEDs

Type

Definition

USB port

Not available.

ETH/LAN port

The ETH/LAN port is used to connect the spectrometer to


a computer on which the OPUS software is installed. The
ETH port is designed for RJ-45 plugs and complies with
the Ethernet standard. To connect the spectrometer to the
PC the supplied data cable (cross over, 10Base-T with
RJ45 ports) is used. See also the ALPHA installation
instructions.

ALPHA User Manual

Bruker Optik GmbH

ALPHA-T Measurement Module

Chapt. 2

Type

Definition

TKD LED

The green TKD LED indicates that the interferometer mirror is within the data acquisition range. When data acquisition actually takes place the light intensity changes to
bright green. The TKD abbreviation means Take Data.

ACC LED

The yellow ACC LED indicates that the network accesses


the optics. During transition of measuring data the LED
will be light yellow. The ACC abbreviation means Access.

DIR/ERR LED

In normal operation mode the DIR/ERR LED flashes


slightly red and indicates the scanner movement. If the
LED lights permanently bright red, there must be an interferometer problem, e.g. missing laser signal. As long as
this LED lights permanently red no data acquisition is possible. The DIR abbreviation means Direction, ERR means
Error.

Ext. Accessory port This port can be used to connect external optional accessories, e.g. detector, remote trigger etc.

TAP port

The TAP male connector includes 10 socket contacts and


is used for service and diagnostics only. The TAP abbreviation means Test Access Port.

CFG switch

CFG is a fourfold DIP switch:


#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: reserved
The CFG abbreviation means Configuration.

SBY/RES button

Depending on how long you press this button you either


activate/deactivate the stand-by mode or reset the spectrometer (i.e. restore the initial spectrometer state). If you
press this button about 2 seconds, you activate/deactivate
the stand-by mode. If you press this button more than 6
seconds, the spectrometer will be reset. The abbreviation
SBY means Standby, RES means Reset.

POWER port

This port is used to connect the spectrometer to the power


supply. 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 installation instructions.

Kensington lock

This optional lock is a kind of safety (anti-theft) lock for


mobile hardware.

2.3

A LPHA-T Measurement Module

The ALPHA-T measurement module is designed for measurements in


transmission. This measurement module allows to spectroscopically
analyze both solids, liquids as well as gases.
Bruker Optik GmbH

ALPHA User Manual

Chapt. 2

ALPHA & Measurement Modules

In case of measuring liquid and gaseous samples optional liquid and gas
cells are available. These gas cells can be mounted into the sample
compartment of the transmission measurement module. For further
details on this subject see also chapter 5.

B
E
C

Figure 3: ALPHA-T

Definition
A

Basic module (with integrated electronics and optics)

Lock/release

ALPHA measurement module (for spectroscopic transmission measurements

Sample compartment lid

Status indicator

2.3.1

A L P H A - T s a m p l e c o m pa r t m e n t

The ALPHA-T sample compartment is behind the blue cover (D in


figure 3) and can be accessed from the front side.

To o p e n t h e s a m p l e c o m pa r t m e n t . . .
...reach under the bottom edge of the sample compartment lid
and lift it up.

ALPHA User Manual

Bruker Optik GmbH

ALPHA-P Measurement Module

Chapt. 2

B
C

Figure 4: ALPHA-T - Sample compartment open

Definition
A

Sample compartment lid

Sample holder

Ports for the IR beam passing the sample compartment

For detailed information on how to prepare and insert samples refer to


chapter 4 and 5.

2.4

A LPHA-P Measurement Module

The ALPHA-P measurement module is designed for measurements in


attenuated total reflection (ATR). This measurement module allows to
spectroscopically analyze both solids (e.g. paste, powder) as well as
liquids.
The following ATR crystal types are available:
Diamond
Germanium (Ge)
For further information on this measurement module refer to chapter 6.

Bruker Optik GmbH

ALPHA User Manual

Chapt. 2

ALPHA & Measurement Modules

Figure 5: ALPHA-P

Definition
A

Lever to move the anvil up and down

Pressure control spot (round recess)

Anvil

ATR crystal

ALPHA-P measurement module for ATR

Height adjustment for pressure arm

Basic module

Status indicator

Crystal plate with integrated ATR crystal

2.5

A LPHA-E Measurement Module

The ALPHA-E measurement module is designed for measurements in


attenuated total reflection (ATR). This measurement module allows to
spectroscopically analyze both solids (e.g. paste, powder) as well as
liquids.

ALPHA User Manual

Bruker Optik GmbH

Exchanging Measurement Module

Chapt. 2

The following ATR crystal types are available:


Germanium (Ge)
Zinc selenide (ZnSe)
For further information on this measurement module refer to chapter 6.

A
E

Figure 6: ALPHA-E

Definition
A

Knob to press and release the anvil

Anvil

Crystal plate with integrated ATR crystal

ALPHA-P measurement module for ATR

Basic module

Status indicator

2.6

Exchanging Measurement
Module

The three different measurement modules available (ALPHA-T,


ALPHA-P and ALPHA-E) can be exchanged. The procedure is the same
for all three measurement modules. See the following figure:
Bruker Optik GmbH

ALPHA User Manual

Chapt. 2

ALPHA & Measurement Modules

Step 1: Press the lock on the basic module


right down.
Note: The measurement module is released
from the basic module and the lock stops at halfheight.

Step 2: Pull out the measurement module


from the basic module.

Step 3: Push the new measurement


module right against the basic module.

Step 4: Press the lock on the basic module


once again right down.

Note: The measurement module engages into


the basic module, and the lock snaps right up.

Figure 7: Procedure when exchanging the measurement module

10

ALPHA User Manual

Bruker Optik GmbH

Operating Spectrometer

Chapt. 2

W h a t h a p p e n s a ft e r e x c h a n g i n g t h e m e a s u r ement module?
OPUS automatically recognizes the newly inserted measurement
module and starts a performance test (accessory test). For more
detailed information refer to the OPUS/MENTOR manual.

2.7

Operating Sp ectrometer

The spectrometer is operated by means of the OPUS software. For


detailed information on the OPUS software refer to the OPUS/MENTOR
manual and chapter 3.

2.8

A c t i v a t i n g Sta n d - b y M o d e

Basically, you can either set the spectrometer to stand-by mode or


completely disconnect it from the mains supply by unplugging the power
cord.
It is recommended to set the spectrometer to stand-by mode overnight.
Only in case of longer shut-down periods (e.g. several days) is it
advisable to completely disconnect the spectrometer from the mains
supply.
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.

H o w t o s e t A L P H A i n t o s ta n d - b y m o d e ?
1

Press the SBY/RES button (A in figure 8) at the spectrometer rear


side for a short time (about 1 to 2 seconds).

Figure 8: ALPHA rear side - Stand-by/Reset key

Bruker Optik GmbH

ALPHA User Manual

11

Chapt. 2

ALPHA & Measurement Modules

Now, the spectrometer beeps and the green status indicator on


the spectrometer top side begins to flash in short intervals. The
OPUS status light becomes gray.

How to set ALPHA into operation mode again?


1
2
3
4

12

Press again the SBY/RES button at the spectrometer rear side


only for a short time (about 1 to 2 seconds).
Now, the spectrometer beeps and the laser, IR source and detector are switched on again.
As the IR source warm-up takes about 7 minutes, the spectrometer status indicator is yellow during this period.
As soon as the IR source has reached its operating temperature,
the spectrometer status indicator permanently lights green.

ALPHA User Manual

Bruker Optik GmbH

Chapt. 3

Quick User Guide


The purpose of this quick user guide is to enable you to familiarize
yourself with the OPUS software within a short period of time and to
learn how to perform the most relevant analytical tasks on your own.
This chapter describes the procedures for realizing the following
analytical task definitions:
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 substance is
it?
Quantitative Analysis - How much of a certain component
does the sample contain?

3.1

M easurement

3.1.1

General Information

It is recommended to perform a measurement using the factory


parameter settings. In this case, you can start with the measurement
immediately. See the following descriptions General Measurement
Procedure.
In addition, OPUS offers you also the possibility to adapt the
measurement parameter settings (e.g. the parameter value Scan Time)
to your special demands. To do this, click in the OPUS wizard with the
left mouse button next to the Measurement button and select the option
Setup "Measurement"... (see figure 9). As a result, the Setup
Measurement Parameters dialog opens. For a detailed description of
this dialog window refer to the OPUS/MENTOR manual.

Figure 9: OPUS Wizard - Opening the Setup Measurement Parameters dialog

Bruker Optik GmbH

ALPHA User Manual

13

Chapt. 3

Quick User Guide

W h e n m e a s u r i n g a s a m p l e , a l w a y s pa y a t t e n t i o n
to the following issues:
If the sample needs to be prepared, due to its composition,
prepare it carefully and avoid preparation errors. For information about sample preparation refer to chapter 4.
Avoid measurement errors (e.g. the ATR crystal is not covered
completely with the sample).

3.1.2

General Measurement Procedure

Generally, the measurement procedure can be subdivided into the


following steps:
1
2
3
4
5
6
7

Measuring a background spectrum


Preparing the sample, if required
Measuring the sample spectrum
Manipulating the sample spectrum
Performing a peak pick, if required
Saving and / or printing the manipulated spectrum
Measuring the next sample, if required

How to perform a measurement:


1

Click in the OPUS Wizard on the Measurement button (see


figure 10).

Figure 10: OPUS Wizard - Starting a measurement

14

The following dialog window opens:

ALPHA User Manual

Bruker Optik GmbH

Measurement

Chapt. 3

Figure 11: Measurement dialog - Starting a Background/Sample Measurement

First, perform a background measurement (i.e. a measurement


without a sample in the spectrometer sample compartment or
without a sample on the ATR crystal) by clicking on the Start
Background Measurement button.

Note: When you acquire a background spectrum using the ATR


module, first check whether the ATR crystal is really clean, i.e.
it is absolutely free from residuals of the previous sample. If
your sample needs to be prepared using a solvent acquire the
background spectrum of the pure solvent (i.e. solvent without
sample).

4
5

The background measurement takes a few seconds. The measurement progress is shown in the lower status bar.
Put the sample in the spectrometer sample compartment or on
the ATR crystal.

Note: Depending on the composition of the sample (solid, powdery,


paste-like, liquid etc.), the sample may need to be prepared
before you can put it in measurement position of the spectrometer. For detailed information about sample preparation
refer to chapter 4.

6
7

Then click on the Start Sample Measurement button (see


figure 11).
The sample measurement takes a few seconds. The measurement progress is shown in the lower status bar. Afterwards, the
acquired sample spectrum is displayed in the OPUS spectrum
window.

Note: If you use the factory parameter settings, the spectrum is


stored by default under OPUS path/meas. The file name is
identical to the sample name you have entered in the Measurement dialog (see figure 11). If you do not enter a different
sample name the file name is incremented with any further
measurement.

Immediately after the sample measurement, the OPUS Wizard switches


automatically to the Manipulate level (see the following section).
Bruker Optik GmbH

ALPHA User Manual

15

Chapt. 3

Quick User Guide

3.1.3

M a n i p u l a t i n g a S a m p l e Spe c t r u m

After the sample measurement, a spectrum postprocessing may be


required to ensure that OPUS yields acceptable evaluation results, for
example when you intend to perform a substance identification or a
quantitative analysis. For this purpose, OPUS offers a number of
manipulation commands. Manipulating in this context means
"optimizing" the measured sample spectrum. This section describes the
following manipulation commands:
Baseline Correction
Atmospheric Compensation
For information about additional manipulation commands refer to the
OPUS/MENTOR manual.
A 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 a sample
prepared as a KBr pellet. (See also chapter 4, Sample Preparation.)
Figure 12 illustrates the effect of a baseline correction. For detailed
information about this command refer to the OPUS/MENTOR manual.

Spectrum before a
baseline correction

Spectrum after a
baseline correction

Figure 12: Baseline Correction

How to perform a baseline correction:


1

16

Measure a spectrum or load the file of the spectrum you intend to


manipulate by clicking on the corresponding button in the OPUS
wizard (see figure 10). Thereupon, the sample spectrum is
displayed in the spectrum window and OPUS switches
automatically to the Manipulate level.
Click in the OPUS Wizard on the Baseline Correction button (see
figure 13).
ALPHA User Manual

Bruker Optik GmbH

Measurement

Chapt. 3

Figure 13: OPUS Wizard - Performing a Baseline Correction

Thereupon, OPUS performs a baseline correction and displays


automatically the corrected spectrum in the OPUS spectrum window.

Note: To undo a baseline correction, select the Undo Changes command in the OPUS File menu.

The OPUS Atmospheric Compensation command 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 moment of the background measurement
and the moment of the sample measurement. Figure 14 illustrates the
effect of an atmospheric compensation. For detailed information about
this command refer to the OPUS/MENTOR manual.

Spectrum before
an
atmospheric
compensation
Spectrum after
an atmospheric
compensation

Figure 14: Atmospheric Compensation

Bruker Optik GmbH

ALPHA User Manual

17

Chapt. 3

Quick User Guide

How to perform an atmospheric compensation:


1

Measure a spectrum or load the file of the spectrum you intend to


manipulate by clicking on the corresponding button in the OPUS
wizard (see figure 10). Thereupon, the sample spectrum is
displayed in the spectrum window (as shown in figure 15) and
OPUS switches automatically to the Manipulate level.

Note: The Atmospheric Compensation command requires a spectrum file that includes, amongst others, the data blocks SSC
(Sample Single Channel) and RSC (Reference Single Channel). (See figure 15.) Otherwise, an atmospheric compensation cannot be performed.
OPUS Browser with a loaded spectrum file.
This file contains, amongst others, a SSC data block and a RSC data block.

Figure 15: Spectrum before an atmospheric compensation

2
3

Click on the Atmospheric Compensation button in the OPUS Wizard.


Thereupon, OPUS performs an atmospheric compensation and
displays automatically the atmospherically compensated spectrum in the OPUS spectrum window (see figure 16).

Note: To undo an atmospheric compensation, select the Undo


Changes command in the OPUS File menu.

18

ALPHA User Manual

Bruker Optik GmbH

Measurement

Chapt. 3

Figure 16: Spectrum after an atmospheric compensation

3.1.4

Peak Picking

The Peak Picking allows you a prompt determination of the exact


spectrum peak positions, i.e. the exact frequency values (x-values) at
which maxima (in case of an absorption spectrum) or minima (in case of
an transmission spectrum) occur in the spectrum.

How to perform a peak pick:


1

2
3

Measure a spectrum or load the file of the spectrum you intend to


manipulate by clicking on the corresponding button in the OPUS
wizard (see figure 10). Thereupon, the sample spectrum is
displayed in the spectrum window and OPUS switches
automatically to the Manipulate level. Depending on the
measurement method, the displayed spectrum is either an
absorption spectrum or a transmission spectrum or an ATR
spectrum.
Manipulate the spectrum, if required. Otherwise, click on the Evaluate tab and then on the Peak Picking button in the OPUS wizard.
Thereupon, the exact frequency values, at which maxima or minima occur, are displayed in the spectrum window. See figure 17a
and 17b.

Figure 17: a)Peak pick result in case of absorption b) Peak pick result in case of transmission

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How to perform an interactive peak pick:


1

Alternatively, you can pick peak(s) also interactively by clicking


with the left mouse button next to the Peak Picking button and
selecting the option Interactive Peak Picking. Thereupon, the
following view appears:

Line

Figure 18: Interactive peak picking

20

Using the line in the spectrum window, you can select interactively the peaks of which the frequency value is of interest to you.
symbol and move the line
To do this, place the cursor on the
with pressed left mouse button up- or downwards. The frequency
values of all peaks above this line are displayed (see figure 18).
Click on the Save button to save the currently displayed peak
position values. Thereupon, a PEAK data block is added to the
spectrum file in the OPUS browser.
Alternatively, you can view the peak picking result in form of a
report. The report is displayed below the spectrum window. See
figure 19. For information about the permanent display of the
information view, refer to the OPUS/MENTOR manual.

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Peak picking
result
displayed in
the
spectrum window

Peak picking
report
Figure 19: Peak picking report

How to perform a single peak pick:


Besides the Peak Picking command in the OPUS wizard, OPUS offers
you also the possibility to pick specifically a single peak (i.e. to have the
frequency value of a certain peak displayed) which is of interest to you.
To do this, proceed as follows:
1

The spectrum in question is displayed in the spectrum window.


Click with the right mouse button on the spectrum window and
select in the context menu the Single Peak Pick command (see
figure 20).

Figure 20: Single peak pick - Step 1

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2
3

As a result, the cursor changes its appearance as follows:


Place the cursor on the peak which is of special interest to you
and press the left mouse button. Thereupon, the frequency value
of the peak in question is displayed above the peak (see
figure 21). You can repeat a single peak pick as often as you like.
Position of an
individually
selected peak

Figure 21: Single peak pick - Step 2

3.1.5

Defining the next procedures

After OPUS has performed a spectrum manipulation, the wizard


switches automatically to the Evaluate level. Depending on your
particular analytical task (quality control, substance identification
quantitative analysis etc.) you can now evaluate your sample spectrum
using the corresponding OPUS evaluation command. The following
sections 3.2, 3.3 and 3.4 provide a detailed description of the most
relevant evaluation commands (Quick Compare, Spectrum Search and
Quantitative Analysis). For information about all available evaluation
commands refer to the OPUS/MENTOR manual.
After OPUS has performed an evaluation (e.g. Spectrum Search) the
wizard switches automatically to the Report level. On this level, you
decide how to deal with the current spectrum file. OPUS offers the
following options:

saving the processed spectrum and/or


printing the processed spectrum and/or
unloading the spectrum file and/or
measuring the next sample.

To do this, activate the corresponding checkbox(es) and click on the Go


button. As a result, OPUS performs automatically the selected action(s).
See figure 22.

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Figure 22: OPUS Wizard - Report level

How to save a processed spectrum:


1
2

Activate the Save Changes checkbox.


Click on the Go button. As a result, OPUS saves the processed
spectrum with the same file name and under the same path as
the original spectrum, i.e. the original spectrum is overwritten by
the processed one.

Note: If you want to preserve the original spectrum select the Save
File As command in the OPUS File menu and define a different
file name and/or path for saving the processed spectrum.

How to print a spectrum:


1
2

Activate the Print checkbox.


Click on the Go button. As a result, the spectrum currently displayed in the spectrum window is printed.

How to unload a spectrum file:


1

Activate the Unload checkbox.

Note: If you want to unload a processed spectrum, it is advisable


also to save it. To do this, also activate the Save Changes
checkbox. (See section How to save a processed spectrum.)

Click on the Go button. As a result, the current spectrum file is


unloaded from the OPUS browser.

H o w t o s ta r t t h e n e x t s a m p l e m e a s u r e m e n t :
1

Activate the Measure Next Sample checkbox.

Note: If you want to measure the next sample after having processed
a spectrum it is advisable to save this spectrum. To do this,
also activate the Save Changes checkbox. (See section How to
save a processed spectrum.)

Click on the Go button. As a result, the Measurement dialog window (figure 10) opens again allowing you to start the next sample
measurement by clicking on the corresponding button (see
section 3.1.2.)

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3.2

Quality Control

3.2.1

General Information

The Quick Compare evaluation command allows to check whether the


delivered goods or the self-made products are consistent with the
specified quality criteria. For realizing this task, there are the following
two OPUS commands:
Quick Compare Setup - This command allows to setup a
quick compare method. The method setup has to be done prior
to the actual Quick Compare.
Quick Compare - This command allows to perform a Quick
Compare using the method you have set up in advance.
(Quick Compare implies the comparison of a sample spectrum
with one or several reference spectra.)

3.2.2

The general course of quality control

Generally, quality control can be subdivided into the following steps:


1
2
3
4
5

Measuring reference sample(s) and storing the spectrum


(spectra)
Setting up a quick compare method and saving method file
Measuring the sample to be analyzed
Performing a quick compare
Interpreting the quick compare result

How to choose and measure a reference sample:


For setting up a quick compare method, you first need to measure at
least one or more reference spectra. In this case, reference spectra are
spectra of samples of which you know for certain that they are absolutely
consistent with the specified quality criteria. These samples are also
called reference standards.
When choosing and measuring reference sample(s), pay attention to the
following aspects:
Use only pure samples as reference standard (i.e. samples
that are free of unwanted contaminants).
Prepare the reference standards carefully (see chapter 4,
Sample Preparation).
Avoid measurement errors (e.g. the ATR crystal is not completely covered with the sample).
For detailed information about how to perform a measurement refer to
section 3.1.
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H o w t o s e t u p a n e w Q u i c k C o m pa r e m e t h o d :
1

Click on the Evaluate tab and then on the Quick Compare button
in the OPUS wizard. Thereupon, the following OPUS message
appears:

Figure 23: OPUS Message

Note: This message appears only when you click on the Quick Compare button for the very first time because at this stage a quick
compare method has not yet be set up. Otherwise, the quick
compare method set up or loaded at last is used automatically.

Click on the OK button. Thereupon, the Quick Compare Setup


dialog window opens. See figure 24.

Click on this button if you want


to modify an existing method
file (*.QCM).
If you want to set up a new
method, click on the other two
tabs (fig. 25 and 26) and enter
the desired parameter values.
Then, return to this page of
the dialog window and click on
the Store Method button.
Note: In the upper part of this
page, an overview of the
parameter values you have
specified on the other pages of
this dialog window is shown.

Figure 24: Quick Compare Setup - Load/Store Method

Click on the Reference Files tab and select reference spectrum


file(s) in question (see figure 25).

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On this page, you select the reference spectrum/reference spectra for Quick Compare.
You can select either:
- only one reference spectrum or
- all reference spectra that are
stored in a certain directory (In
this case, the reference spectra
can originate from the different
sample materials.) or
- the average spectrum of all reference spectra stored in a certain directory. (In this case, the
reference spectra must originate from the same sample
material!)

Figure 25: Quick Compare Setup - Reference Files

Click on the Parameters tab and enter the desired parameter values (see figure 26).
The entry of a comment is
optional.
When defining the frequency
region for the quick compare,
you can either:
- use the file limits or,
- enter the values for one or
more regions manually or
- select one or more frequency
regions interactively. (See
fig. 27.)

The threshold value has an influence on the quick compare


result.a) You can either set this
value (in %) using the slider or
enter it manually.
Figure 26: Quick Compare Setup - Parameters

a) With the threshold value, you determine the degree of similarity between the reference spectrum and the sample spectrum. In other words, you determine how similar reference spectrum and sample spectrum need to be in order that the quick compare result is OK. As a
general guideline: The higher the threshold value is the higher the similarity between the reference and the sample spectrum needs to be in order to get an OK result.

If required, you can also define a data preprocessing method (first or


second derivative) and you can exclude those spectral regions from the
Quick Compare in which CO2 bands occur (between 2400 ... 2275 and
680 ... 660cm-1) by activating the corresponding checkbox.
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We recommend the interactive selection of the frequency region. Select


those regions in which are the most relevant spectral information of the
substance to be analyzed. To define further regions, click with the right
mouse button on the Select Frequency Region(s) dialog and select the
option Add Regions in the popup menu (see figure 27). Then, put the
cursor on a boundary line of the newly added frequency region and
move it with pressed left mouse button to the desired position. After
having defined all relevant frequency regions, click on the OK button.

Figure 27: Interactive selection of the frequency region

To store the newly set-up method, click again on the Load/Store


Method tab an then on the Store Method button. See figure 24.

For detailed information about this dialog window refer to the


OPUS/MENTOR manual.

H o w t o p e r f o r m Q u i c k C o m pa r e :
1

2
3

Measure the sample of which you want to test the quality and
manipulate the sample spectrum, if required. See section 3.1. (Do
not unload the spectrum yet!)
Click on the Evaluate level in the OPUS wizard.
Click on the Quick Compare button. As a result, OPUS performs
automatically a Quick Compare using the method you have set up
before or the method which has been loaded last.
Immediately after OPUS has executed a Quick Compare evaluation, the result is displayed automatically. (See figure 29, for
example.)

Note: Alternatively, you can start a quick compare evaluation using


the Quick Compare dialog window. To do this, click on the
Evaluate level in the OPUS wizard. Then, click with the left
mouse button next to the Quick Compare button and select
the option Select "Quick Compare" method.... Thereupon, the
Quick Compare dialog window opens (see figure 28).
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Spectrum file of the sample to be


analyzed (path and file name)
Path and file name of the currently loaded method Note: Normally, it is the method you have
set up or used at last.

Click on this button if you want to


use a different method.
You can decide whether the result
is to be displayed immediately
after the execution of the Quick
Compare and/or printed automatically by activating the corresponding checkbox(es).
Figure 28: Starting a Quick Compare

H o w t o i n t e r p r e t a Q u i c k C o m pa r e r e s u l t :
The Quick Compare result is OK if the correlation value is higher than
the threshold value you have determined. Analogous to this, the Quick
Compare result is not OK if the correlation value is lower than the
threshold value. In case of a Quick Compare evaluation, the correlation
coefficient1 r is a measure for the similarity between the two items
"reference spectrum" and "sample spectrum".
Depending on what you have selected as reference for the Quick
Compare (a single reference spectrum, an average spectrum or all
spectra of a certain directory), keep in mind the following when
interpreting the result:
If you have selected a single file or an average as reference,
you will get either an OK or Not OK as result (see figure 29, 30
and 31). In both cases, the displayed result allows you to see
at first sight whether the analyzed sample meets the specified
quality criteria or not (see figure 29 and 30).
If you have selected all spectrum files of a certain directory as
reference, you will not get a simply OK or Not OK as result. In
this case, only those reference spectra which have a sufficient
similarity with the sample spectrum, due to the threshold value
you have entered and the correlation value OPUS has calculated, are displayed black. All other reference spectra which do
not show a sufficient similarity with your sample spectrum are
displayed gray (see figure 32)1. Normally, the correlation coefficient values can range from -1,0 (i.e. no similarity between the
reference spectrum and sample spectrum at all) to +1,0 (i.e. absolutely identical spectra). For
the quick compare result, this value is converted into percentage with the range 1 r 0
being mapped to 0% and the range 0 r 1 being mapped linearly to 0% ... 100%.
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Figure 29: Result of a Quick Compare using one Reference - Sample Spectrum is OK

Figure 30: Result of a Quick Compare using one Reference - Sample Spectrum is not OK

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Figure 31: Result of a Quick Compare using an average as reference - Sample spectrum is OK

Figure 32: Result of a Quick Compare using several references - 1 hit has been found

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Identification of an unknown Substance

3.3

Chapt. 3

Identification of an unknown
Substa nce

3.3.1

General Information

The Spectrum Search evaluation command allows to identify an


unknown substance on the basis of its IR spectrum by comparing this
spectrum with the spectra of a library. Those library spectra which show
an obvious similarity with the spectrum of the unknown substance are
listed in a search report.
As already mentioned, a spectrum search is only possible if at least one
spectra library is available. By default, the two non-commercial spectra
libraries (with 350 and 200 entries, respectively) are delivered together
with the OPUS programme (see figure 33). Both libraries contain spectra
of a number of classes of substances (e.g. polymers, pharmaceuticals
etc.).

Figure 33: Available spectra libraries

Note: Besides the two libraries delivered with the OPUS software,
Bruker also offers a number of additional spectra libraries
which you can purchase.

A decisive factor for a successful substance identification is the


appropriateness of the available spectra libraries, i.e. a spectrum search
can yield only acceptable results if the selected library (libraries)
contain(s) entries (i.e. spectra plus additional information) of the classes
of substances (e.g. polymers, pharmaceuticals etc.) that you actually
analyze.

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In addition, OPUS offers you also the possibility to create your own
spectra library which is adapted to your special needs regarding the
substances you intend to identify. See section 3.3.3 Creating, building
up and maintaining your own spectra library.

3.3.2

T h e g e n e r a l c o u r s e o f a s u b s ta n c e i d e n tification

Generally, a spectrum search in a library can be subdivided into the


following steps:
1
2
3

Measuring the sample of an unknown


manipulating the sample spectrum, if required.
Starting the spectrum search.
Interpreting the result of a spectrum search.

substance

and

How to perform a spectrum search in a library:


Measure the sample of an unknown substance and manipulate
the sample spectrum, if required (see section 3.1).
After having executed a manipulation command, OPUS
switches to the Evaluate level. In case you did not manipulate
the spectrum, click on the Evaluate tab in the OPUS wizard.
Click on the Spectrum Search button. Thereupon, OPUS starts
the spectrum search using the factory-set search parameters.
In this case, all spectra libraries that are in the directory OPUS
path/Data/Library are searched.
Note: OPUS offers you also the possibility to change the factory-set
search parameters and/or to select different libraries. For
detailed information about this topic refer to the OPUS/MENTOR manual.

Immediately after OPUS has completed the spectrum search,


the search report is shown (see figure 34).

How to interpret a spectrum search result:


The search report consists of 4 sub-windows (see figure 34). The lower
sub-window shows the list of all hits found in the selected library
(libraries). By default, the first hit in the hit list is marked and its
information (spectrum, structural formula and compound information,
e.g. compound name, molecular formula, molecular weight etc.) are
displayed in the upper three sub-windows. To see this kind of
information for another hit, click in the hit list of the hit of which you want
to see more information.

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Substance
information

Structural
formula

Library spectrum and


query spectrum

Hit quality
value

Hit list

Figure 34: Spectrum Search report

The hit quality value in the hit list gives you a general clue to
what extent the spectrum of the unknown substance (also
called query spectrum) resembles the library spectrum.
The hit quality value can range from 0 (i.e. no resemblance at
all) to 1000 (i.e. absolute conformity of the library spectrum
with the query spectrum). The hit list is sorted according the hit
quality value, i.e. the hit with the highest quality value ranks
first in the hit list.
Moreover, you can compare visually the query spectrum with
the library spectrum to find out whether there is a certain
resemblance between the two spectra.

3.3.3

C r e a t i n g , b u i l d i n g u p a n d m a i n ta i n i n g
your own spectra library

Besides the usage of the delivered and/or commercial spectra libraries,


OPUS offers you the possibility to create your own library that suits your
specific analytical needs.
For creating, building up and maintaining your own spectra library, the
following OPUS commands are available:

Initialize Library
Store Spectrum in Library
Library Editor
Library Browser

For detailed information about these commands refer to the OPUS/


MENTOR manual.

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When creating your own spectra library, pay attention to following


aspects:
When choosing the samples for the library, try to cover the hole
range of the class(es) of substances you want to analyze with
this library in the future. Keep in mind the following: The more
extensive and diverse the library is, the better the search result
will be.
Use only pure substances (i.e. substance that are free of
unwanted contaminants).
Prepare these samples carefully (see chapter 4, Sample Preparation.)
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 adequately using the available manipulation commands.
Add preferably absorption spectra1 to the library.
Think already in advance of the additional information you
want to include in the library and make sure that they are available.
The above mentioned aspects are crucial preconditions for the creation
of a library that is to yield acceptable search results for future analyses.

1. In an IR spectrum, the position and intensity of the absorption bands are very substance-specific. Similar to a human fingerprint, the absorption spectrum of a substance is well-suited for
the identification of it.
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Quantitation of a Sample Component

3.4

Chapt. 3

Quantitation of a Sample Component

3.4.1

General Information

If your sample is a mixture of several components (e.g. a tablet


containing several active agents) OPUS allows you to quantitate one of
these components which is of special interest to you (e.g. the quantity of
active agent A contained in the tablet). For realizing this task, there are
the following two OPUS commands:
Quant Builder - for setting up a QUANT method and
Quantitative Analysis - for performing the actual quantitative
analysis
When you perform a quantitative analysis, it is highly recommended that
you normalize all spectra (i.e. both the calibration spectra and the
spectra of the sample(s) you intend to analyze) before the evaluation.
Spectra normalization is an OPUS manipulation command. Normalizing
means that the spectra are scaled to that effect that the minimum and/or
maximum of the spectra assume the same value. In doing so, the
spectra can better be compared with each other. Especially in case of
ATR spectra, a normalization is highly recommended. For detailed
information about this command refer to the OPUS/MENTOR manual.

3.4.2

T h e g e n e r a l c o u r s e o f a q u a n t i ta t i v e
analysis

Generally, a quantitative analysis can be subdivided into the following


steps:
1

2
3

Getting a set of about 5 samples and determining the exact


concentration values of the sample component in question using
a different technique (e.g. weighing). These samples are also
called calibration samples. They are required for setting up the
QUANT method.
Setting up a QUANT method using the OPUS command Quant
builder and the calibration samples.
Performing a quantitative analysis using the QUANT method you
have set up before and the OPUS command Quantitative Analysis.
Interpreting the analysis.

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W h e n c h o o s i n g t h e c a l i b r a t i o n s a m p l e s , pa y
a t t e n t i o n t o t h e f o l l o w i n g a s p e c ts :
Ideally, the calibration sample set should contain at least 5
samples.
Make sure that the concentration value of the component in
question differs from calibration sample to calibration sample.

How to setup a QUANT method:


1

3
4

Measure one of the calibration samples and manipulate the


sample spectrum, if required (see section 3.1). Keep the
spectrum file loaded in the OPUS browser.
Click on the Evaluate tab in the OPUS wizard, select the option
Quant Builder in the drop-down list and click on the Go button.
Thereupon, the Quant Builder - New dialog window opens (see
figure 35). The dialog window already includes the path and the
file name of the currently loaded spectrum file.
Enter the name of the component to be analyzed.
Specify the unit of the measurement (e.g. mg, ml, %) for the concentration value. Note: The unit of measurement you enter in
this dialog depends on the unit in which you have determined the concentration values of the calibration sample
before. And the result of the quantitative analysis is displayed in this unit as well.
Enter the exact component concentration value for the calibration
sample in question. Note: You need to have determined this
value before using a different analytical technique.
Enter the exact concentration value
of the component in question.

Path and file name of the


current spectrum file

Note: This value needs to be determined before by a different techCalibration line


nique.

Enter
the
component
name

Enter
the
unit of measurement

Figure 35: Dialog Window Quant Builder

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Already at this stage (i.e. on the basis of one calibration spectrum and its
corresponding concentration value), OPUS calculates a calibration line1
(see figure 35). In the further course of the QUANT method setup, this
calibration line will be improved by adding the data of the other
calibration samples.
Note: When you add the first calibration spectrum to a new QUANT
method, make sure that the New option button is activated.

Click on the Set Integration Area button. Thereupon, the window


shown in figure 36 appears allowing you to set an integration area
and select an integration method.

Note: Set the integration area in such a way that the spectral band
resulting from the component in question is within integration
area. For this reason, it is recommended to set the integration
area not until at least 3 or 4 calibration spectra have been
added to the QUANT method because only at this stage you
can recognize clearly the spectral band resulting from the
component in question (see figure 37).

Spectral band resulting


from agent A
Note: You can change the
integration area boundaries interactively by
placing the cursor on a
boundary and shifting it
with pressed left mouse
button.

Figure 36: Defining the Integration Area and the Integration Method

Now click on the Go to Quant button in order to return to the


Quant Builder dialog window.
8 Click on the Save button. As you are setting up a new QUANT
method, OPUS prompts you to enter file name and path under
which the method file is to be saved. Enter a file name, specify
the path and click on the Save button.
9 Thereupon, the Quant Builder dialog window disappears.
10 Measure the next calibration sample by clicking on the Measure
Next Sample... button in the OPUS wizard (see section 3.1).
1.The calibration line visualizes the relation between the calibration spectra and the corresponding concentration values of the component in question. For the quantitation of a certain component, OPUS calculates the quantity of this component on the basis of the spectrum of the
sample to be analyzed and the calibration line.
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11 Open the Quant Builder dialog again by clicking in the OPUS wizard on the Evaluate tab, selecting in the drop-down list the option
Quant Builder and clicking on the Go button.
12 Enter the component concentration value of the calibration sample in question.
Note: For the second and every following calibration sample, you do
not need to enter component name and unit again.

13 When adding the second or any further calibration spectrum to


the existing QUANT method, make sure that the Add spectrum
option button is activated.
14 To add the data of the second calibration sample to the QUANT
method, click on the Save button. Thereupon, the Quant Builder
dialog window disappears.
15 Repeat step 10 to 14 for the remaining calibration samples.
Only after you have added 3 or 4 calibration spectra to the QUANT
method is it recommended to set the integration area. To do this,
activate the Change option button and click on the Set Integration Area
button. Thereupon, the window shown in figure 37 appears.

Figure 37: Defining the integration area on the basis of several calibration spectra

At this stage, the window includes all calibration spectra added to the
QUANT method so far. The display of several calibration spectra
enables you to set the integration area because now the band resulting
from the component to be quantified is clearly recognizable due to
differences in the band height because the band height is quantitydependent.
For detailed information about the Quant Builder command refer to the
OPUS/MENTOR manual.

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H o w t o p e r f o r m a q u a n t i ta t i v e a n a l y s i s :
1

Measure a sample of which you want to quantitate a certain


component. For information about how to perform a
measurement refer to section 3.1.
Click on the Evaluate tab an then on the Quantitative Analysis
button in the OPUS wizard. Thereupon, the Quantitative Analysis
dialog window opens. See figure 38.

Spectrum file of the sample to be


analyzed (path and file name)
Path and file name of the currently loaded QUANT method
Note: Normally, it is the method
you have set up or used at last.

Click on this button if you want to


use a different QUANT method.

Figure 38: Quantitative Analysis dialog

3
4

The sample spectrum file is already included in the File(s) for


Quantitative Analysis field.
The QUANT method you have set up or used at last is already
loaded. In case you want to use a different method click on the
Load Quant Method button and select the QUANT method file
(*.q1) you intend to use.

Note: You can perform a quantitative analysis using either:

a newly set-up method or


an existing method you have modified or
an existing method you select explicitly or
the method which has been loaded last.

Make sure that the Show results immediately button is activated


(see figure 38). In this case, the result is shown immediately after
OPUS has completed the evaluation. The result is displayed in
form of a report (see figure 39).

Note: In case this check box has not been activated double-click on
the QUANT data block of the spectrum file in order to display
the quantitative analysis result.

Finally, click on the Analyze button.

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H o w t o i n t e r p r e t a q u a nt i ta t i v e a n a l y s i s r e s u l t :

Figure 39: QUANT Report - Result of a quantitative analysis

The QUANT report delivers the following information:


name of the component that has been quantitated
concentration value (prediction) of the component in question
calculated by OPUS
standard deviation (sigma1) of the calculated prediction value
unit in which the calculated concentration value is given
Note: You have specified this unit when setting up the QUANT
method.

the integration result for the spectral band which results from
the component to be quantitated.

1. Sigma is the standard deviation of the calculated concentration value. The sigma value is determined by the quality of the QUANT method you have set up. Ideally, the sigma value should
be as small as possible.
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Chapt. 4

S a m p l e P r e pa r a t i o n
Proper sample preparation is crucial to obtain good and meaningful
spectra. This chapter describes the most important sample preparation
methods1. Useful information will give you some help in selecting the
most suitable sample preparation method for a given sample.

How must the sam- homogeneous (constant concentration or composition within the
ple be like?
sample area to be analyzed)
Disadvantages of a misleading or erroneous measuring data
non-homogeneous
sample
What has to be
aggregation state of the sample
considered when
absorptivity of the sample
selecting a sample
preparation
method?
sample has to be very thin
What has to be
considered in case sample has to be diluted by a solvent or powder that is not
of a strongly
strongly absorbing
absorbing sample? (otherwise the spectrum is not meaningful)
What kind of sol Carbon tetrachloride
vents can be used? Carbon disulphide
Chloroform
Cyclohexane
Acetonitrile
Tetrachloroethylene

ALPHA allows to measure both solids and liquids. The most common
sample preparation methods include:
No sample preparation (e.g. self-supporting film or measurement using an ATR unit)
Preparing a KBr pellet (for solids)
Preparing thin film of liquid sample solution between two transparent plates (for liquids)
Caution: Most of the described sample preparation methods involve
the use of hygroscopic materials (such as NaCl or KBr). If
these materials come in contact with water or alcoholic solvents, they begin to dissolve or become cloudy and thus,
impair the measurement results. Therefore, avoid all
sources of water and even alcohol (ethanol and methanol).
1. For more detailed information about the different sample preparation methods refer to the relevant specialist literature.
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Chapt. 4

Sample Preparation

4.1

Type of sample

films and polymers (with a thickness of less than approx. 100m)

Advantage

enables fast sample measurements

Disadvantage

sometimes the samples are too thick

Tip

A large number of solid and liquid samples can also be analyzed


by using an ATR unit. In this case a sample preparation is not
required either.

4.2

42

N o Sample Preparation

K Br Pellet

Type of sample

solids

Advantages

meaningful IR spectrum
KBr shows no absorption in the wavenumber area 4000cm-1 to
250cm-1
this prevents the sample spectrum from containing any disturbing absorption bands

Disadvantages

time-consuming sample preparation method


interference of water bands (3,960 to 3,480cm-1 and 1,950 to
1,300cm-1 and below 500cm-1)
in same cases there may be structural changes caused by high
pressure applied to the KBr/sample mixture

What has to be
considered during
sample preparation?

grind the sample as fine as possible to minimize 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 60C

Tip

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).

ALPHA User Manual

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Thin film between two plates

4.3

Chapt. 4

Thin film between two plates

Type of sample

liquids (e.g. oils)

Advantages

easy sample preparation method


small amount of sample material required

Disadvantages

not suitable for samples which include water


the material of the plates (NaCl or KBr) are extremely moisture
sensitive
frequently there are air bubbles between the plates

What has to be
considered 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

Tips

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 use

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Chapt. 4

44

Sample Preparation

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Chapt. 5

Tr a n s m i s s i o n M e a s u ring
5.1

General Information

To perform transmission measurements the ALPHA-T module is


available, see chapter 5.2. More information on the principle of
transmission measurements is provided in the glossary in appendix D.

M e a s u r i n g i n t r a n s m i s s i o n i s s u i t e d f o r t h e f o llowing samples:
Solids, in the form of powder as well (except for highly absorbing substances)
Liquids
Gases
Depending on the sample material, sample preparation can be very
complex in case of measuring in transmission mode, see chapter 4.

A d v a n ta g e s :
Almost all kinds of samples can be analyzed.
Measurement represents the entire sample.

D i s a d v a n ta g e s :
Depending on the sample material a complex and sometimes
difficult 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 sample.
Too much a sample quantity can cause total absorption.
Additional accessories (e.g. liquid and gas cells) are required.

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Chapt. 5

Transmission Measuring

5.2

A LPHA-T

The ALPHA-T measurement module is designed for measurements in


transmission. This measurement module allows to spectroscopically
analyze both solids, liquids as well as gases.

B
C

Figure 40: ALPHA-T

Definition

46

Sample compartment lid

Sample holder

Ports for the IR beam passing the sample compartment

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Positioning sample in the ALPHA-T sample compartment

5.3

Chapt. 5

Positioning sample in the


ALPHA-T sample compartment

Depending on the type of sample used (solid, liquid or gas) you can
position the sample into the ALPHA-T sample compartment by means of
different measurement accessories:
sample holder supplied by default; especially suited for KBr
pellets or a thin film between two IR-transparent plates
plastic film holder (optional)
liquid cell (optional)
gas cell (optional)

5.3.1

Sample Holder

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.

Fixture

Sample holder

Figure 41: ALPHA-T - Sample compartment

5.3.2

Plastic Film Holder

The plastic film holder is put into the fixture of the sample holder
(figure 41).

5.3.3

Liquid Cell

To spectroscopically analyze liquid samples optional liquid cells are


available. The liquid cells are inserted into the sample holder (see
chapter 5.3.1) supplied by default.

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Chapt. 5

Transmission Measuring

When 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.
Note: 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.

5.3.4

Gas Cell

To spectroscopically analyze gaseous samples optional gas cells are


available. The gas cell (B in figure 42) is supplied with a special gas cell
holder (A in figure 42).
A

Figure 42: Delivery content in case of a gas cell

To insert the gas cell into the ALPHA-T sample compartment you first
have to displace the sample holder in the sample compartment, see
figure 43a and b.

Figure 43: a) Standard position of sample holder

48

b) Right sample holder position (for gas cell)

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Positioning sample in the ALPHA-T sample compartment

Chapt. 5

To d i s p l a c e t h e s a m p l e h ol d e r i n t h e A L P H A - T
s a m p l e c o m pa r t m e n t . . .
1
2
3

...you have to use the supplied TORX screw driver TX20.


Lift up the sample compartment lid.
Remove the detachable blue casing at the front side of the sample compartment, see figure 44.

TORX screw

Detachable casing

Figure 44: Removing the casing at the front of the sample compartment

4
5
6

Loosen the two TORX screws which fix the sample holder, see
figure 44.
Mount the sample holder into the right position, see figure 43b.
Put the detachable blue casing to the front of the sample compartment again.

To i n s e r t t h e g a s c e l l i n t o t h e s a m p l e c o m pa r tment...
1
2

...put the special gas cell holder into the fixture of the sample
holder, see figure 45a.
Position the gas cell on the sample holder as shown in figure 45b.

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Chapt. 5

Transmission Measuring

Figure 45: a) Insert gas cell holder

5.4

b) Gas cell on sample holder

Measuring Sample

Use the OPUS software to measure the sample. Information on


measuring the sample can be obtained from the Quick User Guide in
chapter 3. For detailed information on the OPUS software refer to the
OPUS/MENTOR manual.
As OPUS automatically recognizes the measurement module you work
with, the software can automatically load the right experiment file
supplied (i.e. Trans.XPM in case of transmission measurement). Thus,
you can immediately start to measure.
The experiment file supplied includes the default parameters set by
Bruker. These parameters allow to perform a transmission
measurement. For information on how to set up measurement
parameters refer to the OPUS/MENTOR manual.
Note: Keep the sample compartment closed during measurement.

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Chapt. 6

AT R M e a s u r i n g
6.1

General Information

ATR is the abbreviation of Attenuated Total Reflection. To perform ATR


measurements three different modules are available, see chapter 6.2.
For more information on the principle of ATR measurements refer to the
glossary in appendix D.

M e a s u r i n g i n AT R i s s u i t e d f o r t h e f o l l o w i n g
sample type:

Liquid
Powder
Paste
Gel and cream
Polymer film
Surface coating

A d v a n ta g e s :
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 measurement

D i s a d v a n ta g e s :
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.

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Chapt. 6

ATR Measuring

6.2
6.2.1

ATR Measurement Module


Overview

To perform ATR measurements by using ALPHA, the following ATR


modules are available:
ALPHA-E
ALPHA-P
ALPHA-P High Pressure variant

Figure 46: a) ALPHA-E

b) ALPHA-P

c) ALPHA-P High Pressure variant

These modules differ from each other in the following technical features:

ATR-Module

Crystal material
available

Actual sampling
Moving pressure arm by
surface on ATR crystal means of a

ALPHA-E

Ge, ZnSe

5mm

knob

ALPHA-P

Diamond, Ge

Diamond:2 x 2mm
Ge: 2mm

lever

ALPHA-P
High Pressure
option

Diamond

2 x 2mm

knob

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ATR Measurement Module

6.2.2

Chapt. 6

AT R C r y s ta l Ty p e s

The crystal types available have the following technical features:

Spectral range (cm-1)

Crystal type

To be used for

Diamond

all kinds of sample material, includ- covers the complete


ing hard and sharp-edged samples spectral range specified for ALPHA, see
appendix A

Ge (Germanium) samples with a high absorptivity,


especially carbon-filled samples
(e.g. O-rings, polymer)
ZnSe (Zinc
Selenide)
CAUTION TOXIC!

5,000 - 550

all kinds of sample material, except >500


for acids (pH -value <5) and bases
(pH-value >8) and sharp-edged
samples

Refraction index
n = 2.43

n = 4.01

n = 2.43

Caution: Zinc selenide is a toxic material. During normal spectrometer operation the material does not pose a health risk. Be
careful, however, if the crystal is broken. Avoid generating
dust. The dust is harmful by inhalation, ingestion or skin
absorption.

6.2.3

E x c h a n g i n g AT R C r y s ta l P l a t e

The ATR crystal plates can include one of the following crystal material:
ZnSe, Ge and diamond. The color of the crystal indicates which crystal
material is used.

Crystal material

Crystal color

Diamond

transparent

Ge (Germanium)

silver-gray

ZnSe (Zinc selenide)

yellow

It is not easy to rotate the crystal plate manually. Therefore, it is


recommended to use the stick supplied. The leverage effect of the stick
facilitates rotating the crystal plate.

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Chapt. 6

ATR Measuring

Put the stick into the bore of the crystal plate, see figure 47.

Rotating counterclockwise
releases the crystal plate

Rotating clockwise locks the


crystal plate
Figure 47: Exchanging crystal plate

2
3
4
5
6

Rotate the crystal plate counterclockwise by means of the pin as


far as it will go (approx. 20).
Remove the crystal plate.
Place the new plate onto the ATR measurement module and put
the pin into bore of the crystal plate.
The stick helps to tighten the crystal plate again, by rotating the
plate clockwise as far as it will go.
Remove the pin from the crystal plate bore.

6.2.4

Moving Pressure Application Device

Depending on the measurement module used the pressure application


device can be moved in different ways.

ALPHA-E
The pressure application device is moved upwards or downwards by
means of a knob (figure 48):
upwards - you have to rotate the knob counterclockwise
downwards - you have to rotate the knob clockwise
The inner part of the pressure arm is equipped with a slip-clutch
mechanism which is activated as soon as the optimal contact pressure
between sample 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.
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ATR Measurement Module

Chapt. 6

However, the contact pressure actually applied (i.e. how much the anvil
presses the sample against the ATR crystal) depends on how far you
rotate the pressure arm down.

Knob

Pressure arm
Anvil

Figure 48: ALPHA-E - Pressure application device

You can swing away the pressure arm and the anvil from the sampling
surface. The pressure arm is rotatable by 360. If you swing the
pressure arm towards the sampling surface again, it snaps into place
exactly above the ATR crystal.

ALPHA-P
The pressure application device is moved upwards or downwards by
means of a lever (figure 49).
lever in back position - moves the anvil up
lever in front position - moves the anvil down
Lever to move the anvil
Height adjusting knob to move the complete pressure application device
Red control spot indicates optimal contact pressure
Anvil

Figure 49: ALPHA-P - Pressure application device

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Chapt. 6

ATR Measuring

The optimal contact pressure applied on the sample is ensured if the red
control spot (figure 50) is exactly in the middle of the round recess.

The red spot in the middle of the round recess


indicates an optimal contact pressure applied on
the sample.

Figure 50: ALPHA-P - Indication of the optimal contact pressure

To a d j u s t t h e h e i g h t o f t h e c o m p l e t e p r e s s u r e
application device is required if...
1

56

...the lever is right in the front position but the anvil has not any
contact with the sample. In this case use the height adjusting
knob (see figure 51) and move the complete pressure application
device downwards until the red control spot is exactly in the
middle of the round recess.
You cannot move the lever right to the front position as the sample is too thick. In this case use the height adjusting knob (see
figure 51) and move the complete pressure application device
upwards, until the lever can be moved right to the front position
and the red control spot is exactly in the middle of the round
recess.

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Bruker Optik GmbH

Performing Cleanness Test

Chapt. 6

Turning the height adjusting


knob to the right, moves the
complete pressure application
device downwards.
Turning the height adjusting
knob to the left, moves the complete pressure application device
upwards.

Figure 51: ALPHA-P - Height adjustment knob

You can swing away the pressure application device from the sampling
surface. The pressure application device is rotatable by 360. If you
swing the pressure application device towards the sampling surface
again, it snaps into place exactly above the ATR crystal.
Note: For ALPHA-P as High-Pressure option refer to ALPHA-E.

6.3

Performing Cleanness Te st

Before you start measuring perform a cleanness test by means of the


OPUS software. This kind of test is a reference measurement of the ATR
crystal and defines the maximum allowed limit of the crystal
contamination. For further details refer to the OPUS/MENTOR manual.

6.4

Placing Sample on ATR Crystal


1
2

Make sure that the sampling surface, ATR crystal and anvil are
clean, see chapter 6.6.
Place the sample on the middle of the sampling surface. Use a
small amount of sample, only enough to cover the ATR crystal.

Caution: When using flammable and/or explosive materials, always


wear eye protection and use a very small amount of the
material. In case of extremely volatile materials do not
inhale the vapor and observe the safety requirements.

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Chapt. 6

ATR Measuring

Note: If the sample cannot be placed onto the ATR crystal as the distance between the ATR crystal and anvil is too small, move the
pressure application device upwards (see chapter 6.2.4).

4
5

Press the anvil against the sample (see chapter 6.2.4). Make sure
that the optimum contact pressure is used to press the sample
against the ATR crystal.
Acquire a sample spectrum (see chapter 6.5). For detailed information to perform a measurement refer to chapter 3.
Move the pressure application device up again and remove the
sample.

Note: Samples should not be left in contact with the crystal for an
extended period of time as some samples may degrade the
crystal material, and discoloration of the metal plate may
occur. Once the measurement has been made, remove the
sample from the crystal.

6.5

Thoroughly clean the sampling surface, ATR crystal and anvil


(see chapter 6.6).

M easuring Sample

Use the OPUS software to measure the sample. Information on


measuring the sample can be obtained from the Quick User Guide in
chapter 3. For detailed information on the OPUS software refer to the
OPUS/MENTOR manual.
As OPUS automatically recognizes the measurement module and the
ATR crystal you work with, the software can automatically load the right
experiment file supplied. Thus, you can immediately start to measure.
Depending on the ATR crystal used, the following experiment files are
supplied:
ATR_Di.XPM
ATR_Ge.XPM
ATR_ZnSE.XPM
The experiment files supplied include the default parameters set by
Bruker. These parameters allow to perform an ATR measurement. For
information on how to set up measurement parameters refer to the
OPUS/MENTOR manual.

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Cleaning ATR Module

6.6

Chapt. 6

C leaning ATR Module

When performing one measurement after the other it is important to


clean all remains of the previous sample from the sampling surface and
crystal, as well as from the anvil. Otherwise, you may get falsified
measurement results.

C l e a n i n g s o l v e n ts :
Alcohol
Acetone
Note: When using solvents inspect the materials safety data sheets
associated with the solvents you are using and observe any
recommended handling procedure.

The solvent used for cleaning depends on the sample that has been
analyzed. In all cases it is best to try to clean the sampling surface by the
mildest solvent possible.

Before cleaning...
...swing away the pressure application device from the sampling surface.

When cleaning...

...apply the solvent to the ATR sampling surface using a Q-tip.


Gently remove the solvent using a Q-tip or lint-free cloth.
Clean the anvil as well.
Repeat the cleaning procedure until all sample remains have
been removed.
Caution: Never use caustic or abrasive substances or strong acids.
These substances can damage the ATR sampling surface.
Never rub with paper products as they may be abrasive and
could cause scratches on the crystal surface, especially
with Ge and ZnSe.

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Chapt. 6

ATR Measuring

6.7

ATR Sp ectra

Similar to transmission spectra


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.
Intensity
Is related to the penetration depth of the evanescent wave into
the sample. This depth depends on the refractive index of the
crystal and sample, and on the wavelength of the IR radiation.
Main benefit
The relatively thin depth of penetration of the IR beam into the
sample creates the main benefit of ATR sampling. This is in
contrast to traditional FT-IR sampling by transmission where
the sample must be diluted with IR transparent salt, pressed
into a pellet or pressed to a thin film, prior to analysis to prevent totally absorbing IR bands.

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Chapt. 7

M a i n t e n a n c e & R e pa i r
ALPHA is a low-maintenance instrument, i.e. the operator can replace
components with a limited service life (e.g. IR source). The following
maintenance procedures are described in this chapter:

Replacing IR source
Replacing desiccant
Replacing windows
Cleaning windows
Cleaning spectrometer housing

General Instructions
Perform only the maintenance procedures described in this manual.
Strictly observe the relevant safety precautions. Any failure to do so may
cause property damage or personal injury. In this particular case Bruker
does not assume any liability. Maintenance or repair procedures not
described in this manual should only be performed by a Bruker service
engineer. For service assistance, see appendix E.
Depending on the degree of hazard the safety instructions to be
observed in case of spectrometer maintenance or repair are classified
as follows:
Caution

indicates that minor personal injury or property damage


CAN result if proper precautions are not taken.

Note

draws your attention to particularly important information


on the product, or to the product operation.

The safety instruction Caution is indicated by triangular warning label.

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Chapt. 7

Maintenance & Repair

7.1

Replacing IR Source

ALPHA is equipped with a highly-efficient, low-power, air-cooled infrared


source.

When do you have to replace the IR source?


The average IR source lifetime is specified with about 44.000 operating
hours. Before this period has been expired the following message pops
up in OPUS: End of average lifetime is nearly reached, spare part will be
required. In this case the OPUS status light (
status light allows to continue measuring.

) is yellow. A yellow

Order a replacement source (order no: 1005855). As soon as you have


received the replacement, the existing source should be replaced.
Note: To allow the status light become green again, you have to click
on the Ignore button in the Instrument Status Message dialog
(see figure 65 on page 76).
The End of average lifetime is nearly reached, spare part will
be required message will be displayed in regular intervals.

If the source is defective, the OPUS status light becomes red. The
following message pops up in OPUS: Source is broken. A red status
light does not allow to continue measuring. The source must be
replaced.

How do you have to replace the IR source?

1
2
3

62

Switch off the power plug.


The source is accessible from the rear side of the spectrometer.
Make sure that you have access to the rear side.
Remove the cover plate at the rear side by loosening the 4 TORX
screws (A in figure 52). To loosen the screws use the TORX TX20
screw driver supplied.
Take off the cover plate.

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Replacing IR Source

Chapt. 7

Figure 52: ALPHA rear side - Removing cover plate

Note: During spectrometer operation the light source becomes very


hot. Wait until the light source has cooled down sufficiently
before you begin to replace it. In case of non-observance
there is the risk of skin burn!

5
6

Loosen the two fixing screws of the IR source (see figure 53). Use
the TORX TX20 screw driver supplied.
Strip off the green source plug (see figure 53). There will be a
beep.

IR source

Fixing screws
of the source
(TORX
screws)

Source plug

Figure 53: ALPHA rear side - Removing source

7
8

Pull out the source from the spectrometer housing.


Insert the new IR source into the spectrometer housing. Make
sure that the alignment pin (A in figure 54) correctly fits in the
alignment groove (B in figure 54).

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Chapt. 7

Maintenance & Repair

B
A

Figure 54: ALPHA - Exact positioning of source

9 Fix the source by fastening the two TORX screws (see figure 53).
10 Put the green source plug into the SRC female connector. There
will be a beep.
11 Attach the cover plate and fasten the 4 TORX screws again (see
figure 52).
12 Connect the power plug to the mains socket again.

A ft e r r e p l a c i n g t h e I R s o u r c e . . .
...you have to perform an instrument test.

To p e r f o r m a n i n s t r u m e n t t e s t . . .
1
2
3

64

...click on the Instrument Test button on the OPUS wizard (see


figure 55). The test starts and takes about 5 minutes.
Wait until the test has finished.
If the test has passed, the OPUS status light is green. If the instrument has failed, see chapter 8.

ALPHA User Manual

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Replacing Desiccant Bags

Chapt. 7

Figure 55: Starting instrument test by the OPUS wizard

Resetting source operating hour meter


1
2
3
4

7.2

Click on the OPUS status light (


).
The Instrument Status dialog opens.
Click on the Source Icon. Another dialog opens.
Click on the Reset button of this dialog. If the Reset button is
deactivated, click on the Help button first.

Rep l aci n g D e s ic c a n t B a g s

Too high a humidity inside the spectrometer can be recognized by H2O


bands in the spectrum. As the desiccant inside the spectrometer binds
humidity, H2O bands in the spectrum can be reduced to a minimum.
The air inside the complete ALPHA optics unit (measuring and optics
compartment) is convectively kept dry using a desiccant which is
enclosed in removable small bags.

When do you have to replace the desiccant


bags?
If 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 OPUS.
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Chapt. 7

Maintenance & Repair

Besides, the OPUS status light (


) becomes yellow. Order new
desiccant (order no: 1000917). 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.

How do you have to replace the desiccant


bags?

1
2
3

Switch off the power plug.


The desiccant bags are accessible from the rear side of the spectrometer. Make sure that you have access to the rear side.
Remove the cover plate at the rear side by loosening the 4 TORX
screws (A in figure 56). To loosen the screws use the TORX TX20
screw driver supplied.
Take off the cover plate.
A

Figure 56: ALPHA rear side - Removing cover plate

66

Pull out the used desiccant bags. A pair of tweezers may be helpful.

ALPHA User Manual

Bruker Optik GmbH

Replacing Windows

Chapt. 7

Desiccant
bags

Figure 57: ALPHA rear side - Replacing desiccant bags

The replacement desiccant bags are protected by an extra packaging. Open this packaging and take out the desiccant bags.
Note: Alternatively, you can place the spent bags into an
oven at 130C for at least 10 minutes.
Completely insert the desiccant bags properly into the spectrometer as shown in figure 57.

Caution: Do not cut or tear off the bags into single pieces, nor ingest
the desiccant.

8
9

7.3

Attach the cover plate and fasten the 4 TORX screws again (see
figure 56).
Connect the power plug to the mains socket again.

R eplacing Windows

The ALPHA basic module has two ports: one IR output and one IR input
port (see figure 58). The IR beam enters the measurement module by
the IR output port. Afterwards, the beam is directed to the basic module
again via the IR input port. The ports are closed by means of
exchangeable IR transparent windows.
Note: By default, the spectrometer is equipped with KBr windows. In
case of the High Humidity option the windows are made of
ZnSe.
Caution: Zinc selenide is a toxic material. During normal spectrometer operation the material does not pose a health risk. Be
careful, however, if a window is broken. Avoid generating
dust. The dust is harmful by inhalation, ingestion or skin
absorption.

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Maintenance & Repair

Ports closed by KBr windows

Basic module

Exchangeable
measurement
module

Figure 58: Window position

When do you have to replace the windows?


KBr is a hygroscopic window material which causes the spectrometer
windows to become opaque in the course of time. Opaque windows
substantially reduce infrared transmittance which can be indicated by a
failed performance or instrument test. In this case you have to replace
the windows.
ZnSe windows, however, only need to be replaced when they are
broken.

How to replace the windows?


1

2
3
4

68

Remove the basic module from the measurement module by


pressing the lock on the basic module right down. Pull out the
measurement module from the basic module, towards your
direction (see chapter 2.6).
To remove the windows use the assembly tool supplied.
Insert the two pins of the assembly tool into the respective holes
on the window frame (see figure 59).
Rotate the tool several turns counterclockwise and pull out the
tool including the window assembly (i.e. window and assembly
frame).
Insert the two pins of the assembly tool into the respective holes
of the assembly frame on the new window. Put the window
assembly into the hole of the basic module.
To fasten the window assembly rotate the tool several turns clockwise.

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Replacing Windows

7
8

Chapt. 7

Pull out the assembly tool from the holes on the assembly frame.
After replacing the windows push the measurement module right
against the basic module. Press the lock on the basic module
again right down (see chapter 2.6).

Lock/release

Window assembly
(window in assembly frame)
Fitting
tool
to
replace windows

Figure 59: Replacing windows

A ft e r r e p l a c i n g t h e w i n d o w s . . .
...you have to perform an instrument test.

To p e r f o r m a n i n s t r u m e n t t e s t . . .
1
2
3

...click on the Instrument Test button on the OPUS wizard (see


figure 60). The test starts and takes about 5 minutes.
Wait until the test has finished.
If the test has passed, the OPUS status light is green. If the instrument has failed, see chapter 8.

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Maintenance & Repair

Figure 60: Starting instrument test by the OPUS wizard

7.4

C leaning Windows

Clean the windows by using a dry, lint-free cloth only.


Caution: KBr windows are hygroscopic. Do NOT clean them by
using water or solvents.

7.5

C leaning Spectrometer Housing

The outer spectrometer surface can be cleaned only by using a dry or


damp cloth. Do not use detergents with organic solvents, acid or base!
Caution: Do by no means clean the interior of the spectrometer. This
may lead to serious spectrometer damage.

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Chapt. 8

Tr o u ble s h o o t i n g
8.1

G en era l In fo r m a tio n

This chapter describes only those spectrometer problems and their


causes which you can solve by yourself. In all other cases contact the
Bruker service. For service addresses and telephone numbers refer to
appendix E.
A spectrometer problem can be indicated as follows:
The status light at the spectrometer top side lights yellow or
red or not at all.
The OPUS status light is yellow or red or gray.
The instrument test/performance test failed. (In this case, a
test protocol is automatically displayed.)
Error messages in OPUS
Diagnostics LEDs at the spectrometer rear side
These diagnostic means allow to find out the cause of a spectrometer
problem and to solve it by yourself, or at least to narrow down the cause
of the problem. If the solutions listed below do not solve the problem,
contact Bruker service. For this case OPUS provides the possibility to
send a complete spectrometer status report to the Bruker service for a
remote fault diagnostics. To do this, proceed as follows:
1
2

Click on the OPUS status light. The status light is in lower right
corner of the OPUS interface (see figure 62).
The Instrument Status dialog window opens. Click on the Send
Report button (see figure 63). The report is sent by e-mail to
opusreports@brukeroptics.

Note: This function requires an e-mail program installed on your


computer and a set-up mail account. In addition, your spectrometer needs to be connected to a network computer.

Alternatively, you can save the report on your computer by clicking on


the Save Report button. The report is automatically saved under the
following path: OPUS-Pfad\InstrReports\ .... The folder in question is
named after the current date and time of the storage.

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8.2

Available Diagnostic Means

Sp e c t r o m e t e r Sta t u s I n d i c a t o r
The status indicator is on the spectrometer top side.

Figure 61: ALPHA - Status Indicator

The spectrometer status indicator can have the following colors: green,
yellow and red. These colors indicate the following spectrometer status:
Green (permanent):
Spectrometer is in proper operating condition.
Green (flashing):
Spectrometer is in the stand-by mode.
Yellow:
Spectrometer is in the initialization phase or it indicates a warning (e.g. IR source has not yet reached its operating temperature, the air humidity content inside the spectrometer is too
high etc.)
Red:
Spectrometer malfunction, defective spectrometer component

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O P U S Sta t u s L i g h t
The status light is in the lower right corner of the OPUS interface.

Status
light
Figure 62: OPUS interface

The OPUS status light can have the following colors: green, yellow, red
and gray. These colors indicate the following spectrometer status:
Green (permanent):
Spectrometer is in proper operating condition.
Yellow:
Spectrometer is in the initialization phase, or a warning is indicated (e.g. IR source has not yet reached its operating temperature, the validity period of the instrument is expired, the air
humidity content inside the spectrometer is too high etc.)
Red:
Spectrometer malfunction, defective spectrometer component, performance test / instrument test failed
Gray:
In OPUS, no spectrometer is selected or the spectrometer is
off or the spectrometer is in stand-by mode.
Note: In case of a yellow status light measuring is still possible. If
the status light is red or gray, measuring is not possible.
The color of both status lights, in OPUS and on the spectrometer, corresponds in most cases except for one case: if the
performance test or the instrument test has failed the OPUS
status light is red whereas the spectrometer status indicator
lights yellow.

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Troubleshooting

O P U S I n s t r u m e n t St a t u s D i a l o g
Click on the OPUS status light (see figure 62). The Instrument Status
dialog opens.

Figure 63: Optics Diagnostics - Instrument Status dialog

A The status of the hardware components, e.g. source, laser, interferometer etc. is displayed in the upper icon line. The status can be
as follows:
OK (green):
Component is okay.

WARNING (yellow):
The exact meaning of a warning depends on the component in question. In case of the source a warning means:
End of the specified component lifetime is nearly
reached. In this case, measuring is still possible.
The source is still warming-up (duration: about 7 min.)
In this case, measuring is not possible.
ERROR (red):
Component is defective. In this case measuring is not
possible.

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B The second row of icons refer to the possible active test channel
and indicates the result of the last instrument test performed. The
results can be as follows:

INACTIVE (yellow):
The single tests of the particular test category are disabled.

PASSED (green):
Instrument test passed. Test is still valid.

EXPIRED (light blue):


Instrument test validity period has
expired.

FAILED (red):
Instrument test failed.

To p e r f o r m a f a u l t d i a g n o s i s o f a pa r t i c u l a r
hardware component...
1
2

...click on the respective icon in the first row of the Instrument


Status dialog.
The Instrument Status Message dialog opens:

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Troubleshooting

Status indication
(for the component in question)
Error message (for
the component in
question)

Component
in question

Figure 64: Instrument Status Message

When you click on the Service Info button the diagnostics page of the
component in question opens. Figure 65 shows the diagnostics page of
the source. These pages contain all relevant information about the
current operating state of the respective spectrometer component.
Note: You can send these diagnostics pages as full report to the
Bruker service by e-mail allowing the technician a first remote
fault diagnostics (see section 8.1).

Figure 65: Source Diagnostics Page

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Available Diagnostic Means

Chapt. 8

Error Messages in OPUS


Error messages concerning the spectrometer can appear in OPUS as
follows:
in the Instrument Status Message dialog (see figure 64).
in a yellow message bubble in the lower right corner of the
OPUS interface (see figure 66a).
in a normal message window (see figure 66b).

Error Message

Figure 66: a) Information bubble

b) Message window

Note: In case of a spectrometer problem indicated by an error message, the status indicator on the spectrometer and the OPUS
status light are yellow or red.

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Troubleshooting

Sp e c t r o m e t e r D i a g n o s t i c L E D s
The diagnostic LEDs are at the spectrometer rear side.

ABC
Figure 67: ALPHA rear side -Diagnostic LEDs

Type

Definition

TKD LED

The green TKD LED indicates that the interferometer mirror is


within the data acquisition range. When data acquisition actually
takes place the light intensity changes to bright green. The TKD
abbreviation means Take Data.

ACC LED

The yellow ACC LED indicates that the network accesses the
optics. During transition of measuring data the LED will be light yellow. The ACC abbreviation means Access.

DIR/ERR LED

In normal operation mode the DIR/ERR LED flashes slightly red


and indicates the scanner movement. If the LED lights permanently bright red, there must be an interferometer problem, e.g.
missing laser signal. As long as this LED lights permanently red no
data acquisition is possible. The DIR abbreviation means Direction,
ERR means Error.

P e r f o r m a n c e Te s t a n d I n s t r u m e n t Te s t
Both tests check whether the spectrometer achieves the specified
performance. But they differ as follows:

Performance Test

Instrument Test

The test procedure includes


the following tests

Signal-to-noise test
Deviation from 100% line

Signal-to-noise test
Deviation from 100% line
Wavenumber accuracy test

Number of test measurements

11

Test duration

about 1 minute

about 5 minutes

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Problem - Possible Causes - Solutions

When is the test performed?

8.3

Chapt. 8

Performance Test

Instrument Test

automatically after OPUS


has been opened again
automatically after ALPHA
has been accessed again
automatically after the
measurement module or
the ATR crystal plate has
been substituted by
another measurement
module or another ATR
crystal plate

automatically when the PC and


ALPHA communicate with each
other for the very first time
automatically when you use a measurement 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 expired; Note: The factory-set validity period is 7 days.

Problem - Possible Causes Solutions

8.3.1

A P r o b l e m i n d i c a t e d b y t h e Sp e c t r o m e t e r
Sta t u s I n d i c a t o r

The status indicator is on the spectrometer top side (see figure 61).

Sp e c t r o m e t e r s ta t u s i n d i c a t o r i s o f f
Possible Cause

Solution

Spectrometer is not connected properly to the mains supply.

Check the power cord connection at both ports, the


mains outlet and the POWER port at the spectrometer
rear side. See ALPHA Installation Instructions,
chapter 3.2.

No voltage is applied

Check whether the proper voltage is applied at the


mains outlet to which the spectrometer is connected.

Short circuit in the mains adapter of


power cable.

A short circuit is accompanied by a "ticking" sound in


the mains adapter. Unplug the power cord immediately
and contact Bruker service (see appendix E).

If the problem has a different cause... ...contact Bruker service (see appendix E).

Sp e c t r o m e t e r s ta t u s i n d i c a t o r i s y e l l o w
Possible Cause

Solution

Spectrometer is still in the initialization Wait until the spectrometer initialization is completed.
(duration: about 1 minute)
phase.
IR source has not yet reached its operating temperature.
Note: In this case the following
message appears: Device not ready.

Bruker Optik GmbH

The warm-up takes about 7 minutes. As soon as the IR


source has reached its operating temperature the status light will automatically turn green. Wait until the
warm-up has been completed.

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Troubleshooting

Possible Cause

Solution

The end of the specified lifetime of the


source is nearly reached.
Note: In this case the following
message appears: End of average
lifetime is nearly reached, spare will
be required.

Order a spare source (part no. 1005855). After the


receipt, replace the old source (see chapter 7 Repair
and Maintenance, section 7.1).
Note: Despite this message, measuring is still possible. To turn the OPUS status light green again click
on the Ignore button in the Instrument Status Message
dialog (figure 64). The message will be repeated in certain time intervals until you have replaced the source.

Performance test or instrument test


failed.

For information about the solution of this problem refer


to section 8.3.4 Performance Test failed or
section 8.3.5 Instrument Test failed.

Instrument test validity period is


expired. Note: In this case the following message appears: An instrument test is required or one of the
instrument components does not
meet its specifications.

Click on the OPUS status light (figure 62). The Instrument Status dialog (figure 63) opens. The measurement channel of which the instrument test validity
period is expired is labelled Expired.
Start a new instrument test by clicking on the Instrument Test button in the OPUS wizard. Wait until the test
is completed (duration: about 5 minutes).

Air humidity inside the spectrometer is Replace the desiccant bags (see chapter 7 Repair and
too high. Note: In this case the folMaintenance, section 7.2).
lowing message appears: Humidity
out of range.
Laser wavenumber needs to be recali- Click on the Calibrate button (figure 68) and wait until
brated. Note: In this case a correthe calibration is completed.
sponding message appears in the
lower right corner of the OPUS
interface. See fig. 68.
If the problem has a different cause...

...contact the Bruker service (see appendix E).

Figure 68: OPUS message prompting an instrument calibration

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Sp e c t r o m e t e r s ta t u s i n d i c a t o r i s r e d
Possible Cause

Solution

Defective spectrometer component

To find out which component is defective, click on the


OPUS status light (figure 62). The Instrument Status
dialog opens (figure 63). If the laser or the interferometer or the electronics or the automation or the detector
is defective, contact Bruker service. In case of a defective source, replace the old source as described in
chapter 7 Maintenance and Repair, section 7.1.

No measurement module is placed in


the basic module or the measurement
module is not locked properly in place.
In case of the ATR-module: No ATRcrystal plate is installed, or the plate is
not installed properly.

Place the measurement module into the basic module


and lock it properly in position (see chapter 2,
section 2.6). In case of an ATR-Module, install the ATRcrystal plate properly (see chapter 6, section 6.2.3).

If the problem has a different cause...

...contact Bruker service (see appendix E).

8.3.2

A P r o b l e m i n d i c a t e d b y t h e O P U S Sta t u s
Light

The OPUS status light is in the lower right corner of the OPUS interface
(see figure 62).

O P U S Sta t u s l i g h t i s y e l l o w
Possible Cause

Solution

IR source has not yet reached its operating temperature.


Note: In this case the following
message appears: Device not ready.

The warm-up takes about 7 minutes. As soon as the IR


source has reached its operating temperature the status light will automatically turn green. Wait until the
warm-up is completed.

The end of the specified lifetime of the


source is nearly reached.
Note: In this case the following
message appears: End of average
lifetime is nearly reached, spare will
be required.

Order a spare source (part no. 1005855). After the


receipt, replace the old source (see chapter 7 Repair
and Maintenance, section 7.1).
Note: Despite this message measuring is still possible. To turn the OPUS status light green again click
on the Ignore button in the Instrument Status Message
dialog (figure 64). The message will be repeated in certain time intervals until you have replaced the source.

Instrument test validity period is


expired.
Note: In this case the following
message appears: An instrument
test is required or one of the instrument components does not meet its
specifications.

Click on the OPUS status light (figure 62). The Instrument Status dialog (figure 63) opens. The measurement channel of which the instrument test validity
period is expired is labelled Expired.
Start a new instrument test by clicking on the Instrument Test button in the OPUS wizard. Wait until the test
is completed (duration: about 5 minutes).

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Troubleshooting

Possible Cause

Solution

Air humidity inside the spectrometer is Replace the desiccant bags (see chapter 7 Repair and
too high.
Maintenance, section 7.2).
Note: In this case the following
message appears: Humidity out of
range.
Laser wavenumber needs to be recali- Click on the Calibrate button (figure 68) and wait until
brated.
the calibration is completed.
Note: In this case a corresponding
message appears in the lower right
corner of the OPUS window. See
figure 68.
If the problem has a different cause...

...contact Bruker service (see appendix E).

O P U S s ta t u s l i g h t i s r e d
Possible Cause

Solution

Performance test or instrument test


failed.

For information about the solution of this problem refer


to section 8.3.4 Performance Test failed or
section 8.3.5 Instrument Test failed.

Defective spectrometer component

To find out which component is defective, click on the


OPUS status light (figure 62). The Instrument Status
dialog opens (figure 63). If the laser or the interferometer or the electronics or the automation or the detector
is defective, contact Bruker service. In case of a defective source, replace it as described in chapter 7 Maintenance and Repair, section 7.1.

If the problem has a different cause...

...contact the Bruker service (see appendix E).

O P U S s ta t u s l i g h t i s g r a y
Possible Cause

Solution

Spectrometer is still in the initialization Wait until the spectrometer initialization is completed.
phase.
(duration: about 1 minute)
For other possible causes...

...refer to the above section 8.3.1 Spectrometer Status


Lamp does not light.

The OPUS status light is gray while the spectrometer status light has
one of the three possible colors. This state indicates a communication
problem between ALPHA and the PC. This problem can be caused by:

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Problem - Possible Causes - Solutions

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Possible Cause

Solution

The IP address of the ALPHA spectrometer is not selected in OPUS or


the wrong IP address has been
selected.

Enter the correct spectrometer IP address in OPUS. To


do this, select in the OPUS Validation menu the Optic
Setup and Service command. The Optic Setup and
Service dialog opens. Select the Alpha option in the
Configuration drop-down list and enter the spectrometer IP address (by default 10.10.0.1) into the field below
(Optical Bench URL). See figure 69.

Spectrometer is not connected to the


computer.

Connect the spectrometer to the computer using the


supplied data cable (crossover, Cat-5). See Installation
Instructions, chapter 3.

The spectrometer is connected to the


PC using the wrong cable type.

Connect the spectrometer to the PC using only the supplied cross-over, Cat5-cable. See Installation Instructions, chapter 3.

The RJ45-plug(s) of the data cable has Check the data cable cord connection at both RJ45(have) not been connected properly.
ports, the ETH/LAN port at the spectrometer rear side
and the Network/LAN port of the PC. See Installation
Instructions, section 3.2.
The factory-set standard IP address of Reassign the standard IP address to the spectrometer
the spectrometer (10.10.0.1) has been using the DIP-switch at the spectrometer rear side. See
changed.
Installation Instructions, chapter 6, section Assigning
the standard IP address using the DIP switch.
Spectrometer is in stand-by mode. In
this case, the status light on the spectrometer top side flashes green.

Deactivate the stand-by mode by pressing the SBY/


RES button at the spectrometer rear side shortly (about
1 sec.). See chapter 2, section 2.8.

Spectrometer
IP address

Figure 69: Entering the Spectrometer IP Address in OPUS

Checking the Communication Connection


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Troubleshooting

between ALPHA and PC


To check the communication connection you can use either the Internet
Explorer provided as part of Windows or any other internet browser
program installed on your PC. Proceed as follows:
1
2

Open the internet browser.


Make sure that the internet browser is not in the offline mode. In
case of the Microsoft Internet Explorer, the offline mode is indicated by a tick in front of the Offline Mode command in the File
menu of the browser.
Make sure that the internet browser does not use a proxy server,
at least, for addresses of direct access in the 10.10.x.x-range. In
case of the Microsoft Internet Explorer, you can check this by
selecting the Internet Options command in the Extra browser
menu. Click on the Connections tab. Then, click on the Settings
button in the LAN-Settings group field.
Enter the standard spectrometer IP address in the corresponding
browser entry field as follows: http://10.10.0.1/diag.htm. Then,
press the Enter button.
Now, the Internet Explorer should display the diagnostics page of
your ALPHA spectrometer (see figure 70). If, however, the Internet Explorer displays a blank page and is not able to access the
ALPHA diagnostics page a wrong spectrometer IP address is the
cause of the problem
Close the internet browser.

Figure 70: Diagnostics page of the ALPHA spectrometer

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Problem - Possible Causes - Solutions

8.3.3

Chapt. 8

P e r f o r m a n c e t e s t d o e s n o t s ta r t a u t omatically

Normally, the performance test starts automatically after OPUS has


been opened again, after ALPHA has been accessed again or after the
measurement module or the ATR crystal plate has been exchanged. If
the performance test does not start automatically, the following problems
may exist:
Possible Cause

Solution

No measurement module is placed Snap the measurement module correctly into place
in the basic module, or the measure- (see also chapter 2, section 2.6).
ment module is not snapped properly in place.
No ATR-crystal plate is installed or
not installed properly.

8.3.4

Install the ATR-crystal plate properly (see chapter 6,


section 6.2.3).

P e r f o r m a n c e Te s t f a i l e d

The performance test procedure comprises the following tests:


Signal-to-noise test
100% line test
If the performance test failed, an OVP - PQ Test Protocol (as pdf file)
appears automatically. The pdf files with the PQ test protocol are saved
automatically under OPUS path\Validation\Reports.

Figure 71: Test protocol of a failed performance test

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Troubleshooting

Possible Cause

Solution

As the performance test performs


only one measurement, this test
may fail under certain circumstances without a spectrometer
problem or malfunction.

In this case we recommend to perform an instrument


test which will normally be passed. To do this, click on
the Instrument Test button in the OPUS wizard and wait
until the test is completed (duration: about 5 minutes).
If this measure does not solve the problem and the
instrument test fails as well, see the following
section 8.3.5.

Ensure that the spectrometer is not exposed to strong


During the performance test, the
spectrometer was exposed to strong vibrations and perform an instrument test. To do this,
vibrations.
click on the Instrument Test button in the OPUS wizard
and wait until the test is completed (duration: about 5
minutes).
The ambient temperature is too low
so that the warm-up of 7 minutes
was not sufficient.

Wait until the source has reached its operating temperature. Then, perform an instrument test by clicking on
the Instrument Test button in the OPUS wizard. Wait
until the test is completed (duration: about 5 minutes).

Transmission module: There is a


Remove the sample or object. Then, perform an instrusample or another object in the sam- ment test by clicking on the Instrument Test button in
the OPUS wizard. Wait until the test is completed
ple compartment.
(duration: about 5 minutes).
ATR module: ATR crystal is dirty or
there is a sample on the ATR crystal.

8.3.5

Remove the sample or clean the ATR crystal (see


chapter 6, section 6.6). Then, perform an instrument
test by clicking on the Instrument Test button in the
OPUS wizard. Wait until the test is completed (duration:
about 5 minutes).

I n s t r u m e n t Te s t f a i l e d

The instrument test procedure comprises the following tests:


Signal-to-noise test
100% line test
Wavenumber accuracy test
In case the instrument test failed an OVP - PQ Test Protocol (as pdf file)
appears automatically. The pdf files with the PQ test protocol are saved
automatically under OPUS path\Validation\Reports.

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Problem - Possible Causes - Solutions

Chapt. 8

Figure 72: Test Protocol of a failed Instrument Test

A l l t h r e e t e s ts f a i l e d
Possible Cause

Solution

Defective spectrometer component

To find out which component is defective, click on the


OPUS status light (figure 62). The Instrument Status
dialog opens (figure 63). If the laser or the interferometer or the electronics or the automation or the detector
is defective, contact Bruker service. In case of a defective source, replace the source as described in
chapter 7 Maintenance and Repair, section 7.1.

A l l t h r e e t e s ts o r o n l y t h e s i g n a l - t o - n o i s e - t e s t
or only the 100%-line test failed
Possible Cause

Solution

Transmission measurement module:


The IR beam has been obstructed by
an object (e.g. sample) in the spectrometer sample compartment.

Remove the object and repeat the instrument test by


clicking on the button Instrument Test in the OPUS wizard.

In case of an ATR module: No ATRcrystal plate is installed or is not


installed properly.

Install the ATR-crystal plate properly (see chapter 6,


section 6.2.3).

ATR crystal is dirty.

Clean the crystal (see chapter 6, section 6.6).

ATR crystal is damaged.

Order a new crystal plate with the corresponding ATRcrystal material. After receipt, replace the crystal plate
(see chapter 6, section 6.2.3).

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Troubleshooting

Possible Cause

Solution

In the course of time, the hygroscopic


KBr windows have become opaque to
such a degree that the infrared transparency is seriously reduced.

Order new KBr windows (part no.: 1005847). After the


receipt of the spare windows replace the existing windows. See chapter 7 Maintenance and Repair,
section 7.3.

If the problem has a different cause...

...contact the Bruker service (see appendix E).

Only the wavenumber accuracy test failed


Possible Cause

Solution

Laser wavenumber needs to be recali- Select the Setup Instrument Test command in the Valibrated.
dation menu. Click on the Measure LWN button in the
Setup OPV dialog.
If the problem has a different cause...

8.3.6

...contact the Bruker service (see appendix E).

A Sp e c t r o m e t e r P r o b l e m i n d i c a t e d b y a n
Error Message in OPUS

Error Message in OPUS

Possible Cause

Solution

Device not ready.

IR source has not yet


Wait until the warm-up is completed. It
reached its operating tem- takes about 7 minutes.
perature.

End of average lifetime is The end of the specified


nearly reached, spare
lifetime of the source is
part will be required.
nearly reached.

Order a spare source (part no. 1005855).


After the receipt, replace the old source
(see chapter 7 Repair and Maintenance,
section 7.1).
Note: Despite this message measuring is still possible. To turn the OPUS
status light green again click on the
Ignore button in the Instrument Status
Message dialog (figure 64). The message will be repeated in certain time
intervals until you have replaced the
source.

Source is broken.

IR source is defect.

Order a spare source (part no.:


1005855). After receipt, replace the old
source as described in chapter 7 Maintenance and Repair, section 7.1.

Source is not connected

When you have replaced


the IR source, the plug of
the IR source is not connected at all or not connected properly.

Connect the source correctly (see


chapter 7, Maintenance and Repair,
section 7.1.

No accessory connected. There is no measurement Place the measurement module in the


module connected to the basic module and lock it properly in posibasic spectrometer mod- tion (see chapter 2, section 2.6).
ule.

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Problem - Possible Causes - Solutions

Chapt. 8

Error Message in OPUS

Possible Cause

Front sample not connected.

This message can appear Install the ATR-crystal plate properly


only in case you work with (see chapter 6, section 6.2.3).
an ATR module and no
ATR crystal plate is
installed or it is not
installed properly.

Standby mode activated.

The spectrometer is in
stand-by mode.

Deactivate the stand-by mode by pressing the SBY/RES button for about 1 second. This button is at the spectrometer
rear side (see chapter 2, section 2.8).

Humidity out of range.

Air humidity inside the


spectrometer is too high.

Replace the desiccant bags. See


chapter 7 Repair and Maintenance,
section 7.2.

Temperature out of range. Temperature inside the


spectrometer is too high.
Cause: Ambient temperature is too high.

Solution

Operate the spectrometer only in the


ambient temperature range specified by
the manufacturer.
Specified temperature range: 18 - 35C.
(64 - 95F)

An instrument calibration
is required. ...

Note: This message


Click on the Calibrate button (figure 68)
appears every six
and wait until the calibration is commonths. It is factory-set. pleted.
The purpose of a regular
recalibration is to ensure
that the measurements
are performed with a correctly set laser wavenumber.

Wrong accessory
inserted, unable to run
OVP tests.
Can not run OVP tests,
please check OVP Setup.

You use two different


Make sure that the measurement module
measurement modules. If defined in the planer and the actually
you start the instrument
connected module are the same.
test automatically by the
OPUS planer you have to
define the module. If the
defined module is not connected to the spectrometer these error messages
appear.

Wrong accessory
inserted, unable to run
OVP tests.
Can not run OVP tests,
please check OVP Setup.

In case of a manual test


start: the actually connected measurement
module and the selected
test channel in OPUS are
different.

If an error message
appears which is not
listed above...

Bruker Optik GmbH

Either connect the right measurement


module or select the right test channel in
OPUS. To do this, select the Setup
Instrument Test command in the Validation menu. Select the correct test channel in the Setup OPV dialog. Note: The
actually connected module and the
selected test channel have to be the
same.
...contact Bruker service (see
appendix E).

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89

Chapt. 8

Troubleshooting

8.3.7

A problem indicated by the spectrometer


diagnostic LEDs

The diagnostic LEDs are at the spectrometer rear side (see figure 67).

N o L E D l i g h ts
Possible Cause

Solution

Spectrometer is not connected properly to the mains supply.

Check the power cord connection at both ports, the


mains outlet and the POWER port at the spectrometer
rear side. See ALPHA Installation Instructions.

No voltage is applied

Check whether the proper voltage is applied at the


mains outlet to which the spectrometer is connected.

Short circuit in the mains adapter of


power cable.

A short circuit is accompanied by a "ticking" sound in


the mains adapter. Unplug the power cord immediately
and contact Bruker service (see appendix E).

The yellow ACC LED does not light at all


A permanent dark ACC LED indicates that there is no communication
between the spectrometer and the computer.
Possible Cause

Solution

Spectrometer is not connected to the


computer.

Connect the spectrometer to the computer using the


supplied data cable (crossover, Cat-5). See Installation
Instructions, chapter 3.

The spectrometer is connected to the


PC using the wrong cable type.

Connect the spectrometer to the PC using only the supplied cross-over, Cat5-cable. See Installation Instructions, chapter 3.

The RJ45-plug(s) of the data cable has Check the data cable cord connection at both RJ45(have) not been connected properly.
ports, the ETH/LAN port at the spectrometer rear side
and the Network/LAN port of the PC. See Installation
Instructions, chapter 3 section 3.2.
The IP address of the ALPHA spectrometer is not selected in OPUS or
the wrong IP address has been
selected.

Enter the correct spectrometer IP address in OPUS. To


do this, select the Optic Setup and Service command in
the OPUS Validation menu. The Optic Setup and Service dialog opens. Select the Alpha option in the Configuration drop-down list and enter the spectrometer IP
address (by default 10.10.0.1) into the field below
(Optical Bench URL). See figure 69.

The factory-set standard IP address of Reassign the standard IP address to the spectrometer
the spectrometer (10.10.0.1) has been using the DIP-switch at the spectrometer rear side. See
changed.
Installation Instructions, chapter 6, section Assigning
the standard IP address using the DIP switch.

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Problem - Possible Causes - Solutions

Chapt. 8

Possible Cause

Solution

Spectrometer is in stand-by mode. In


this case, the status indicator on the
spectrometer top side flashes green.

Deactivate the stand-by mode by pressing the SBY/


RES button at the spectrometer rear side shortly (about
1 sec.). See chapter 2, section 2.8.

T h e r e d E R R L E D l i g h ts p e r m a n e n t l y
A permanent red ERR LED indicates an interferometer and/or laser
problem.
Note: During a trouble-free spectrometer operation, this red LED
flashes in the rhythm of the scanner movement.
Possible Cause

Solution

A spectrometer problem caused by


the laser and/or interferometer.

Contact Bruker service (see appendix E).

Strong vibrations or other strong


Put the spectrometer on a vibration-free surface. If this
mechanical impacts on the spectrom- measure does not solve the problem, contact Bruker
eter which impair the spectrometer
service (see appendix E).
operation

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Chapt. 8

92

Troubleshooting

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A
General

Sp e c i f i c a t i o n s
Parameter

Specification

Dimension

22 x 30 x 25cm (w x d x h)

Weight

approx. 7kg

Power consumption

Maximal: 100 - 240VAC, 50 - 60Hz (max 1.3A)

Environmental conditions

Operational temperature range: 18C - 35C (64 95F)


Temperature variation: max. 1C/h and max. 2C/day
Humidity (non-condensing): less than 80 % (relative
humidity)
Installation site: in a closed room, max. 2000m
above sea level
Installation overvoltage category: II
Pollution degree: 2

Safety regulations met

Complies with EN/IEC 61010-1/08.2002 (Safety


requirements for electrical equipment for measurement, control and laboratory use)

EMI regulations met

Complies with EN/IEC 61326/05.2004 (Electrical


equipment for measurement, control and laboratory
use - EMC requirements)
7500 - 360cm-1

Performance Spectral range

Optik

Electronics

Resolution

better than 2cm-1, optional better than 0.9cm-1

Wavenumber accuracy

Better than 0.01cm-1

Wavenumber reproducibility

Better than 0.04cm-1

Photometric accuracy

0.1 % T

Design

Sealed optics housing, convective desiccating

Source

Air-cooled (can be replaced)

Interferometer

RockSolid, gold mirrors, permanently aligned

Beamsplitter

Multi-layer coating on Quarz

Detector

DTGS

HeNe laser

ALPHA is a CLASS 1 LASER PRODUCT and contains a laser diode (850nm).

A/D converter

100kHz with 24bit

Connectors

Ethernet

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93

Appendix A

94

Specifications

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10

Consumables
Part Number

Description

1005855

IR source with housing, pre-adjusted

1000917

Desiccant bags

1005847

2x replacement window (KBr), frame-mounted

1006041

2x replacement window (ZnSe), frame-mounted

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95

Appendix B

96

Consumables

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11

Dimensional Drawings
A L P H A - T:

Figure 73: ALPHA-T - Isometric view

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97

Appendix C

Dimensional Drawings

Figure 74: ALPHA-T - Top view

Figure 75: ALPHA-T - Front view

98

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Appendix C

Figure 76: ALPHA-T - Front view, open module

Figure 77: ALPHA-T - Left side view, open module

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99

Appendix C

Dimensional Drawings

ALPHA-P

Figure 78: ALPHA-P - Isometric view

100

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Appendix C

Figure 79: ALPHA-P - Top view

Figure 80: ALPHA-P - Front view

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Appendix C

Dimensional Drawings

Figure 81: ALPHA-P - Right side view, module

102

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Appendix C

ALPHA-E

Figure 82: ALPHA-E - Isometric view

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103

Appendix C

Dimensional Drawings

Figure 83: ALPHA-E - Top view

104

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Appendix C

Figure 84: ALPHA-E - Front view

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Appendix C

106

Dimensional Drawings

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12

Glossary

ATR

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 contact 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 intensity, which is recorded as
absorption spectrum, depending on the wavenumber.
Note: The sample needs to have a lower refraction index than the
crystal to achieve total internal reflection.

Beamsplitter

A device used to produce two separate beams from one incident beam.
Generally a coated substrate that reflects and transmits approximately
equal portions of the incident radiation.

Calibration

The entirety of working steps to define the relation between analyte


concentrations and the corresponding standard measurement values.
Under specified conditions the analyte concentrations are indicated by
an instrument, measuring system, or values which have been evaluated by material measuring or reference material.

Cross-over cable

Cable used for the direct connection of two workstations Network Interface Cards (NICs). NICs have been dedicated to send and receive
lines. A crossover cable connects from the send line of one NIC to the
receive line of the other NIC.

Detector

A device that converts incoming light into an electrical signal.

Ethernet

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
(e.g. an office building). Ethernet is a set of hardware and signaling
standards used for LANs. The most commonly installed systems are
10/100 BaseT.

Fourier Transform

The mathematical transformation used in FT spectroscopy to convert


an interferogram into an infrared spectrum. Essentially, Fourier Transform decomposes or separates a waveform or function into sinusoids of
different frequency which sum to the original waveform. It identifies or
distinguishes the different frequency sinusoids and their respective
amplitudes.

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Appendix D

Glossary

Frequency

The frequency is the number of periods per time unit. Since all electromagnetic waves travel at the speed of light, the frequency corresponding to a given wavelength can be calculated as: = c/

FT-IR

Fourier Transform InfraRed Spectroscopy


A method to obtain infrared spectra of a sample using an interferometer
and then performing a Fourier transform 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.

Instrument test

The instrument test checks the spectrometer performance. It automatically runs when ALPHA communicates with the PC for the very first
time. The test has to be repeated if the validity period (7 days) set by
Bruker has been expired.

Interferogram

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 infinite number of wavelengths. The interferogram
is the continuous 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 and sum to a maximum signal. As
the optical retardation increases different wavelengths undergo constructive and destructive interference 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. Any dispersive element in
the beam path may lead to chirping of the centerburst.

108

Interferometer

Inside the interferometer the light beam is splitted into two beams by
the beam splitter. The most-commonly used Michelson interferometer
consists of a beam splitter, stationary and movable mirror. Due to the
continuous movement of one mirror the optical path lengths of the two
separated beams changes in time. Interference is effected when the
two light beams are recombined.

IP address

Network address of a workstation or network. IP addresses are always


in the form of 4-number fields separated by dots. Each number field
represents 1 byte. Values can be in the range of 0-255. The numbers
on the left of the string define the network, the numbers on the right
define the individual workstation or Network Interface Card (NIC).

Laser

The laser is a coherent source of monochromatic radiation. It is an


essential part of the interferometer system. Due to laser light interferrence the position of the movable mirror (see Interferometer), and the
data sampling positions are determined.

Micrometer (m)

10-6 of a meter; a micron

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Bruker Optik GmbH

Appendix D

MIR

Mid InfraRed; covers the spectral range from 4,000 to 400cm-1 wave
numbers. In this range fundamental vibrations are typically excited.

Performance test

The performance test checks the spectrometer performance. It automatically runs after starting OPUS, and exchanging a measurement
module or ATR crystal plate.

Reflectance

Reflectance is the ratio of the radiation energy reflected from a surface


to the radiation energy incident on the surface.

Reflection

The process by which incident illumination reacts with the sample and
is converted to radiation energy that subsequently travels back from
the sample surface at a defined wavelength.

Relative humidity

The amount of water vapor contained within an air sample, expressed


on a scale of 0 - 100%.

Resolution

Resolution in FT-IR is determined by the maximum optical path difference reached in the measurement of an interferogram. 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 samples 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 values), the higher the noise in the
spectrum at a given measurement time.

Sample

Special kind of substance which is put into the sample position and
measured.

Single-channel
spectrum

The arithmetical transformation of the interferometer, the Fourier transformation, made by the spectroscopic software results in the so-called
single-channel spectrum. This spectrum shows the intensity of each
single wavenumber. The single-spectrum includes the entire spectral
characteristics of the spectrometer, i.e. the signal detected by the
detector as function of the wavenumber. This signal is influenced by
the source type, beamsplitter transmittance, detector response etc.

Spectrometer

From the Latin word specere meaning image, and the Greek word metron meaning to measure. A spectrometer uses some sort of mechanical or electrical detection device to obtain the infrared spectrum of a
sample. It contains a source of infrared radiation, a sample compartment to allow the radiation to interact with a sample, a detector for radiation and units to determine and display the intensity of radiation.

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 presence of functional groups of
molecules of a sample.

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Appendix D

Glossary

Transmission

A portion of the incident illumination energy passes directly through the


sample without any interactions with electrons or molecules in the sample. Another portion of energy is absorbed and re-emitted over and
over again in the same direction as the incident illumination. Transmission is the process of these events. In either case, the photons are
transmitted through the sample.

Transmission measurement

In spectroscopy transmission is the classical method for the IR analysis


of samples. Depending on the sample material, sample 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 intensity ratio of
the IR light before and after passing the sample is measured within a
specific wavelength.

Transmittance

Transmittance is the ratio of the beam energy transmitted through a


sample to the beam energy incident on the surface of the sample.

Validation

During validation the x-axis (frequency) and y-axis (transmission,


reflection) are verified by transmission or reflectance standards which
may be included in the internal validation unit. The validation can be
performed at individual time intervals by the application software.

Wave number

The term wave number is the commonly used dimension for the x-axis
1
in FT-IR spectroscopy. It is defined as = ----. The unit is cm-1.
0

Wavelength

110

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.

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13

Service Addresses
Bruker Optik has an international network of branch offices and
representations to ensure a competent customer service throughout the
world. The following list includes the addresses of Bruker headquarters.
For a complete list with the addresses and telephone numbers of the
Bruker branch offices and representations worldwide, refer to the
internet:
http://www.brukeroptics.com/offices.htmll

North America
Bruker Optics Inc
19 Fortune Drive, Manning Park
Billerica, MA 01821 - 3991
USA
Phone: +1 978 439 9899 (ext. 5227)
Fax: +1 978 663 9177
www.brukeroptics.com
info@brukeroptics.com

Europe
Bruker Optik GmbH
Rudolf-Plank-Str. 27
76275 Ettlingen
Germany
Phone: +49 7243 504 619/600
Fax: +49 7243 504 698
www.brukeroptics.com
ir_service@brukeroptics.de

Asia
Bruker Hong Kong Ltd.
Unit 509, 5/F, Tower II
Enterprise Square No 9
Sheung Yuet Road
Kowloon Bay
Hong Kong
www.brukeroptics.com
Phone: +852 2796 6100
Fax: +852 2796 6109
hk@brukeroptics.com.hk

No responsiblility can be taken for the correctness of this information.


Subject to changes.
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Appendix E

112

Service Addresses

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Index

In OPUS 88
Error Messages
In OPUS 77
ETH/LAN Port 4
Ethernet 107

A
ALPHA-E 8, 9, 54
ALPHA-P 7, 8, 55
ALPHA-T 5, 6, 46
Gas Cell 48
Liquid Cell 47
Sample Compartment 6, 47
Sample Holder 47
Atmospheric Compensation 17, 18
ATR
Cleaning 59
Crystal Types 53
Height Adjustment 56
Measuring 51
Measuring Sample 58
Module 52
Placing Sample 57
Pressure Application Device 54
Sample Measurement 58
Spectra 60
B
Baseline Correction 16
Basic Module 3

I
Instrument Test 78, 86, 108
Interferometer 108
IR Source 62
Replacing 62, 64
K
KBr Pellet 42
Kensington Lock 5
L
Laser 108
LEDs 4
M
Maintenance Instructions 61
Measurement 13, 14
Background 15
Procedure 14
Sample 15
Measurement Module
Exchanging 9
O

C
Calibration Line 37
Calibration Samples 36
CFG Switch 5
Communication Connection 83
Connecting Port 4
Consumables 95

OPUS Status Light 73, 81, 82


P
Peak Pick 19, 21
Interactive 20
Performance Test 78, 85, 109

Desiccant 65
Replacing 66
Detector 107
Diagnostic LEDs 78
Troubleshooting 90
Diagnostics LEDs
Troubleshooting 90, 91

Quality Control 24
Procedure 24
Quantitative Analysis 35, 39
Method 36
Result 40
Quick Compare 24, 27
Method 25
Result 28
Quick User Guide 13

E
Error Message
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Index

R
Reference Sample 24
Relative Humidity 109
S
Sample Measurement 50
Sample Preparation 41
Methods 41
Service Addresses 111
Sigma 40
Specifications 93
Spectra Library 33, 34
Spectrometer Status Indicator 72, 79,
81
Spectrum Search 31
Result 32
Stand-by Mode 11
Substance Identification 31, 32
T
TAP Port 5
Transmission Measurement 45
Troubleshooting 71, 74
V
Validation 110
W
Wave Number 110
Wavelength 110
Windows 67
Cleaning 70
Replacing 67, 68, 69

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Chapt. 14

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