PerkinElmer UATR User manual

UNIVERSAL ATR SAMPLING ACCESSORY
User’s Guide
MOLECULAR SPECTROSCOPY

Release History
Part Number Release Publication Date
L1050231 C September 2017
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, CT 06484
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of
any kind with regard to this document, including, but not limited to, the implied warranties of
merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in
connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever or
translated into any language without the prior, written permission of PerkinElmer, Inc.
Copyright © 2017 PerkinElmer, Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such,
are protected by law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.
Spectrum and Spectrum Two are trademarks of PerkinElmer, Inc.

Contents
Conventions Used in this Manual........................................................................ 4
Notes, Cautions and Warnings..................................................................... 4
Introduction...................................................................................................... 5
Unpacking the UATR ......................................................................................... 7
Installing the UATR ........................................................................................... 8
Fitting the accessory................................................................................... 8
Accessory detection by Spectrum software..................................................10
Taking a Reference Background spectrum...................................................10
Contamination Check........................................................................................11
Cleaning the crystal ...................................................................................11
Performing a Contamination Ready Check...................................................11
Performing Ready Checks that use Polystyrene ..................................................12
Handling Samples ............................................................................................13
Solid samples ............................................................................................13
Liquid samples ..........................................................................................13
Obtaining a Sample Spectrum with Spectrum Software.......................................14
Obtaining a spectrum of a solid sample, using the pressure arm...................14
Obtaining a spectrum of a liquid sample......................................................17
Maintenance ....................................................................................................19
Replacing the pressure arm o-ring ..............................................................19
Replacing the top-plate..............................................................................19

4 . Universal ATR Sampling Accessory User’s Guide
Conventions Used in this Manual
Normal text is used to provide information and instructions.
Bold text refers to text that is displayed on the screen.
UPPERCASE text, for example ENTER or ALT, refers to keys on the PC keyboard. '+' is
used to show that you have to press two keys at the same time, for example, ALT+F.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
The term ‘instrument’ refers to a Spectrum Two Series spectrometer, and any sampling
accessory fitted.
Notes, Cautions and Warnings
Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.
NOTE: A note indicates additional, significant information that is provided with some
procedures.
CAUTION
ATTENTION
We use the term CAUTION to inform you about situations that could
result in
serious damage
to the instrument
or other equipment.
Details about these circumstances are in a box like this one.
Nous utilisons le terme «ATTENTION» pour vous informer des situations
pouvant entraîner des dommages sérieux à l'instrument ou à d'autres
équipements. Les détails sur ces circonstances se trouvent dans une boîte
comme celle-ci.
WARNING
AVERTISSEMENT
We use the term WARNING to inform you about situations that could
result in personal injury to yourself or other persons. Details about
these circumstances are in a box like this one.
Nous utilisons le terme AVERTISSEMENT pour vous informer des
situations pouvant entraîner des blessures personnelles pour vous-
même ou pour d'autres personnes. Les détails sur ces circonstances se
trouvent dans une boîte comme celle-ci

Universal ATR Sampling Accessory User’s Guide . 5
Introduction
The Universal Attenuated Total Reflectance Accessory (UATR) is an internal reflection
accessory, used with a Spectrum Two Series spectrometer, for simplifying the analysis of
solids, powders, pastes, gels and liquids. The technique is non-destructive.
As the beam does not penetrate deeply into the sample, this technique is ideal for analyzing
strong infrared absorbing solutions, such as emulsions or aqueous solutions. The technique
can also prove useful in measuring homogeneous solid samples, solid surfaces and coatings
on solid samples.
Figure 1 The Universal ATR Sampling Accessory

6 . Universal ATR Sampling Accessory User’s Guide
How the UATR works
The technique involves placing a sample on top of a crystal with a high refractive index. An
infrared beam from the instrument is passed into the accessory and up into the crystal. It is
then reflected internally in the crystal, and back towards the detector which is housed in the
instrument. When the beam is reflected within the crystal, it penetrates into the sample by a
few microns. Figure 2 illustrates this process.
Figure 2 Principle of UATR operation
The UATR can be used to analyze homogenous solid samples, solid surfaces, or coatings on
solid samples. Force may be applied to ensure good contact.
The Spectrum Two UATR uses a diamond crystal. The diamond crystal is hard, is not easily
scratched, is resistant to strong acids and bases, and can withstand high pressures. The
diamond UATR has an effective scanning range that matches the full range of the
instrument, although sensitivity is somewhat reduced in the approximate range 1900–
2700 cm−1.

Universal ATR Sampling Accessory User’s Guide . 7
Unpacking the UATR
As soon as you receive your UATR Accessory, make sure that it includes the parts listed
below. If anything is missing or damaged, contact your local PerkinElmer office.
The UATR Accessory itself is shipped fully assembled and ready to install.
Part Number Description Quantity
UATR Accessory 1
L1600239 Test Sample Holder 1
L1601742 Medium Shoe 1
L1601743 Large Shoe 1
L1601746 Volatiles Cup 1
L1601856 Apron 1
L1601857 Transit Shoe 1
L1601862 Transit Friction Pad 1
L1050242 Spectrum Two Manuals CD 1
L1100667 UATR Accessory Shipping Disk 1
The Shipping Disk contains reference spectra for your accessory which can be used to check
if its performance has changed.

8 . Universal ATR Sampling Accessory User’s Guide
Installing the UATR
Fitting the accessory
The UATR fits into the sample compartment of the spectrometer, replacing the sample plate.
NOTE: Before you begin you should, if necessary, loosen the pressure arm and release the
transit block that secures the UATR pressure arm during transport.
You may also need to remove the covers on the left and right sides of the accessory,
and the top-plate dust cover.
Store all these in a safe place for future use, if required.
To remove the sample plate and install the UATR:
1. Raise the sample cover of the spectrometer to the vertical position and lift it upwards,
clear of the instrument.
Store it in a safe place for future re-use.
2. Slide the sample plate out of the sample area (Figure 3).
Store it in a safe place for future re-use.
Figure 3 Removing the basic sample plate

Universal ATR Sampling Accessory User’s Guide . 9
3. Pivot the UATR on the ledge at the front of the sample area (Figure 4a), then tip it
backwards (Figure 4b).
NOTE: If the accessory is pivoted too far forward on the sample area ledge it will not move
correctly into position.
(a)
(b)
Figure 4 Installing the accessory
4. Push the UATR home firmly, ensuring that the top of the accessory mates properly with
the lid of the instrument (Figure 5).
The UATR is now ready for use.
Figure 5 UATR installed in a Spectrum Two

10 . Universal ATR Sampling Accessory User’s Guide
NOTE: When the UATR is installed, a connection is made between the accessory and the
purge system used in the instrument. To purge the accessory, connect to the white
plastic purge connector on the underside of the instrument, at the right.
Accessory detection by Spectrum software
The Spectrum software detects the presence of the accessory automatically, and the Setup
Instrument Basic (Figure 6) and Setup Instrument BeamPath (Figure 7) tabs are updated to
show details of the UATR accessory.
Figure 6 Setup Instrument Basic tab with UATR details circled
Figure 7 Setup Instrument BeamPath tab with UATR icon circled
Taking a Reference Background spectrum
Once you have installed your UATR, and before you use it for the first time, you should
consider taking a background spectrum which will act as a reference background for use with
those Ready Checks that need one for comparison purposes, including the
Contamination
Check
described on page 11.
NOTE: For information about taking a background spectrum, see the Spectrum on-screen
Help.

Universal ATR Sampling Accessory User’s Guide . 11
Contamination Check
The surface of the crystal must be clean before a measurement is taken. The contamination
check can be used to ensure this. If the crystal is not properly cleaned, negative bands in the
spectra may be observed.
Cleaning the crystal
Once data has been collected, the crystal should be cleaned.
The surface of the crystal can be cleaned with a cotton-bud moistened with pure water or a
pure organic solvent. The liquid should not be allowed to evaporate, but should be removed
with a clean, dry cotton-bud.
Take care not to scratch the surface of the crystal. Ensure the crystal is completely dry
before re-use.
A PVC “apron” (L1601856) is provided, that protects the top and front of the accessory when
cleaning with solvent.
Performing a Contamination Ready Check
NOTE: For information about setting up Ready Checks, see the Spectrum on-screen Help.
The following description assumes that Ready Checks are already set up and
enabled.
To perform a Contamination Ready Check:
1. From the Measurement menu, select the Instrument Checks sub-menu and then
Contamination from the Ready Checks available.
The Ready Checks dialog is displayed.
2. Make sure that you have removed any sample from the UATR and cleaned the crystal,
and then click Scan.
A new background spectrum is collected, compared to the reference background
spectrum (a spectrum taken when the crystal is known to be totally clean), and the
result of the test displayed.
3. If required, click the link that enables you to see a print preview of the Instrument
Ready Checks Report.

12 . Universal ATR Sampling Accessory User’s Guide
Performing Ready Checks that use Polystyrene
The Ready Checks available in the Spectrum software can be used to demonstrate that
various aspects of the performance of your complete system, including your UATR, are fit-
for-purpose.
Some of these Ready Checks, including Abscissa Check and Ordinate Check, use a
polystyrene sample as reference.
A polystyrene sample that can be used on the top-plate of your UATR is provided for use
when carrying out these Ready Checks.
NOTE: For information on Ready Checks, see the Spectrum on-screen Help.

Universal ATR Sampling Accessory User’s Guide . 13
Handling Samples
Care should be taken with all samples to ensure that spillages do not occur and that the
sample does not come into contact with any part of the accessory other than the top-plate.
A PVC “apron” (L1601856) is provided, that protects the top and front of the accessory.
Solid samples
Good contact between the sample and the surface of the crystal is important to prevent loss
of beam penetration. To aid this good contact the UATR pressure arm can be used, in
conjunction with a “shoe”, to apply a controlled force to the sample and make better contact
with the crystal.
The following shoes are available:
•Large (L1601743) – for low sample pressures
•Medium (L1601742) – for higher sample pressures
Liquid samples
Viscous liquids can be placed directly onto the surface of the UATR crystal.
Samples of volatile and non-viscous liquids should be placed in a “volatiles cup” (L1601746).

14 . Universal ATR Sampling Accessory User’s Guide
Obtaining a Sample Spectrum with Spectrum
Software
The following pages outline the procedure for obtaining a sample spectrum using a
Spectrum Two instrument fitted with a UATR and running Spectrum software.
For further information on how to use Spectrum software, see the on-screen help provided.
NOTE: When you first fit the accessory, the software automatically sets default scan
parameters to values that are appropriate to the UATR.
Obtaining a spectrum of a solid sample, using the
pressure arm
1. To view or change any of the instrument parameters, select Instrument from the Setup
menu.
The Setup Instrument pages are displayed in the Dialog Pane at the bottom of the
workspace. Figure 6 on page 10 shows the Setup Instrument Basic tab.
2. If you need to collect a background spectrum, ensure that the top-plate is clean and
then click , on the toolbar, to collect a background spectrum.
Spectrum automatically alerts you when you need a new background, and can be
configured to request a new background at set intervals (on the Setup Instrument Data
Collection tab).
NOTE: If you want to collect a background that will be added to the Sample View and can
be saved separately, then select Background as the Scan type on the Setup
Instrument Basic tab.
3. Push the pressure arm back, until it is clear of the top-plate.
4. Slide the appropriate shoe over the end of the shaft until it clips into place.
5. Place your sample in the center of the top-plate, over the crystal.
6. Swing the pressure arm across, so that the end is positioned directly above the sample
and the crystal.
CAUTION
ATTENTION
Do not use the pressure arm without a shoe. The high point loads may
damage the crystal.
Avoid using thick samples that require you to unscrew the pressure arm
to the level of the o-ring.
N'utilisez pas le bras de pression sans une chaussure. Les charges
élevées peuvent endommager le cristal.
Évitez d'utiliser des échantillons épais qui vous obligent à dévisser le bras
de pression au niveau du joint torique.

Universal ATR Sampling Accessory User’s Guide . 15
Figure 8 Moving the pressure arm into its operating position (large shoe)
7. Enter a suitable Sample ID and Description in the toolbar, and then click to
enter Preview mode.
The Live tab is displayed.
NOTE: If you have deselected the Preview checkbox on the toolbar, you should select the
Monitor option from the Measurement menu in order to enter Preview mode.
8. Screw down the pressure arm to apply the minimum force to the sample required to
give a good spectrum, as shown on the Live tab.
If an adequate spectrum, with a transmission level of between 40 and 80%, cannot be
achieved, the pressure should be released and a new sample prepared with an
increased or decreased amount of material.
The Force Gauge area of the dialog will display the force being applied. If the indicator
bar turns red, then too much force is being applied; the pressure arm and/or the crystal
is in danger of being damaged.
NOTE: If you want to compare various samples, or use quantitative techniques, ensure you
use the same amount of force each time. You can zero the force gauge by collecting a
background when no pressure is applied to the crystal. Subsequent force
measurements should then be consistent.
You should also ensure that you have the same type of shoe fitted when collecting
each spectrum.

16 . Universal ATR Sampling Accessory User’s Guide
Figure 9 Force Gauge indication in Spectrum software
You are now ready to collect data.
NOTE: An over-pressure device is fitted to the pressure arm that significantly reduces the
risk of crystal breakage. This clutch-slip mechanism should never operate in day-to-
day use, as the pressure required for this to happen is greater than should be
necessary to achieve optimum transmission of between 40 and 80%.
The Force Gauge indicator bar, if displayed, will turn red before the over-pressure
device comes into effect.
9. Click to obtain the sample spectrum.
The History settings of your sample will contain information about the UATR accessory type.
The Spectrum Help file describes how to format, process and report your results. To open
the Help file, select Contents from the Help menu.

Universal ATR Sampling Accessory User’s Guide . 17
Obtaining a spectrum of a liquid sample
1. To view or change any of the instrument parameters, select Instrument from the Setup
menu.
The Setup Instrument pages are displayed in the Dialog Pane at the bottom of the
workspace. Figure 6 on page 10 shows the Setup Instrument Basic tab.
2. If you need to collect a background spectrum, ensure that the top-plate is clean and
then click , on the toolbar, to collect a background spectrum.
Spectrum automatically alerts you when you need a new background, and can be
configured to request a new background at set intervals (on the Setup Instrument Data
Collection tab).
NOTE: If you want to collect a background that will be added to the Sample View and can
be saved separately, then select Background as the Scan type on the Setup
Instrument Basic tab.
3. If your sample is volatile or non-viscous, continue the procedure below; otherwise,
place a drop of your sample on top of the crystal and go straight to step 11.
4. Push the pressure arm back, until it is clear of the top-plate.
5. Slide the medium size shoe over the end of the shaft until it clips into place.
6. Place an empty volatiles cup in the center of the UATR top-plate, over the crystal.
7. Swing the pressure arm across, so that the shoe is positioned directly above the cup.
Figure 10 Using the pressure arm with a medium shoe to position the
volatiles cup
8. Screw down the pressure arm gently, until the shoe just meets the cup.
This ensures that the center of the cup is positioned exactly over the crystal.
9. Loosen the pressure arm, so that it is clear of the cup, and then swing it back, until it is
clear of the top-plate.

18 . Universal ATR Sampling Accessory User’s Guide
10. Place a drop of your liquid sample in the cup.
If your sample is particularly volatile you can bring the pressure arm back into position
and screw it down gently, so that the shoe acts as a cover.
Figure 11 Using the pressure arm and medium shoe to cover the volatiles cup
NOTE: The volatiles cup is not intended to be used as a pressure shoe for solid samples.
11. Enter a suitable Sample ID and Description in the toolbar, and then click to
enter Preview mode.
The Live tab is displayed, showing a preview of your sample spectrum.
You are now ready to collect data.
12. Click to obtain the sample spectrum.
The History settings of your sample will contain information about the UATR accessory type.
The Spectrum Help file describes how to format, process and report your results. To open
the Help file, select Contents from the Help menu.
CAUTION
ATTENTION
Clean the volatiles cup immediately after use. Do not place a used
volatiles cup back on a storage peg, on the top of the accessory, until it
has been cleaned.
Nettoyez la cuvette volatile immédiatement après l'utilisation. Ne placez
pas une tasse volatile sur une pince de rangement, sur le dessus de
l'accessoire, jusqu'à ce qu'elle soit nettoyée.

Universal ATR Sampling Accessory User’s Guide . 19
Maintenance
Replacing the pressure arm o-ring
If the o-ring on the pressure arm becomes worn, the pressure shoes may slip off when the
arm is being moved. A replacement o-ring is available from PerkinElmer (L9004319).
Replacing the top-plate
In the event that the top-plate becomes damaged, it can be replaced with one of the same
type. Contact your PerkinElmer representative for details of part numbers.
1. Remove the accessory from your Spectrum Two instrument.
2. Position the transit block supplied with your UATR on top of the crystal.
3. Swing the pressure arm across and screw it down, securing the transit block firmly in
place.
This provides an even pressure over the surface of the top-plate.
Figure 12 Removing the top-plate
4. Use a ball-ended hexagonal wrench to remove the two fixing screws from the rim of the
top-plate.
5. Loosen and swing back the pressure arm.
6. Remove the transit block and then lift the top-plate off the body of the accessory.
CAUTION
ATTENTION
Lift the top-plate off the accessory very slowly and carefully to avoid
damaging the optics immediately underneath.
Retirez la plaque supérieure de l'accessoire très lentement et
soigneusement pour éviter d'endommager l'optique immédiatement en
dessous.
Screw
position
Screw
Transit
block

20 . Universal ATR Sampling Accessory User’s Guide
7. Insert the two fixing screws into the rim of the new top-plate, so that they are just
captured.
Figure 13 Fixing screws captured in top-plate
8. Place the new top-plate on the body of the accessory.
Ensure that it is oriented correctly, so that the indent on the underside accomodates the
gold mirror that protrudes from the body of the accessory.
CAUTION
ATTENTION
If you put the top-plate on in the wrong orientation you may cause
damage to the gold mirror.
Si vous placez la plaque supérieure dans la mauvaise orientation, vous
risquez d'endommager le miroir d'or.
The top-plate should fit easily into position on top of the two support pillars and on the
O-ring inside the rim. Ensure that the O-ring is seated correctly and is not twisted or
deformed.
Figure 14 UATR with top-plate removed
Support
pillar
Support
pillar
O-ring
Gold
mirror