Specac Quest User manual

2I-10800-10
The Quest
Single Reflection ATR Accessory
User Manual

2I-10800-10 2
List of Safety Symbols
Safety Symbol
Meaning
Caution! indicates Important information which
needs to be followed for the safe operation of
this accessory.
Caution! –Hot Surface where used indicates
the product contains heated surfaces which
need to be taken into consideration while
handling and operating this device
Caution –Possibility of Electric Shock
Indoor Use Only

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Quest Heated Puck
User Manual

2I-10800-10 4
The Quest Single Reflection ATR Accessory
P/N GS10800
CONTENTS
1. INTRODUCTION..............................................................................5
2. SAFETY ........................................................................................6
3. CHECKLIST OF CONTENTS .............................................................7
4. “BUBBLE NUMBERS”PART IDENTIFICATION LIST..............................8
5. INSTALLATION ...............................................................................9
5.1. Mounting the Quest into the Spectrometer sample
compartment...................................................................................9
5.2. Quest Puck Assembly........................................................10
6. ALIGNMENT PROCEDURE FOR QUEST ATR...................................12
6.1. Front Cover Removal.........................................................12
6.2. Synopti-Focal Mirror System .............................................13
6.3. Alignment Procedure .........................................................14
6.4. Procedure to Follow from Any Accidental Mis-Alignment..16
7. PURGING THE QUEST ATR OPTICAL UNIT ....................................18
8. QUEST ATR CLAMP ARM AND ANVILS ..........................................20
8.1. Clamp Arm Assembly ........................................................20
8.2. Choice of Anvils .................................................................21
9. SAMPLING USING THE QUEST ATR ACCESSORY...........................22
9.1. Background Acquisition .....................................................22
9.2. Solid Sampling Procedure .................................................22
9.3. Liquid Sampling procedure ................................................23
9.4. Cleaning Tips.....................................................................24
10. QUEST SAMPLING ACCESSORIES..............................................26
10.1. The Volatiles Cover........................................................26
10.2. Luer Lock Liquids Anvil ..................................................27
10.3. The Specular Reflectance Puck.....................................27
11. QUEST ATR PART NUMBERS AND SPARES ...............................29
12. QUEST ATR TECHNICAL SPECIFICATIONS .................................31
13. QUEST ATR SERIAL NUMBERS.................................................32
© 2021 Specac Ltd. All rights reserved.
Benchmark and Brillian Spectroscopy are trademarks of Specac
Ltd. Other product names mentioned herein may be trademarks
of their respective owners.

2I-10800-10 5
1. Introduction
Thank you for buying a Specac product. We trust it will provide you with
invaluable and excellent service in use.
The Quest Single Reflection ATR Accessory is designed for the
quantitative and qualitative analysis of solids, powders, liquids, pastes
and gum-like samples using mid-IR spectroscopy at a nominal 45°
incident angle under ambient or elevated temperature conditions.
The Quest is based upon Synopti-Focal technology –an innovative
synoptic focusing array of highly reflective gold coated mirror only optics
–in an optical unit fitted with interchangeable ATR puck assemblies
(choice of diamond, ZnSe, Ge or Si). The ATR crystal is mounted in
either a Standard (flat), Liquid or Heated Puck Assembly. For solid
samples, where good contact with the ATR crystal is required, a clamp
arm produces a highly reproducible load of 40 lbs.
The use of mirror optics maximizes the spectral range as follows:
ATR Crystal
Notes
Range (cm-1)
Diamond
AR Coated
7800 - 400
Non-AR Extended Range
10000 - 10
ZnSe
AR Coated
7800 - 500
Non-AR heated puck
7800 - 500
Ge
AR coated
5500 - 500
Si
Non-AR coated
8333-1350 and
500-33
Arrow (Si wafer)
Thin Wafer
8333-33
Specular Reflectance measurements are also possible by the use of a
specular reflectance puck at a nominal 45 ° angle.

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2. Safety
Caution! Always use personal protective equipment (PPE)
when operating this device and follow local safety operating
procedures and practices with respect to potential toxic and
flammable sample substances.
Make sure that all samples intended to be used with the ATR are
chemically compatible with the accessory surfaces, including:
•The ATR crystal material (diamond, ZnSe, Ge, or Si)
•The indium sealing material around the crystal.
•Stainless-steel used in the puck and anvil components.
•Anodized aluminum & Viton O-ring in the volatiles cover.
•For Arrow only: polypropylene slide, thermoelastic seal (SBS-
SEBS), anodized aluminum puck.
Safety data sheets (SDS) are available in the product support section of
the Specac web site where required and are provided with each crystal
type. As an alternative please contact your Specac representative for
further details.
It is recommended to wear suitable gloves and eye protection PPE at all
times when using this device.
Important! This manual should be read in conjunction with
the Arrow QS user manual where applicable.
Important! This manual should be read in conjunction with
the manual for the heated puck and USB temperature
controller where applicable.

2I-10800-10 7
3. Checklist of Contents
The Quest ATR Accessory is provided in its own specific packaging.
The items that require checking upon delivery depend on which Quest
ATR system has been ordered.
Please check for the following standard items:
1 x Quest ATR Accessory including optical unit
1 x Flat anvil P/N GS10820
1 x Pellet anvil P/N GS10821
1 x Pair of purge bellows P/N GS10707
1 x Volatiles cover P/N GS10825
1 x Ball driver 3.0 mm (for optical unit cover plate removal)
1 x Ball driver 2.5 mm (for mirror adjustment in optical unit)
1 x Benchmark™ baseplate for your FTIR spectrometer
1 x USB manual
Along with any Puck assemblies included with your order, which may
include:
ATR Flat puck (choice of diamond, ZnSe, Ge or Si)
ATR Liquid puck (choice of diamond, ZnSe, Ge or Si)
Arrow Puck and 100 Slides
Heated puck (choice of diamond or Znse)
(consult relevant manuals for checklist of parts)
Specular Reflectance Puck
Carefully remove your Quest ATR Accessory and ATR puck
assembly(s) from the packaging in readiness for use.

2I-10800-10 8
4. “Bubble Numbers” Part Identification
List
1) Optical unit thumb screw. (Figure 5-1).
2) Location slot of ATR puck assemblies (Figure 5-3).
3) Location pin on top surface of the optical unit (Figure 5-4).
4) Magnetic catch for ATR puck assemblies (Figure 5-4).
5) Front cover plate of optical unit (Figure 6-1).
6) Captive screw of front cover plate (Figure 6-1).
7) Grub screw for M6 mirror rotation (Figure 6-3).
8) Cap head screw for M6 mirror tilt (Figure 6-3).
9) Grub screw for M3 mirror rotation (Figure 6-3).
10) Cap head screw for M3 mirror tilt (Figure 6-3).
11) Grub screw for M1 mirror rotation (Figure 6-3).
12) Cap head screw for M1 mirror tilt (Figure 6-3).
13) Aperture port on optical unit (Figure 7-1).
14) Purge tube location port in front cover plate (Figure 7-1).
15) Curved grip plate for purge tubing in front cover plate (Figure 7-2).
16) Purge bellow (Figure 7-3).
17) Flat or Pellet Anvil (igure 8-3).
18) Clamp arm assembly (igure 8-3).
19) Anvil storage port (igure 8-3).
20) Torque screw knob (igure 8-3).
21) Volatiles cover (Figure 10-1).
22) Luer Lock Liquids anvil (Figure 10-3).
23) Specular reflectance puck (Figure 10-4).
24) Reference mirror for specular reflectance puck (Figure 10-4).

2I-10800-10 9
5. Installation
5.1. Mounting the Quest into the Spectrometer sample
compartment
Figure 5-1: Quest ATR Accessory –Optical Unit and ATR Puck Assembly
The Quest ATR Accessory is supported on a Benchmark™ baseplate
when installed into a spectrometer. A Benchmark™ baseplate has three
pillars across the front for location/fixing and a fourth to the rear for
support only. The thumb screw (1) at the front of the Quest ATR optical
unit screws into the front central pillar, while the outer studded pair locate
in slots beneath the Quest unit.”
Note: Install the Benchmark™ baseplate in the spectrometer first
before locating the Quest ATR Accessory.
Fixing holes and studs in the Benchmark™ baseplate will vary
depending upon the make and model of the spectrometer. Refer to the
Benchmark™ baseplate Installation Guide/User Manual.
1

2I-10800-10 10
5.2. Quest Puck Assembly
5.2.1. Quest ATR Puck Assemblies Identification
Top and underside views of the Quest ATR Flat and Liquid puck
assemblies are shown in Figure 5-2 and Figure 5-3.
Figure 5-2: Top view of Quest ATR Diamond Crystal puck: Standard (left) and
Liquids (right) Puck Assembly
Figure 5-3: Underside view of Quest ATR Diamond Crystal
Puck Assembly
ATR Crystal
2
ATR
Crystal
Serial Number
Label
Crystal Puck
Identification
Label

2I-10800-10 11
Puck assemblies have an ATR crystal that protrudes from the top
surface of the puck. Please refer to the Arrow/Heated puck manuals for
more details on these pucks.
Note: The fixing nuts for the underside support bracket of the puck
assembly will be covered with tamperproof red marking strips and
these fixing nuts should never be touched. Any attempt to adjust
these nut fixings will be identifiable and will invalidate any
warranty for the puck assembly.
5.2.2. Fitting the Puck Assembly to the Quest
Install the puck assembly onto the Quest by lining up the alignment
notch (2) in the puck with the locating pin (3) on the Quest top plate (see
Figure 5-3 and Figure 5-4). Three magnets (4) capture and hold the puck
in place when it is correctly positioned on the Quest ATR optical unit.
Some puck assemblies (e.g. heated puck) may need to be firmly pushed
into position.
Figure 5-4: Top view of Quest ATR Optical Unit showing location area for the
Puck Assemblies
3
4

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6. Alignment Procedure for Quest ATR
The Quest ATR Accessory has been factory aligned with your choice of
puck. However, it may be necessary to maximize the optical throughput
for a specific spectrometer by adjusting the mirrors in the optical unit of
the Quest ATR Accessory.
Set up your Quest as described above. For alignment purposes an ATR
crystal puck should be fitted to the Quest. Alternatively, the Quest can
be aligned using an Arrow puck + slide or a specular reflectance puck
fitted with a reference mirror. Setup your spectrometer to monitor the
energy throughput. The precise method of doing this will vary depending
on your spectrometer and software. Please refer to your spectrometer
manual for further information. If no energy throughput is observed,
please refer to page 16.
An overall spectral throughput of light energy between 10% and 35% of
the open beam energy should be achievable, depending upon the ATR
puck assemblies and spectrometer used.
6.1. Front Cover Removal
The optical unit front cover plate (5) is removed by undoing the two
captive cover plate screws (6) (see Figure 6-1) using the 3 mm ball driver
supplied. The front cover plate (5) is pulled up and forward over the fixing
thumb screw (1) to gain access to the internal mirrors.

2I-10800-10 13
Figure 6-1: Quest ATR - Front Cover Plate Removal
6.2. Synopti-Focal Mirror System
The Synopti-Focal mirror arrangement is shown in figure 5-2. For a right-
to-left beam direction, the beam strikes the mirrors in the following
sequence from source-side (S) to detector-side (D):
S, M1, M2, M3, M4, ATR Crystal, M5, M6, D
A left to right beam direction spectrometer inverts the order of the mirrors
between the source and detector. The mirrors M1, M2, M3 and M6 are
flat, gold coated mirrors. (M6 is the slightly larger sized mirror). Mirrors
M4 and M5 are aspheric, focusing gold coated mirrors. The angle of
incidence for the IR light beam when it interacts at the crystal/sample
interface surface is nominally set at 45°.
5
6
1

2I-10800-10 14
Figure 6-2: Cutaway front view of Quest ATR Accessory showing the Synopti-
Focal arrangement of mirror components
6.3. Alignment Procedure
The alignment procedure consists of adjusting mirrors M1, M3 and M6
mirrors, optimizing first rotation then tilt.
Note: The mirrors M2,M4 and M5 do not require adjustment. A cover
has been placed over the rotation adjustment screw for mirror M2
to prevent adjustment.
M5
M4
M6
M3
M1
M2
ATR Puck
S
D

2I-10800-10 15
Figure 6-3: Access to Mirrors M1, M3 and M6 - Cover Plate Removed
1. Using the 2.5 mm ball driver tool supplied, adjust the rotational
alignment of the mirrors M6, M3 and M1 in that sequential order, via
the grub screws, (7), (9) and (11). Carefully adjust each mirror one
at a time, maximizing the energy signal as far as possible before
moving onto the next mirror.
2. Again using the 2.5 mm ball driver, carefully adjust the tilt alignment
of the mirrors using the grub screws labeled (8), (10) and (12) in turn
for these three mirrors (in the same sequence) to maximise the
energy.
3. Repeat steps 1 and 2 a second time to obtain the best possible
alignment.
M6
M1
7
8
12
11
9
10
M3

2I-10800-10 16
When satisfied after one or two adjustment sequences have been
carried out that an acceptable throughput energy has been established,
the front cover plate (5) can be repositioned onto the optical unit.
For some spectrometer configurations, if the Benchmark™ baseplate is
mounted on a rail or is movable in the spectrometer, further
improvements may be possible by adjusting the position of the Quest.
Firmly secure the Benchmark™ baseplate with the Quest Accessory into
this new position before use.
Note: In some spectrometers it may be necessary to remove the Quest
ATR optical unit before securing the baseplate. Where this is the case,
ensure that the Benchmark™ baseplate does not move when removing
the Quest ATR optical unit.
6.4. Procedure to Follow from Any Accidental Mis-
Alignment
If a mistake is made during the alignment procedure and no signal from
the detector can be obtained, then it may be possible to recover the
situation by making a rough visual alignment of the mirror optics M1,
M3, and M6. This will allow enough energy to reach the detector for the
alignment procedure described above to be followed.
Note: The following procedure should also be used if no energy is
observed at the detector on installation.
1. Ensure the fault is with your Quest unit by removing the accessory
and checking for a signal to show that the spectrometer is functioning
correctly (consult Spectrometer manual/dealer for more information).
2. Remove the Benchmark™ baseplate, front cover plate (5) and any
puck assembly from the top of the optical unit.
3. Using the 2.5 mm ball driver tool in the screws (8), (10) and (12),
adjust all three mirrors M1, M3 and M6 ONLY for their angle of tilt
such that these mirror surfaces are normal (i.e. at a 90° right angle)
with relation to the back plane of the main mirror mount frame
assembly.

2I-10800-10 17
4. Adjust the rotation of mirrors M3 and M1 using grub screws (9) and
(11) to form a straight line. Refer to Figure 6-2.
5. Adjust Mirror M6 using grub screw (7) until it is approximately
perpendicular to the plane of mirrors M3 and M1, as shown in Figure
6-2.
6. With the three mirrors M1, M3 and M6 now roughly positioned for
their tilt and rotation angles, the optical unit can be placed back onto
the Benchmark™ baseplate within the spectrometer compartment
and the puck fitted back on top of the optical unit.
7. Set up your IR spectrometer to monitor the energy throughput. If
there is still no signal after the procedural steps above have been
completed, then turning the grub screw (7) for rotation of the mirror
M6 (first one way and then the other), which should lead to the
energy level signal returning.
8. There should now be some energy level indication (however small),
at the detector after passage of light through the Quest ATR
Accessory and so the fine alignment procedure can now be followed
starting with rotation of mirror M6 as described from step 1) on page
15 of this instruction manual.

2I-10800-10 18
7. Purging the Quest ATR Optical Unit
The Quest is fitted with an optional purging port into which 1/4” tubing
can be inserted. This is useful for suppressing atmospheric water vapor
and/or CO2with inert gas from a cylinder or from a purge gas generator.
To fit a purge line remove the front cover plate (5), push your tube
through the purging port (14) and secure in place using the curved grips
(15), as shown in Figure 7-1 and Figure 7-2. Then refit the front cover
plate (5).
Figure 7-1: Aperture Ports and Purge Connection on the
Quest ATR Optical Unit
Figure 7-2: Front Cover Plate with Purge Tube –Front and Back Views
14
13
5
15

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A pair of purge bellows (16) (P/N GS10707) are supplied to help
maintain the purged environment inside the accessory. They attach to
the accessory’s two aperture ports (13) and seal the gaps between the
accessory and the spectrometer bulkhead (see (see Figure 7-1 and
Figure 7-3.)
Figure 7-3: Quest ATR Accessory fitted with Purge Bellows
The purge bellows (16) are installed by a push fit to the aperture ports
(13) of the Quest. If the gap/distance between the optical unit and
bulkhead is small, the purge bellows can be cut to size for a better fit. It
is best to cut along one of the ridged grooves. For optimal results ensure
a flush fit with the inlet/outlet bulkhead faces of the spectrometer sample
compartment
Tip: It is recommended that purge bellows (16) are fitted during use to
help stabilize the spectrometer/instrument background even if
purging is not to be carried out.
16

2I-10800-10 20
8. Quest ATR Clamp Arm and Anvils
8.1. Clamp Arm Assembly
When using the Quest ATR Accessory with a solid sample a load must
usually be applied to ensure good contact between the ATR crystal and
sample. To use: rotate the clamp arm assembly into the position shown
in Figure 8-1, if necessary adjusting the height of the anvil (17) by
adjustment of the Torque Knob (20). When in the correct position the
arm will click into place. When not in use it can be rotated out of the way
and will again click into the parked position.
Figure 8-1: Clamp Arm Assembly with Flat Anvil in Sampling Position
8.1.1. Torque Limiter
To apply a load to the sample it should be placed onto the crystal with
the anvil positioned directly over it. A load is applied by rotating the
torque limited screw knob assembly (20) until it clicks three times. This
will apply a consistent load of 40 lbs to your sample. Further rotation of
the knob will not increase the load beyond 40 lbs.
Always apply force to the sample slowly, applying the
load gradually via the clamping arm assembly. Beware of
point loads, particularly with harder samples, which could
damage your ATR crystal. An acceptable ATR spectrum
for the sample may be produced without having to apply
the maximum load.
17
18
20