Specac Golden Gate GS10500 Series User manual

Golden Gate™ Single
Reflection Diamond ATR System
User Manual
2I-10500 Issue 19

Golden Gate™Single Reflection
Diamond ATR System
User Manual
2I-10500 Issue 18

User Manual
2
Golden Gate™Single Reflection Diamond ATR
System (GS10500 Series)
CONTENTS –USER MANUAL
1INTRODUCTION ..................................................................................4
2. SAFETY CONSIDERATIONS ................................................................6
3. UNPACKING AND CHECKLIST .............................................................7
4. GOLDEN GATE™ATR SYSTEM TOP PLATES .....................................8
5. INSTALLATION INTO A SPECTROMETER.............................................16
6. ALIGNMENT OF GOLDEN GATE™ATR ACCESSORY .........................18
7. FITTING A POLARIZER AND PURGING THE GOLDEN GATE™ATR
ACCESSORY...................................................................................22
FITTING A POLARIZER .....................................................................22
PURGING THE SYSTEM....................................................................23
8. CHANGING LENSES IN THE GOLDEN GATE™ATR OPTICAL UNIT ......25
REMOVING THE LENSES ..................................................................25
FITTING NEW LENSES .....................................................................26
9. ANVILS FOR GOLDEN GATE™ATR ACCESSORY .............................28
FITTING OF AN ANVIL ......................................................................33
10.SAMPLING USING THE GOLDEN GATE™ATR ACCESSORY.............34
GENERAL PRINCIPLES ...................................................................34
FEATURES OF THE GOLDEN GATE™ATR ACCESSORY ..................35
PREPARING THE GOLDEN GATE™ATR ACCESSORY FOR
ANALYSIS .....................................................................................37
COLLECTING ATR SPECTRA FOR DIFFERENT SAMPLE TYPES ..........38
POWDER SAMPLES ........................................................................38
FLAT SOLID SAMPLES ....................................................................40
PELLET BEAD SAMPLES .................................................................43
FIBER SAMPLES.............................................................................43
LIQUIDS AND PASTE SAMPLES ........................................................44
CORROSIVE SAMPLES....................................................................45
PRESSURE ON SAMPLE (LOAD).......................................................47
NOTES ON CLEANING.....................................................................48

Golden Gate™ Single Reflection Diamond ATR System
3
11.LEGEND -BUBBLE PART NUMBER IDENTIFICATION .......................... 54
12.SPARE PARTS FOR THE GOLDEN GATE™ATR ACCESSORY
SYSTEM ........................................................................................ 56
13.TECHNICAL SPECIFICATION............................................................ 58
14.GOLDEN GATE™ATR SERIAL NUMBERS ....................................... 59
© April 2016 Specac Ltd. All rights reserved.
Golden Gate, Benchmark and Brilliant Spectroscopy are trademarks of
Specac Ltd. Other product names mentioned herein may be
trademarks of their respective owners.

User Manual
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1 Introduction
Thank you for purchasing a Specac Product.
The Golden Gate™Single Reflection Diamond ATR system (GS10500
Series) is an extremely versatile sampling accessory to allow for many
different sampling options in the quantitative and qualitative analysis of
solids, liquids, pastes and microsamples by FTIR spectroscopy.
A complete Golden Gate™ATR accessory system consists of an ATR
crystal top plate assembly fixed over an optical beam condensing unit.
This complete accessory is mounted into an infrared spectrometer
using a Benchmark™ baseplate.
The angular incidence of light at the ATR crystal sample interface is
nominally at 45°. Although liquid samples by their nature in general
make excellent sample contact to the ATR crystal being used for any
spectral analyses, most of the Golden Gate™ ATR top plate options
available have a special bridge and clamping mechanism that provides
for excellent and reproducible contact between a solid sample and the
single reflection ATR crystal. The different top plate options that have
a bridge and clamping mechanism can utilise a choice of different
compression anvil types to provide the best possible contact and
sample containment over the ATR crystal for an extremely diverse
range of solid sample forms.
In sampling of solid sample types, when pressure is applied to force
the sample into contact against the ATR crystal, any anvil being
employed does not rotate against the sample. This ensures that heat is
not generated by friction in the force application, as heat could change
the sample. It also ensures that the sample is not displaced from the
correct sampling position for consistent measurement.
The optical unit of the Golden Gate™ ATR consists of a combination of
mirrors and beam condensing lenses designed to achieve optimal
infrared radiant energy throughput. The beam condensing lenses used
in the optical unit are a choice of ZnSe or KRS-5 material. These
lenses are distinctly separate from the single crystal diamond ATR

Golden Gate™ Single Reflection Diamond ATR System
5
crystal that is used in the top plate assembly (in all but the germanium
crystal top plate option), where the sample to be studied makes
contact. Use of a specific set of lenses in the optical unit determines
the spectral throughput range achievable for the Golden Gate™ ATR
accessory, but the structural and chemical integrity of the ATR crystal
is maintained. KRS-5 lenses allow for a slightly wider spectral
transmission range for Mid IR studies to circa 350cm-1 rather than
ZnSe lenses which fully absorb at circa 550cm-1. However, an anti-
reflection coating on ZnSe lenses allows for a better overall light
energy throughput than the uncoated KRS-5 lens options, over the
typical “fingerprint” region of the IR spectrum.
The choice of top plates available to be mounted on an optical unit for
a Golden Gate™accessory system includes:
•Diamond crystal top plate P/N GS10563.
•Germanium crystal top plate P/N GS10566.
•Heated diamond crystal top plate P/N GS10540.
•High temperature diamond crystal top plate P/N GS10640.
•Wire holder diamond crystal top plate P/N GS10565.
•Microspecular reflectance top plate P/N GS10514.
•Reaction cell diamond crystal top plate P/N GS10507.
•Low temperature diamond crystal top plate P/N GS10590.
•Supercritical fluid diamond crystal top plate P/N GS10585.
Golden Gate Accessory GS10500 Series

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2. Safety Considerations
With use of any spectroscopic accessory that
involves the study of a wide range of chemical
samples, the associated risk in handling may mostly
be attributed to the specific sample type to be
handled itself. As far as it is possible you should
follow a procedure for safe handling and
containment of the type of sample to be used.
With respect to safety in operation specifically for the Golden Gate™
ATR accessory, a single crystal daimond or germanium crystal
material for the ATR crystal is used in the top plate assembly where a
sample makes contact. There is a choice of either ZnSe or KRS-5
material for the lens assemblies in the optical unit.
Out of these four different crystal material types, KRS-5 and then ZnSe
are the most potentially hazardous materials with respect to a toxicity
risk in use and handling. Both diamond and germanium crystal
materials can be considered relatively safe to use, although
germanium may be harmful to the body if it is ingested in significant
quantity. The general rule when working with any crystal material (and
sample) is to always wear gloves and safety gear (e.g. safety
spectacles) when handling to obviate the risk of contact with the skin.
Specifically in operation of a Golden Gate™ ATR accessory there is a
minimal risk associated with contact to the KRS-5 or ZnSe materials
used for the lens assemblies as these are safely contained within the
optical unit and should not require being handled after an initial
alignment and optimum throughput has been obtained at installation.
Crystal material safety data sheet information for each of the material
types can be consulted for safe handling. A copy of each of these
datasheets can be found in this instruction manual in the Notes On
Cleaning Section found on pages 50 to 53.

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3. Unpacking and Checklist
The configuration of Golden Gate™ATR accessory ordered from a
specific part number will determine the items to check on delivery.
Please refer to Section 4 of this manual for the specific top plate option
and additional items that are supplied for the accessory combination.
All Golden Gate™ATR accessory systems will include the following:
●1 Golden Gate™optical unit with beam condensing lens
assemblies (ZnSe or KRS-5 lens material options).
●1 Benchmark™baseplate for your model of FTIR spectrometer.
●1 Ball driver 3.0 mm.
●1 Allen key 2.0 mm.
●1 Purge bellows (GS10707).
●1 Essential Spares Kit for the particular Golden Gate™ ATR
accessory.
●1 Quick Start Guide for the Golden Gate™ ATR accessory.
●1 Benchmark™ baseplate installation guide instruction manual.
Carefully lift your Golden Gate™
top plate and optical unit from the
carry case and place onto a flat
bench. Installation of the top plate
(1) is achieved by positioning it on
to the optical unit (2) and securing
by turning the two thumb screws (3)
clockwise.
Important: The top plate must be
fitted the correct way around. When
fitted correctly the sides of the top
plate will be flush with the sides of
the optical transfer unit.
Fig 1. Fitting of Golden Gate™
Top Plate to Optical Unit
3
1
2

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4. Golden Gate™ATR System Top Plates
There are a variety of top plates for the Golden Gate™Single
Reflection ATR system. The top plates can be ordered as part of a
complete Golden Gate™ ATR accessory, or separately as upgrades.
Diamond Crystal ATR Top Plate (P/N GS10563) from P/N’s
GS10500-Z or GS10500-K Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™Diamond ATR Top Plate (GS10563).
•1 Sapphire anvil (GS10531).
•1 Pellet anvil (GS10532).
•1 Volatiles cover (GS10503).
•1 Essential Spares Kit of parts (GS10550). (When ordered as accessory).
Fig 2. Golden Gate™ Diamond ATR Top Plate GS10563

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Germanium Crystal ATR Top Plate (GS10566) from P/N GS10516
Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™ Germanium ATR Top Plate (GS10566).
•1 large stainless steel anvil (GS10567).
•1 Volatiles cover (GS10503).
•1 Essential Spares Kit of parts (GS10550). (When ordered as accessory).
Fig 3. Golden Gate™ Germanium ATR Top Plate GS10565
Important! - Note for Use of Germanium Crystal
The germanium crystal does not have the same hardness and
chemical resistance as a diamond and should be treated accordingly.
Be careful not to put a point loading on the crystal, particularly with
hard or abrasive samples. With samples such as rubber and soft
polymers covering the crystal, normal anvil pressures may be used.
Check on the chemical resistance before potentially damaging
materials are brought into contact with the crystal. Thin films on plastic
substrates can be analysed, but take care if the substrate is metallic.
Test for suitability by applying pressure gradually from the clamp anvil
mechanism, taking scans to see if the spectra are acceptable.

User Manual
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Heated Diamond ATR Top Plate (GS10540) from P/N’s GS10542-Z
or GS10542-K Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™ Heated Diamond ATR Top Plate (GS10540) to 200°C.
•1 4000 Series Temperature Controller for the heated top plate.
•1 Sapphire anvil (GS10531).
•1 Pellet anvil (GS10532).
•1 Volatiles cover (GS10503).
•1 Essential Spares Kit of parts (GS10550). (When ordered as accessory).
•1 Instruction manual for 4000 Series Temperature Controller operation.
Fig 4. Golden Gate™ Heated Diamond ATR Top Plate GS10540 (to 200°C)
Warning! The diamond ATR crystal and tungsten carbide support
puck in the heated top plate GS10540 has a very small air gap around
its circumference edge. This minimizes heat loss to the surrounding
top plate and ensures a quick warm up. However, if excessive
amounts of solvent are used on the diamond crystal, it is possible for
the liquid (or vapour) to leak past the puck into the optical unit below,
giving unwanted solvent absorption bands in any experimentation. For
this reason, the diamond should only be covered with a minimum of
liquid sample or cleaned using a tissue moistened with solvent.

Golden Gate™ Single Reflection Diamond ATR System
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High Temperature Diamond ATR Top Plate (GS10640) from P/N’s
GS10642-Z or GS10642-K Accessory Order
Please check on delivery that the following have been included:
•1 High Temperature Diamond ATR Top Plate (GS10640) to 300°C.
•1 4000 Series Temperature Controller for the heated top plate.
•1 Sapphire anvil (GS10531).
•1 Pellet anvil (GS10532).
•1 Volatiles cover (GS10503).
•1 Essential Spares Kit of parts (GS10550). (When ordered as accessory).
•1 Instruction manual for 4000 Series Temperature Controller operation.
Fig 5. Golden Gate™ High Temperature Diamond ATR Top Plate
GS10640 (to 300°C)
Note: The diamond ATR crystal and tungsten carbide support puck in
the high temperature top plate GS10640 does not have a small air
gap around its circumference edge. The tungsten carbide material is
sealed around its circumference edge to PEEK material as a circular
barrier which acts as both a thermal insulator and a protection from the
ingress of liquid samples and any volatile solvent vapours into the
optical unit below. Nevertheless, the diamond should still be cleaned
using a tissue moistened with a minimum amount of solvent.

User Manual
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Microspecular Reflectance Top Plate (GS10514) from P/N’s
GS10523-Z or GS10523-K Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™ microspecular reflectance top plate (GS10514).
•1 Reference mirror.
•1 Essential Spares Kit of parts (GS10527). (When ordered as accessory).
Fig 6. Golden Gate™ Microspecular Reflectance Top Plate GS10514
The microspecular reflectance top plate can be fitted to the Golden
Gate™ optical unit to provide a single reflection 45° angle specular
reflectance measurement of small solid sample types. The top plate
slot aperture is 5mm x 2.5mm and so any sample must be larger than
these dimensions when placed over the slot aperture for spectral
analysis to prevent the sample from falling into the optical unit below.
Reaction Cell Diamond ATR Top Plate (GS10507) from P/N’s
GS10525-Z or GS10525-K Accessory Order
This is a “specialist” Golden Gate™ top plate that incorporates a 45°
angle diamond crystal puck at the base of a 24mls volume reaction
chamber. It is capable of operating at temperatures up to 200°C and
at up to 3000 psi pressure.
A specific temperature controlling system and relevant instruction
manuals are provided for this Golden Gate™top plate option for
explanation of operation. A dedicated stirring mechanism (GS10513)

Golden Gate™ Single Reflection Diamond ATR System
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can also be used as an alternative top pressure plate assembly with
the Reaction Cell Diamond ATR top plate option if this is ordered.
Please check on delivery that the following have been included:
•1 Golden Gate™ Reaction Cell Diamond ATR Top Plate (GS10507).
•1 4000 Series Temperature Controller for the reaction cell top plate.
•1 Torque Wrench (GS10504).
•1 Square/Hexagon Drive Adapter.
•2 Open Ended Spanner 7/16 inch and 3/8 inch AF.
•1 3.0mm AF Hexagon Head Bit.
•1 6.0mm AF Hexagon Head Bit (Ball End).
•1 Allen Key 2mm AF Long Arm.
•1 3.0mm AF Hexagon Ball Driver.
•1 Essential Spares Kit of parts (GS10528). (When ordered as accessory).
Stirring Mechanism Reaction Cell Top Plate
Fig 7. Reaction Cell Top Plate GS10507 and Pressure Cap Stirring
Mechanism GS10513

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Low Temperature Diamond 45° ATR Top Plate (GS10590) from
P/N’s GS10592-Z or GS10592-K Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™ Low Temperature Diamond ATR Top Plate (GS10590).
•1 4000 Series Temperature Controller for the Low Temperature Diamond
ATR Top Plate.
•1 Sapphire tipped solids anvil.
•1 Liquid sample injector (insulated hypodermic needle and glass syringe).
•1 Plastic funnel.
•1 Long T-bar Allen key (5 mm).
•1 Allen Key (3 mm).
•1 Glass filled PTFE gaskets (5).
•1 High thermal transfer gaskets (20).
•1 Spare Viton O-ring.
•1 User manual for Low Temperature Golden Gate™top plate operation.
•1 Essential Spares Kit of parts (GS10550). (When ordered as accessory).
Fig 8. Golden Gate™ Low Temperature ATR Top Plate GS10590
The Golden Gate™ Low Temperature Diamond ATR Top Plate
operates over a temperature range of -150°C to + 80°C.

Golden Gate™ Single Reflection Diamond ATR System
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Supercritical Fluid (SCF) Diamond ATR Top Plate (GS10585) from
P/N’s GS10586-Z or GS10586-K Accessory Order
Please check on delivery that the following have been included:
•1 Golden Gate™ SCF Diamond ATR Top Plate (GS10585).
•1 4000 Series Temperature Controller for the SCF Diamond ATR Top
Plate.
•2 Open Ended Spanner 1/4” – 5/16”.
•1 Torque wrench (GS10504).
•1 Socket drive 2.5 mm A/F.
•1 Graphite pressure gaskets (10 in packet).
•1 User manual for the SCF Diamond ATR top plate operation.
•1 Essential Spares Kit of parts (GS10529). (When ordered as accessory).
Fig 9. Golden Gate™ Supercritical Fluid ATR Top Plate GS10585
The Golden Gate™ SCF Diamond ATR Top Plate is specified to
operate at temperatures up to 300°C and pressures up to 6000 psi.

User Manual
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5. Installation into a Spectrometer
The Golden Gate™Single Reflection ATR accessory is supported on a
Benchmark™baseplate when installed into a spectrometer. The
baseplate has three support pillars (one flat at the back and two with
location pins at the front) and a fourth front central pillar into which the
fixing thumb screw (4) on the optical unit (2) is tightened. (See Fig 10.)
Note: It is usually preferable to install the Benchmark™baseplate in
the spectrometer first, before locating the Golden Gate™ATR
accessory.
Fixing pillars, plates and studs in the Benchmark™ baseplate will vary
dependant on the make and model of your spectrometer. For details
on how to install your Benchmark™ baseplate and Golden Gate™
ATR accessory into the spectrometer, refer to the Benchmark™
baseplate installation guide instruction manual as supplied.
Fig 10. Fixing Thumbscrew on Golden Gate™ Optical Unit.
4
2

Golden Gate™ Single Reflection Diamond ATR System
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6. Alignment of Golden Gate™ ATR Accessory
When you have installed the Golden Gate™Single Reflection ATR
accessory into your spectrometer please check the alignment of the
accessory. The Golden Gate™ATR Accessory will be preliminarily
aligned when first supplied from Specac. On a local installation for the
specific spectrometer to be used, some transmitted energy will be
recorded by the spectrometer, but for best results adjusting the
accessory optics will maximize the optical throughput.
Note: The energy (optical) throughput of the Golden Gate ATR
accessory when installed varies with the spectrometer design
and optical settings It should usually be possible to achieve at
least 6% transmission at 1000 cm-1 when a spectrum is
recorded of the ATR accessory against an open beam
background It is important on installation of any accessory into a
spectrometer that a maximum throughput is achieved to ensure
an optimum analytical performance and signal-to-noise ratio
relationship.
The Golden Gate™ optical unit (2) contains six optical components.
Two mirrors and one lens make up the input system and an identical
set of mirrors and lens form the output system (see Fig 11.). The two
mirrors (M1 and M4) are fixed while the two mirrors (M2 and M3) have
rotation and tilt adjustments. The focusing lenses (L1 and L2) are
adjustable for their focus by sliding them within their support mounts.
The simplified diagram at Fig 12. shows the positioning of these optical
components within the optical unit (2). A diamond ATR top plate (from
GS10563) is shown in position representing the sample to complete a
beam path. The procedure for alignment of the accessory is the same
with use of any other ATR top plate (sample) in position on the optical
unit, except for the microspecular reflectance top plate GS10514,
which requires its own reference mirror to be placed over the sampling
aperture slot. In any spectrometer system, the source of light that
passes to the detector may be either from a left to right (Lto R) or right
to left (Rto L) beam direction through the sample compartment when
viewed from above or at the front of the spectrometer system. Hence,
for any alignment procedure to be made on the Golden Gate™ ATR

User Manual
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accessory it always best to start with the adjustable output mirror in
the optical unit (2) that is nearest to the detector.
Note: Fig 11. shows the optical components for a beam passage in
sequence from M1 - M2 - L1 –Sample - L2 - M3 –M4 for an
Lto Rbeam spectrometer and M3 is the adjustable output
mirror. For an R to Lbeam spectrometer, the beam sequence is
reversed and M2 becomes the adjustable output mirror.
Fig 11. Optical Components in the Golden Gate™ Optical Unit Related to
the Beam Passage for L to R or R to L Direction Spectrometers
Alignment of the Golden Gate™ATR Accessory
The following alignment procedure has been written for the Golden
Gate™ ATR accessory when installed into an Lto Rbeam direction
spectrometer. If the Golden Gate™ ATR accessory is installed into a
Rto Lbeam direction spectrometer the input and output mirrors and
lens positions are reversed. Prior to installation of the accessory into
the spectrometer, set the spectrometer system to read an energy value
to measure as a guide during the alignment procedure. An energy level
(throughput count number value) or a voltage peak to peak signal level
for an unobstructed beam can be used as the reference to compare.
With the Golden Gate™ ATR accessory installed into the sample
compartment of the spectrometer, loosen the two thumb screws (5)
L1
Sample
L2
M3
M4
M1
M2