User Manual Golden Gate™ Single Reflection Diamond ATR System (GS10500 Series) CONTENTS – USER MANUAL .................. 4 NTRODUCTION 2. S ..............6 AFETY ONSIDERATIONS 3. U ............. 7 NPACKING AND HECKLIST 4. G ™ ATR S ........8 OLDEN YSTEM LATES 5.
User Manual 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.
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Golden Gate™ Single Reflection Diamond ATR System 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™...
User Manual 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.
Golden Gate™ Single Reflection Diamond ATR System 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.
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User Manual 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:...
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Golden Gate™ Single Reflection Diamond ATR System 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). •...
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User Manual 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. •...
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Golden Gate™ Single Reflection Diamond ATR System 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. •...
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User Manual 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.
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Golden Gate™ Single Reflection Diamond ATR System 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: •...
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User Manual 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.
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Golden Gate™ Single Reflection Diamond ATR System 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). •...
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User Manual 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.
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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.
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User Manual 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 L to R beam spectrometer and M3 is the adjustable output mirror.
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Golden Gate™ Single Reflection Diamond ATR System and remove the front cover (6) on the optical unit (2) to reveal the optical components for their adjustment (See Figs 12 and 13). Fig 12. Optics Cover Removal from Golden Gate™ ATR Accessory Note: The diamond top plate of the Golden Gate™...
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User Manual Fig 13. View of Optical Components in the Golden Gate™ ATR System Usually, from installation of the Benchmark™ baseplate into the sample compartment it remains in a fixed position. The alignment procedure begins from this fixed positioning of the accessory in the sample compartment.
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Golden Gate™ Single Reflection Diamond ATR System 2. Start by using the 3mm ball driver supplied in the screw (8) of the adjustable output mirror (M3) to very gently adjust the rotational movement of the mirror to achieve a maximum energy reading. Tip: If the energy reading on the instrument monitor goes to zero while making any adjustment to an optical component, always bring the energy throughput back to a readable value adjusting the same...
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User Manual 6. Now, maximize the energy throughput on the input adjustable mirror (M2) by adjusting it for rotation and tilt in the same way as completed for mirror (M3) (see procedure steps 2 and 3). 7. Complete the alignment procedure by adjusting the focus of the input lens (L1), in the same way as completed for lens (L2) (see procedure steps 4 and 5).
ATR accessory. Fitting a Polarizer The FTIR Infrared polarizers (GS12000 Series) from Specac can be fitted to the aperture ports (15) of the Golden Gate™ ATR optical unit (2). (See Fig 14.) The polarizers push fit into the aperture port openings and can be rotated to the desired orientation by hand.
Golden Gate™ ATR accessory. This rotator mount allows for an easier setting of a polarized grid plane of light than that required in use of a GS12000 Series polarizer. (Please ask Specac for details). Purging the System The Golden Gate™ ATR optical unit (2) is fitted with purge ports (16).
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Golden Gate™ Single Reflection Diamond ATR System Make Any Cut Between Ridges of the Bellow Length “X” Fig 15. Fitting Purge Bellows to the Golden Gate™ ATR Optical Unit 2. Using a sharp razor, cut lengths of the flexible purge bellow (17) tubes which are equivalent to the measured length (X) plus an additional 10 mm for each bellow.
User Manual 8. Changing Lenses in the Golden Gate™ ATR Optical Unit The Golden Gate™ ATR accessory is provided with ZnSe or KRS-5 beam condensing lenses as standard in the optical unit (2). If you wish to change from one set of lenses to the other they are available as upgrade kits.
Golden Gate™ Single Reflection Diamond ATR System 2. Any Golden Gate™ ATR Top Plate being used must be removed from the optical unit (2). This is achieved by loosening the two thumb screws (3) on the Top Plate and lifting it up and away from the optical unit (2).
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User Manual Important: For a correct insertion of the new lens barrel assemblies (12), ensure the tiller bar (14) screw holes are aligned with the front slots in the mount (13) casings. 2. Tighten the tiller bars (14) into their holes in the lens barrels assembly (12) (turn clockwise).
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Golden Gate™ Single Reflection Diamond ATR System 9. Anvils For Golden Gate™ ATR Accessory Choice of Anvils and their Uses There are many different compression head anvils that can be used with the Golden Gate™ Single Reflection ATR top plates. The types and their uses are shown in the following table:- Anvil P/N Description...
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User Manual Sapphire Anvil (GS10531 - Fig 18.) This anvil can be used with all diamond ATR top plates (see anvil table), for solid or powder samples. The sapphire element on the anvil face is 3.8 mm in diameter. Fig 18. Sapphire Anvil GS10531 Pellet Anvil (GS10532 - Fig 19.) This anvil is made of stainless steel and has a concave recess designed for round samples...
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Golden Gate™ Single Reflection Diamond ATR System Stainless Steel Anvils (GS10549 and GS10567 - Figs 21a & 21b) Either of these stainless steel anvils can be used in place of the sapphire flat anvil GS10531 if desired. GS10549 has a surface pressing face of 4mm diameter.
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ATR crystal instead of use of the volatiles cover GS10503. (Please contact Specac for more details). Fig 23. Micro Reaction Flow Cell Anvil GS10568 View Thru Anvil Bridge Assembly (GS10569 - Fig 24.) This is a standard anvil for viewing of a sample being compressed into contact onto the ATR crystal.
Golden Gate™ Single Reflection Diamond ATR System assembly. This is achieved simply by undoing and removing the hinge screw pin from the Golden Gate™ top plate bridge pivot hole, swapping over the standard clamp head bridge assembly with the view-thru anvil bridge assembly and refitting the hinge screw. Hinge Screw Pin of Bridge Passes Through This...
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User Manual General View of Clamp Head Area Anvil Recess 8mm Dia. Fits Over O-ring (21) Detailed View of Clamp Head Area Fig 25. Fitting of an Anvil to the Clamp Head of the Torque Limiter Screw on the Golden Gate™ ATR Accessory Tip: To fit, apply a small twist to the anvil (18) itself whilst pushing it over the O-ring (21).
Golden Gate™ Single Reflection Diamond ATR System 10. Sampling Using the Golden Gate™ ATR Accessory General Principles When using the Golden Gate™ Single Reflection ATR accessory the sample is placed onto the crystal area (23) of the top plate. (See Fig 25.) The contact between a solid sample and crystal is improved using the clamp bridge (19) and an appropriate compression head anvil (18).
User Manual Fig 27. Angled View of Diamond ATR Top Plate (Bridge Open) Features of the Golden Gate™ ATR Accessory Torque Limiter Screw Mechanism The Golden Gate™ ATR top plates with a bridge assembly (19) have a built-in torque limiter screw (22) mechanism. With an appropriate anvil (18) fitted for a solid sample to be compressed against the ATR crystal (23) and when the bridge (19) is closed, the torque limiter screw (22) is turned clockwise to lower the anvil face towards the sample to provide...
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Golden Gate™ Single Reflection Diamond ATR System Fig 28. Torque Limiter Screw Showing Torx Head Screw Fixing Quick Lock and Release Mechanism The clamp bridge (19) has a quick lock and release mechanism (25). When pressure needs to be applied to a solid sample via an appropriate fitted anvil (18), the bridge must be closed (see Fig 26.).
User Manual bridge assembly (19) from accidentally falling back down to its closed position onto the bridge support (27). In addition, when sampling liquids (with the exceptions of the micro reaction flow cell anvil GS10568 or view thru anvil bridge assembly GS10569), there is no need to use the bridge (19) with an appropriate anvil (18) as the liquid sample will be in adequate contact with the ATR crystal to enable an ATR spectrum to be collected.
Golden Gate™ Single Reflection Diamond ATR System Fig 29. Closed Bridge Golden Gate™ Diamond ATR Top Plate Collecting ATR Spectra for Different Sample Types Important: Golden Gate™ diamond crystals are selected for their freedom from natural structural flaws using optical test methods.
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User Manual 1. Collect a background spectrum as described on page 37. 2. Take the powder sample and spread it very carefully to form a level surface that covers the entire surface of the diamond ATR crystal (23). Ideally the powder sample should be fine, smooth and homogenous with no hard lumps or inclusions.
Golden Gate™ Single Reflection Diamond ATR System After cleaning (see Notes On Cleaning page 48), the Golden Gate™ ATR Accessory is ready to accept a new sample for measurement. Flat Solid Samples When analyzing for a flat solid sample it is best to use the sapphire anvil GS10531 (18) fitted to the clamp head (20) assembly.
GS10531 (18) instead. Beware to avoid any point loading on the ATR crystal with a small pellet/bead sample. For hard or very hard samples Specac recommend use of diamond ATR crystal top plates only instead of the germanium ATR top plate.
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Golden Gate™ Single Reflection Diamond ATR System 3. Gently lower the bridge (19) past the stay up catch (26) and lock it closed using the quick lock T-knob (25), ensuring that the anvil (18) is initially retracted far enough clear of the sample to be pressed. 4.
User Manual Fiber Samples The measurement of fibers or wire type samples can be achieved from utilization of the narrow groove GS10547 and wide groove GS10548 anvils (18) for centralisation of the sample over the ATR crystal. If neither of these anvils are available for use with any Golden Gate™ ATR top plate fitted to the optical unit (2), then it is best to use the sapphire anvil GS10531 (18) fitted to the clamp head assembly (20).
Golden Gate™ Single Reflection Diamond ATR System Note: If the sample may be hard or could produce a point load effect, carry out rotation of the torque knob slowly and apply the load gradually. An acceptable ATR spectrum for the sample may be produced without having to apply a maximum load setting from the torque knob assembly.
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User Manual O-ring fitted into a groove at the circumference of the underside surface. (See Fig 30.) After a volatile liquid sample has been spotted onto the ATR crystal, the volatiles cover (28) is simply placed over the ATR crystal area (23) with the O-ring in contact against the diamond/tungsten carbide or germanium/stainless steel puck in a respective diamond or germanium top plate assembly.
(e.g. phosphoric acid), from prolonged contact under hostile conditions of elevated temperature. Specac recommend that your sample is confined to the center of the diamond only, if there is a risk of chemical attack upon contact with the other materials of construction.
User Manual potentially aggressive chemicals.) A sample spot size of 2 microns deep with a diameter of 600 microns is sufficient. Specac recommend that a pipette, or similar glass capillary tube, is used to apply small sample spots to the center of the diamond only.
Golden Gate™ Single Reflection Diamond ATR System Notes On Cleaning When cleaning the diamond or germanium ATR crystal of the Golden Gate™ ATR accessory in preparation for a new sample, it is very important to take care to avoid damage to the crystal materials. As mentioned in the Safety Considerations (Section 2, page 6), these two crystal materials that are used for sample contact are not particularly hazardous in terms of risk of toxicity if they contact with the skin.
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User Manual In common with general use, it will only be necessary to wipe and clean away at the ATR crystal area (23) between samples and possibly the face of any anvil (18) if used. If possible try to avoid any solvent or cleaning solution materials from getting to the underside of the crystal area (23) and into the optical unit (2) and onto the lens and/or mirror components, if the Golden Gate™...
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Golden Gate™ Single Reflection Diamond ATR System Data Sheet For Diamond General Hardest substance known for carbon (C) elemental form. Can be shaped, cut and polished to form spectral transmission window or crystal for ATR spectroscopy. Has a highish Refractive Index value and can suffer reflection losses but these can be improved with antireflection optical coatings Extremely chemically resistant to practically all known materials.
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User Manual Data Sheet For Germanium General Hard and very brittle material, but can be shaped, cut and polished to form spectral transmission window or crystal for ATR spectroscopy. Because of its high Refractive Index value suffers from large reflection losses but these can be improved with antireflection optical coatings Is temperature sensitive and loses transmission when heated.
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Golden Gate™ Single Reflection Diamond ATR System Data Sheet For Zinc Selenide General Toxic and hard, yellow coloured crystalline powder when fused together as a solid can be used as a transmission window material or as a crystal material for attenuated total reflectance (ATR) FTIR spectroscopy. Insoluble in water, but attacked by strong acids and bases.
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User Manual Data Sheet For KRS-5 General Synonyms: Mixture of Thallium Bromide and Thallium Iodide (typically 58% Iodide content). Very toxic red coloured soft crystalline powder when fused together as a solid can be used as a transmission window material or as a crystal material for attenuated total reflectance (ATR) FTIR spectroscopy.
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Golden Gate™ Single Reflection Diamond ATR System 11. Legend – Bubble Part Number Identification...
User Manual (1) Golden Gate™ ATR top plate assembly. (2) Golden Gate™ optical unit. (3) Fixing thumb screw for top plate to optical unit. (4) Fixing thumb screw for optical unit to Benchmark™ baseplate. (5) Fixing screw for front cover plate of optical unit (position for thumb screw shown in diagram).
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12. Spare Parts for the Golden Gate™ ATR Accessory System For details of upgrade options and spares for your Golden Gate™ ATR accessory, please contact your local Specac office. Golden Gate™ Top Plate Options GS10563 Diamond crystal ATR top plate.
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User Manual GS10567 Large Stainless Steel Flat Anvil (for germanium top plate). GS10568 Microreaction Flow Cell Anvil. GS10569 View-Thru Anvil Bridge Assembly. Spares GS10504 Torque wrench. GS10505 Torx adapter bit for torque wrench. GS10509 Torque wrench and Torx adapter bit (combined). GS10707 Purge Bellows.
Golden Gate™ Single Reflection Diamond ATR System 13. Technical Specification ATR Crystal Diamond Germanium Single Crystal Diamond ° Ge 45 ° - 2 mm x 2 mm 4 mm x 4 mm Accessory 5000 -700 cm 5000 -700 cm Transmission (with ZnSe lenses) (with ZnSe lenses) Range...
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To help, please use the table below to fill in the serial number information against the part number of the Golden Gate™ ATR accessory and parts you have received. If you need to contact Specac for any issues regarding your Golden Gate™ ATR accessory it may be necessary to provide the serial number of the item to identify for certain specific replacement parts.
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Systems Engineering Inc. -Tokyo Fax: 215 793 4011 Tel: 03 3946 4993 Fax: 03 3946 4983 United Kingdom email:systems-eng@systems-eng.co.jp Specac Ltd. - London Website: www.systems-eng.co.jp Unit 12, Science & Innovation Centre Halo Business Park Spain Orpington Teknokroma S.Coop C. Ltda...
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Brilliant Spectroscopy™ www.specac.com SPECAC INC. SPECAC LTD. 414 Commerce Drive Unit 12, Science & Innovation Centre Suite 175, Halo Business Park Fort Washington, Orpington PA 19034, USA Kent BR5 3FQ Tel: 215 793 4044 Tel: +44 (0) 1689 873134 Fax: 215 793 4011...
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