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Specac Gateway ATR User Manual

6 reflection horizontal atr accessory kit
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Gateway™ ATR
6 Reflection Horizontal
ATR Accessory Kit
User Manual
2I-11165-5

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  • Page 1 Gateway™ ATR 6 Reflection Horizontal ATR Accessory Kit User Manual 2I-11165-5...
  • Page 3 Gateway™ ATR 6 Reflection Horizontal ATR Accessory Kit User Manual 2I-11165-5...

  • Page 4: Table Of Contents

    User Manual Gateway™ ATR Accessory Kit P/N GS11165 GATEWAY™ 6 REFLECTION HORIZONTAL ATR ACCESSORY KIT USER MANUAL 1. I ................. 4 NTRODUCTION 2. S ..............6 AFETY ONSIDERATIONS 3. C ............... 7 HECKLIST AND ONTENTS ™ ATR A 4. P ........
  • Page 5 ECHNICAL PECIFICATION ™ ATR S 12. G ..........48 ATEWAY ERIAL UMBERS © April 2016 Specac Ltd. All rights reserved. Brilliant Spectroscopy is a trademark of Specac Ltd. Other product names mentioned herein may be trademarks of their respective owners.

  • Page 6: Introduction

    Specac. The Gateway™ ATR Accessory is simple to install and operate within a wide range of FTIR spectrometer systems via use of the Specac Benchmark™ baseplate mounting assembly. Different Benchmark™ baseplates are available for specific fit into a particular make and model of spectrometer system.
  • Page 7 (2.4 and 4.0 respectively). The range of Gateway ATR top plates that can be used on the optical unit are:- P/N GS11133 Gateway™ ATR Flat top plate with 45° ZnSe crystal.

  • Page 8: Safety Considerations

    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 possible you should follow a procedure for safe handling and containment of the type of sample to be used.

  • Page 9: Checklist Andc

    Gateway™ ATR Accessory 3. Checklist and Contents The Gateway™ ATR Kit as P/N GS11165 is packed in protective wrappings within its container box. The box contains the following: • 1 Gateway™ ATR incompartment optical unit – GS11170. • 1 Trough top plate assembly with 45...
  • Page 10 User Manual • 1 Pair of flexible purge bellow tubes – GS10707. • 1 PTFE pad (used with trough plate and clamp). • 1 Spatula (for spreading pastes or powders) • 1 Allen key - 2.0 mm A/F. • 1 Allen key - 2.5 mm A/F. •...

  • Page 11: Preparing The Gateway

    Gateway™ ATR Accessory 4. Preparing the Gateway™ ATR Accessory Before the Gateway™ ATR Accessory is to be installed and optimized for its optical alignment within a particular spectrometer system to be used, it is necessary to fit the clamp assembly (1) to the optical unit (2) and also to fit either the trough (3) or flat (4) top plate crystal assembly to the optical unit (2).

  • Page 12: Fixing The Clampa

    User Manual The complete Gateway™ ATR clamp assembly (1) consists of a movable (up and down) arm mechanism (7) which is locked into its down position when the top T-bar handle (8) is pushed fully down and closed. (As shown in Fig 2.) The arm mechanism (7), that is raised by pulling up on the T-bar handle (8) or lowered by pressing down on the T-bar handle (8), is connected to a pressure plate and pad assembly (9) with use of an adjustable screw (10) for tensioning of a spring bar...
  • Page 13 Gateway™ ATR Accessory Threaded Screw Holes for Clamp Assembly Fixing Fig 3. Fixing the Clamp Assembly to the Optical Unit Note: The support block (13) is orientated correctly as shown in Fig 3. when the two screw holes of the four that are closest to the edge of the support block (13) are facing towards the pressure plate and pad assembly (9) for fitting.
  • Page 14 User Manual 3) Using the larger 3mm A/F Allen key supplied, secure the clamp assembly (1) to the Gateway optical unit (2) by clockwise rotation for tightening of the four fixing screws (14) through the aligned holes of the clamp assembly (1) and support block (13). (Do not over tighten).

  • Page 15: Fitting The Trough Or

    Benchmark™ baseplate within the spectrometer sample compartment, but either top plate assembly must be fitted for a necessary optimum alignment of the Gateway ATR accessory to be made. On either side of the top surface plate (15) of the optical unit (2) there are two location pins (16).

  • Page 16: Trough (3) And Flat

    ATR spectral measurement to be made. Trough (3) and Flat (4) Gateway ATR Top Plates The trough (3) and flat (4) top plate assemblies provided with the Gateway™...
  • Page 17 Gateway™ ATR Accessory Fig 7. Gateway™ ATR Accessory Trough Top Plate Assembly, Top, Side (Cross Section) and Underside Views...

  • Page 18: Crystal Removal From The Changing The Isolast

    User Manual Crystal Removal from the Trough Top Plate Assembly If the ATR crystal (17) from the trough (3) top plate assembly needs to be removed for thorough cleaning or has become damaged and needs replacing by a new crystal material of the same type or an alternative crystal material, please use the following procedure.
  • Page 19 Gateway™ ATR Accessory Tip: Using gloves and with the fore fingers of both hands covered with soft lens tissue to prevent any scratching to the crystal (17) surface, exert light even pressure on both ends of the crystal (17) simultaneously from inside the trough. With the crystal safely removed, if it needs cleaning please refer to the Notes on Cleaning pages 40 and 41.

  • Page 20: R E - Assembly Of Thet

    User Manual Fig 8. Isolast Gasket in the Trough Top Plate Assembly 4) Place a new Isolast gasket (21) seal (from P/N GS11167) in place of the original seal, centrally in the recessed back face of the trough top plate metal work (18). (See Fig 8.) Ensure that the gasket (21) lays flat within and tight to the edges of the recess.
  • Page 21 Gateway™ ATR Accessory Please use the following procedure. 1) Lay the top plate metalwork (18) with the Isolast gasket (21) fitted, upside down on a clean, flat, soft tissue covered surface as shown at Fig 8. 2) Carefully take the ATR crystal (17) and gently position it with the longest surface downwards onto the Isolast gasket (21) seal.
  • Page 22 User Manual correct pressure for holding the ATR crystal (17) in position and for its upper surface edge to seal tight against the Isolast gasket (21). Warning! Do not over tighten the grub screw (22) as you risk damage to or breakage of the ATR crystal (17). Test the trough (3) top plate assembly for any fluid leaks past the new seal with a 50% mixture of acetone/water in the trough recess and allow the top plate assembly to stand on some tissues for 30 minutes.

  • Page 23: The Flat Top Platea

    Gateway™ ATR Accessory The Flat Top Plate Assembly The flat (4) top plate assembly is shown for its top, side (cross section) and underside views in Fig 9. Fig 9. Gateway™ ATR Accessory Flat Top Plate Assembly, Top, Side (Cross Section) and Underside Views...

  • Page 24: The Ptfe Pad

    User Manual The ATR crystal (17) in the flat (4) top plate assembly is held in place within its surrounding plate metalwork (25) using an epoxy resin glue. From this design it means that the ATR crystal (17) is not removable for replacement in a flat (4) top plate assembly.

  • Page 25: Installation Of Theg

    Gateway™ ATR Accessory 5. Installation of the Gateway™ ATR Accessory Using the Benchmark™ Baseplate The Gateway™ ATR Accessory is base plate mounted. The Gateway™ optical unit (2) fixes to the Benchmark™ baseplate via a central fixing thumbscrew (26). (See Fig 11.) Usually, a spectrometer’s own 3”...
  • Page 26 User Manual 6. Alignment of the Gateway™ ATR Accessory When the Gateway™ ATR clamp assembly (1) has been fitted to the optical unit (2) and the whole assembly of parts (with or without a crystal top plate assembly (3 and 4) already fitted), is installed on the Benchmark™...

  • Page 27: Front Cover Plater

    Gateway™ ATR Accessory The beam passage of light through the optical components of the Gateway™ ATR Accessory is symmetrical, depending upon whether the light passes from the source (S) to the detector (D) of the spectrometer in a left to right (LR) or right to left (RL) beam direction through the sample compartment.

  • Page 28: Alignment Procedure

    User Manual To gain access to the movable mirrors (5) within the optical unit (2) for alignment, the front cover plate (27) is removed. There are two fixing thumbscrews (28) holding the cover plate (27) in position that are loosened by pushing them in and turning anticlockwise (see Fig 13.) (The thumbscrews (28) will remain captive in the cover plate (27).) Alignment Procedure With removal of the front cover plate (27), the two movable mirrors (5)
  • Page 29 Gateway™ ATR Accessory Begin alignment of the Gateway™ ATR Accessory from the following procedure: 1) Establish a beam of light energy level throughput to be monitored from the spectrometers own detection system. The Gateway™ ATR Accessory is aligned in the factory before despatch. On installation, some transmitted signal will be recorded on the spectrometer’s energy monitoring system, but it will be necessary to maximize the optical throughput by adjusting the mirrors (5) for...
  • Page 30 User Manual away from the black anodized mirror mount arm carriage assembly and turn the grub screw (30) clockwise until it re-sets again behind the mount. 4) Having established an optimum signal throughput from both sequential rotation and tilt adjustments of the output mirror (5), repeat the rotation and tilt adjustment steps 2) and 3), but for the input mirror (5).

  • Page 31: Features On Theg

    1/8” I.D. black silicone rubber tubing) is push fitted over the barbed hose connection. Either of the two purge port connections (31) can be used as the inlet port for any purge gas flow. (See Fig 15.) Fig 15. Gateway ATR™ Purge Port Connections and Aperture Ports...

  • Page 32: Fitting The Purgeb

    User Manual To purge the system and maintain a local N gas environment within the optical unit (2), it is necessary to enclose the IR beam between the ends of the Gateway™ ATR optical unit (2) and the sample compartment of the spectrometer itself. This is done with the flexible purge bellows (32) (P/N GS10707 as supplied) when the purge bellows (32) have been trimmed appropriately for fit.
  • Page 33 Gateway™ ATR Accessory These faces of the purge bellows to be a flush fit with the source and detector bulkhead faces of the spectrometer sample compartment To shorten length of purge bellow cut between a groove Fig 16. Gateway™ ATR Accessory fitted with Purge Bellows 1) With the Benchmark™...

  • Page 34: Fitting A Polarizer

    (26) to secure the Gateway™ ATR Accessory back into position. Fitting a Polarizer Specac’s FTIR Infrared polarizers (P/N GS12000 Series) can be inserted into the aperture port rings (33) on the Gateway™ ATR accessory. The polarizers push-fit in these ring apertures and can be rotated to the desired orientation between 0°...

  • Page 35: Sampling Using Theg

    Gateway™ ATR Accessory 8. Sampling Using the Gateway™ Accessory Important Note for Usage! The ZnSe, Ge and Si crystals in the trough (3) or flat (4) top plate assemblies for the Gateway™ ATR Accessory have a specific hardness and chemical resistance and should be treated accordingly. The crystals have been sealed into position by epoxy resin gluing for any flat (4) top plate assembly, but in any trough (3) or flow through top plate assembly the crystal types are removable.
  • Page 36 User Manual Preparing the Gateway™ ATR Accessory for Analysis For any of the ZnSe, Ge and Si crystal top plate assemblies, the active sampling area extends across the whole of the ATR crystal surface. It is therefore preferable to have enough liquid or solid sample type to completely cover the ATR crystal to utilise the maximum energy throughput available for the Gateway™...
  • Page 37 Gateway™ ATR Accessory Spectral Collection Using the Gateway™ Accessory The procedure for collecting a sample ATR spectrum requires first obtaining a background spectrum as a reference using the Gateway™ ATR Accessory with no sample in position on the ATR crystal (17) for any top plate assembly as fitted to the Gateway™...
  • Page 38 User Manual 2. Take the powder sample and spread it very carefully to form a level surface that covers the entire surface area of the ZnSe, Ge or Si ATR crystal (17). Ideally the powder sample should be fine, smooth and homogenous with no hard lumps or inclusions. This will help to avoid any risk of “point load”...
  • Page 39 Gateway™ ATR Accessory 7. Clean the powder sample carefully away from the ATR crystal (17) (avoid the possibility of scratching the ATR crystal (17) surface, particularly if using ZnSe material) and wipe and clean any powder off the surface of the pressure plate and pad (9), if any sample powder has adhered here.
  • Page 40 Hence, when analyzing for a liquid or paste sample it is best to use the trough (3) top plate assembly fitted to the optical unit (2). If the liquid sample is volatile by nature, Specac recommends use of a volatiles cover (P/N GS11132 – not supplied), to place over the open trough plate area to prevent evaporation of the liquid and to enable an ATR spectral measurement to be obtained.
  • Page 41 Gateway™ ATR Accessory Volatiles Cover GS11132 on Trough Top Plate Assembly Fig 17. Volatiles Cover for Gateway™ ATR Trough Top Plate Assemblies Note: If the volatiles cover is to be used on any trough (3) top plate assembly then the clamp assembly (1) must be removed from the optical unit (2) as shown in Fig 17.
  • Page 42 User Manual 3. Place the volatiles cover into position over the sample if necessary. 4. Collect and record the ATR spectrum for the sample. 5. To remove a liquid sample, any excess can be removed by sucking up into a dropping pipette and cleaning any residual liquid sample away using soft lens tissues and an appropriate solvent.
  • Page 43 Gateway™ ATR Accessory wiping with a tissue and therefore minimise any risk of contamination being carried over to other components of the Accessory whilst in situ. Solvents such as water, methanol and acetone are suitable to use for cleaning purposes. Sample solutions that fall within the pH range of pH5 to pH9 are tolerated by the ZnSe crystal material.
  • Page 44 User Manual 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.
  • Page 45 Gateway™ ATR Accessory Keep powder or windows stored in a cool, dry container, with appropriate safety labelling. 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.
  • Page 46 User Manual Keep windows or crystal stored in a cool, dry container. Data Sheet For Silicon General Synonyms: Defoamer S-10. When powder is fused together, is used as a transmission window material. Very hard, but brittle and relatively inert material. Insoluble in water, resists acids and bases but is attacked by combination of hydrofluoric and nitric acid.
  • Page 47 Gateway™ ATR Accessory Keep powder or windows stored in a cool, dry container. 9. Gateway™ ATR Accessory “Bubble Numbers” Part Identification List (1) Clamp assembly (complete). (2) Optical unit (complete). (3) Trough top plate assembly (complete). (4) Flat top plate assembly (complete). (5) Movable mirror in optical unit (2).
  • Page 48 User Manual (33) Aperture ports on the optical unit (2). 10. Gateway™ ATR Accessories Parts List Gateway™ ATR Optical Unit P/N GS11170 Gateway™ In-Compartment ATR optical unit. Gateway™ ATR Top Plates P/N GS11133 Gateway™ ATR Flat top plate with 45° ZnSe crystal. P/N GS11134 Gateway™...
  • Page 49 Flat with epoxy resin with epoxy resin assembly in Flat assembly in Flat assembly Gateway ATR Dimensions 160 x 130 x 130 160 x 130 x 130 160 x 130 x 180 W x D X H (mm)
  • Page 50 Gateway™ ATR Accessory parts you have received. If you need to contact Specac for any issues regarding your Gateway™ ATR Accessory it may be necessary to provide the serial number of the item to identify for replacement parts.
  • Page 51 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...
  • Page 52 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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