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Specac Golden Gate User Manual
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Specac Golden Gate User Manual

Low temperature diamond atr system
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Low Temperature
Golden Gate
Diamond ATR System
TM
User Manual
2I-10590 Issue 10

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Summary of Contents for Specac Golden Gate

  • Page 1 Low Temperature Golden Gate Diamond ATR System User Manual 2I-10590 Issue 10...

  • Page 2: List Of Safety Symbols

    (Reference ISO 7010-W010) CAUTION! Only use the configured temperature controller supplied with this accessory. CAUTION! This user instruction manual should be read in conjunction with the temperature controller and Golden Gate manuals provided separately with the respective Specac accessory.
  • Page 3 Low Temperature Golden Gate™ Diamond ATR User Manual 2I-10590 Issue 10...
  • Page 4 OP PLATE 8. S PARE ARTS FOR EMPERATURE OLDEN OP PLATE © April 2016 Specac Ltd. All rights reserved. Golden Gate™ and Brilliant Spectroscopy™ are trademarks of Specac Ltd. Other product names mentioned herein may be trademarks of their respective owners.
  • Page 5 Thank you for purchasing a Specac Product. The Low Temperature Golden Gate™ single reflection diamond ATR top plate is designed for use on the Golden Gate™ ATR optical base unit. It is used to study liquid or solid samples at temperatures from minus 150C to +80C.
  • Page 6 1 and 2.) Fig 2. Diamond/Tungsten Carbide Puck and Gasket detail area of Low Temperature Golden Gate™ Top Plate Using liquid nitrogen as an example refrigerant in the dewar chamber (6) and from control of power to the heaters, temperatures below ambient can be achieved.
  • Page 7  Low Temperature Golden Gate™ single reflection diamond ATR top-plate (P/N GS10590).  Golden Gate Optical unit with choice of ZnSe or KRS-5 lenses and appropriate Benchmark baseplate (if ordered as a complete Golden Gate system (P/N GS10592)).  4000 Series Temperature Controller, instruction manual and power cables.

  • Page 8: Safety Of Use

    User Manual 3. Safety of Use WARNING – Low Temperature / Freezing conditions The Low Temperature Golden Gate™ ATR system requires the use of liquid nitrogen (LN ) for operation at sub ambient temperatures. When using refrigerants, ensure all local laboratory safety procedures are followed and wear appropriate personal protective equipment (PPE).
  • Page 9 Only clean with a soft, lightly dampened cloth. Do not use harsh and/or abrasive cleaners on any Specac product. Consult Specac or their authorized agent if in any doubt. Always check before use that the safety protection provided have not been compromised or impaired.

  • Page 10: Installation

    User Manual 4. Installation For the Low Temperature Golden Gate™ ATR system, P/N GS10592 the system is fully assembled before shipping (See Fig.3). Fig 3. Low Temperature Golden Gate™ ATR System Once installed into the host spectrometer, connect the heater and thermocouple cables to the 4000 Series Temperature Controller (Not shown).
  • Page 11 GS10590), the heated top plate is attached to the dewar assembly before shipment. The dewar assembly and will need to be separated from the heated top plate to enable fitment of the Golden Gate™ optical unit. The dewar assembly is then re-installed to complete the assembly.
  • Page 12 User Manual The heated top plate assembly (3) attaches to the Golden Gate™ optical unit (11) with the two new M4 x 16mm screws (12) supplied (See Fig 5.). The new screws replace of the original thumb screws and are shorter in length to allow the fixing of the dewar assembly to the flat stainless steel heated top plate (Refer to P/N GS10500 Golden Gate™...
  • Page 13 Additional Information: When conducting the alignment procedure on the optical components (mirrors and lenses) within the Golden Gate™ optical unit, ensure that the cold dewar assembly (2) and the thermal transfer gasket (5) has been tightened/screwed down correctly to the heated top plate assembly (11).
  • Page 14 (6). This is to prevent condensation or frost forming on the internal optics of the Golden Gate™ optical unit. The purge can be established by using a spectrometers own purge facility (if available) by using the purge bellows (P/N GS10707) to bridge the gap between the Golden Gate™...
  • Page 15 ATR crystal. See Fig 7. Fig 6. Low Temperature Golden Gate™ Dewar area with Dewar Cap removed. (Inner and Outer Dewar Chambers) Fig 7. Low Temperature Golden Gate™ Dewar Cap Purge Holes...
  • Page 16 User Manual CAUTION! Use of alternative refrigerants The minimum recommended operating temperature is -150°C when used in combination with liquid nitrogen (LN ) and the graphite high thermal transfer gasket. Other types of refrigerant mixture are listed in the table below. Table of Refrigerant types Refrigerant Type Mixed Temperature (a)
  • Page 17 Preparation for Use and General Operation The successful use of the Low Temperature Golden Gate™ ATR accessory depends on the correct balancing of a specific refrigerants “heat removing” capability against the energy (heat) input from the electrical block heaters (17), built into the heated top plate assembly (3) at the base of the dewar assembly (2).
  • Page 18 User Manual Fig 8. Low Temperature Golden Gate™ Heated Top Plate Assembly underside view If it is a requirement to obtain spectra for a sample at two different physical states, solid and liquid, depending upon the freezing point of a liquid sample it may be preferable to use the graphite high thermal transfer gasket (5) in position.
  • Page 19 Low Temperature Golden Gate™ ATR Reference Spectrum Collection For collection of a background reference spectrum, at room temperature conditions, establish the nitrogen purge gas conditions in the optical unit (11) and within the internal sample chamber area (15) from connection of the purge gas via a suitable flow pipe or tubing through one of the dewar cap purge gas holes (16), before any refrigerant is added.
  • Page 20 User Manual Note: It is important for this type operation at very low temperatures to ensure the LN2 refrigerant level is kept topped up to provide the “balancing effect” against the power from the heaters (15). Sample Spectrum Collection When a reference spectrum at a particular low temperature value has been collected the procedure of operation needs to be repeated, but with some subtle changes.
  • Page 21 Low Temperature Golden Gate™ ATR there will be some fuming of the LN2 as it boils off when contacting with a warmer environment, but by adding small amounts of LN2, after time the actual temperature on the controller display will begin to drop fairly quickly indicating the effect of the LN2 refrigerant action to the sample area for temperature measurement.
  • Page 22 Install the accessory in the Spectrometer, align the optics according to the Golden Gate™ instruction manual (GS10500) and connect up the 4000 Series Temperature Controller. Establish the nitrogen purge to both the optical unit (11) and the internal chamber area (15) via the dewar cap (10).
  • Page 23 (18) is put down into the center part of the dewar (15) through the hole (19) in the dewar cap (10) and the bridge assembly (20) of the Low Temperature Golden Gate™ top plate is closed and locked. A flat anvil (21) is fixed to the clamp part (22) of the bridge assembly (20) and is used to transfer the pressure to the long sapphire anvil (18).
  • Page 24 User Manual Fig 9. Low Temperature Golden Gate™ Bridge Assembly with Dewar Cap, Flat Anvil and Sapphire Rod in position Fig 10. Low Temperature Golden Gate™ Flat Anvil, Sapphire Rod and Dewar Cap Parts.
  • Page 25 7. Using the long T bar type Allen Key 5mm loosen the four captive clamp screws (4) and remove the complete dewar assembly (2) from the Golden Gate™ heated diamond ATR top plate (3). It is now possible to dry off any remaining sample and clean the diamond surface (1).
  • Page 26 User Manual Solid Samples The ideal solid sample shape for the Low Temperature Golden Gate™ diamond ATR top-plate is a 5mm diameter disc. The solid sample is dropped down into the centre part of the dewar (15) such that it lies correctly on the diamond (1).
  • Page 27 4000 Series Temperature Controller to explain how to access the factory set parameter list values for the Low Temperature Golden Gate™ accessory and how these values/settings can be changed. For this specific type of experiment using the cardice/acetone refrigerant with the white PTFE low thermal transfer gasket (5) over the temperature range from -30°C to 20°C at 5°C steps for temperature...
  • Page 28 6. Operating Parameters for the Low Temperature Golden Gate™ ATR Top Plate The Low Temperature Golden Gate™ ATR system is provided with its own dedicated 4000 series 150W temperature controller. A separate manual is supplied with the controller. For operation of the Low temperature Golden Gate™...
  • Page 29 Low Temperature Golden Gate™ ATR Displayable Parameters For Low Temperature Golden Gate ATR Top-plate 10590 with WEST 6100+ (4000 Series™) Controllers Parameter Parameter Name Parameter Factory Display (In Set Value Green) FiLt Input Filter Time Constant OFFS Process Variable Offset...
  • Page 30 17. Heated diamond ATR top plate block heater. 18. Long sapphire anvil rod. 19. Dewar cap long sapphire anvil rod hole. 20. Low Temperature Golden Gate™ top plate bridge assembly. 21. Low Temperature Golden Gate™ flat anvil. 22. Clamp part fixing for flat anvil.
  • Page 31 Low Temperature Golden Gate™ ATR 8. Spare Parts for Low Temperature Golden Gate™ Top Plate P/N GS10593 Glass filled PTFE gaskets (white colour) (Pkt of 5) P/N GS10594 High thermal transfer graphite gaskets (grey colour) (Pkt of 20) P/N GS10595 Liquid sample injection device.
  • Page 32 User Manual Notes...
  • Page 33 Low Temperature Golden Gate™ ATR Notes...
  • Page 34 User Manual Notes...
  • Page 35 Tel: 215 793 4044 Japan Fax: 215 793 4011 Systems Engineering Inc. -Tokyo Tel: 03 3946 4993 United Kingdom Fax: 03 3946 4983 Specac Ltd. - London email:systems-eng@systems-eng.co.jp Unit 12, Science & Innovation Centre Website: www.systems-eng.co.jp Halo Business Park Orpington Spain Kent BR5 3FQ Teknokroma S.Coop C.
  • Page 36 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...