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Specac Quest User Manual

Single reflection atr accessory
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The Quest
Single Reflection ATR Accessory
User Manual
2I-10800-8

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  • Page 1 The Quest Single Reflection ATR Accessory User Manual 2I-10800-8...
  • Page 3 The Quest Single Reflection ATR Accessory User Manual 2I-10800-8...

  • Page 4: Table Of Contents

    ™ ........ 7 INSTALLATION USING BENCHMARK BASEPLATE ......8 ALIGNMENT PROCEDURE FOR QUEST ATR ACCESSORY ....8 FITTING OF QUEST ATR CRYSTAL PUCK TO THE OPTICAL UNIT ................12 FINE ALIGNMENT ............. 13 SYNOPTI FOCAL MIRROR SYSTEM ..............14 ALIGNMENT PROCEDURE ...........

  • Page 5: Introduction

    ATR crystal puck assemblies. An IR light beam that is projected towards the ATR crystal is presented at a nominal 45° angle of incidence to the sample surface. As the optical unit of the Quest ATR Accessory consists of mirrors as reflective components only, it allows for as wide a range as possible of the spectral frequency throughput for the specific ATR crystal puck assembly being used.
  • Page 6 The optical unit of the Quest ATR Accessory can be supplied in a variety of different top surface colours on a light grey optical unit. The standard colour is black (B), but there are options of red (R), yellow (Y), orange (O), green (G), aqua (A) and purple (P).

  • Page 7: Safety Considerations

    With respect to safety of use specifically to the Quest ATR Accessory, this uses different crystal materials for the ATR crystal puck assemblies where a sample is bought into contact for analytical spectroscopic study.

  • Page 8: Checklist Of Contents

    3. Checklist of Contents The Quest ATR Accessory is provided in its own specific packaging. Depending on which Quest ATR system (the colour of the optical unit and a specific crystal puck assembly), has been ordered will determine the items to check on delivery.

  • Page 9: Installation Using Benchmark™ Baseplate

    (one flat support pillar towards the rear and two at the front with location pins) and a fourth front central pillar into which the fixing thumb screw (1) of the Quest ATR optical unit is tightened.

  • Page 10: Alignment Procedure For Quest Atr Accessory

    Quest ATR Accessory. To carry out any alignment procedure one of the Quest ATR flat crystal puck assemblies must be fitted to the optical unit.
  • Page 11 P/N GS10810 as an example are shown as Figs 2 and 3. (ZnSe, Ge and Si top plates are similar.) The top surface area of the Quest ATR optical unit for positioning of the ATR crystal pucks, is shown as Fig 4.
  • Page 12 User Manual ATR Crystal Fig 2. Top view of Quest ATR Diamond Crystal Puck Assembly Serial Number Label Crystal Crystal Puck Identification Label Fig 3. Underside view of Quest ATR Diamond Crystal Puck Assembly 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.
  • Page 13 Quest Single Reflection ATR Accessory Fig 4. Top view of Quest ATR Optical Unit showing location area for the Crystal Puck Assemblies The ATR crystal puck assemblies will fit onto the top surface area of the Quest ATR Accessory in one orientation only. Align the location slot (notch) (2) on the underside of the crystal puck (see Fig 3.) with...

  • Page 14: Fine Alignment

    User Manual Fine Alignment With a Quest ATR crystal puck assembly in position on the optical unit and when this completed assembly is installed in the spectrometer on an appropriate Benchmark™ baseplate, the Quest ATR Accessory can be finely aligned. The optical unit front cover plate (5) is removed by undoing the two captive cover plate screws (6) (see Fig 5.) using the...

  • Page 15: Synopti-Focal Mirror System

    ATR crystal puck assembly is positioned for use on the optical unit. The mirror arrangement for an IR beam passage through the Quest ATR Accessory can be seen from the cutaway front view in Fig 6.

  • Page 16: Alignment Procedure

    User Manual The Quest ATR Accessory can be used in any standard spectrometer system irrespective of the beam direction of light through the sample compartment from source to detector. However, for explanation of the internal IR beam passage through the Quest ATR Accessory the...
  • Page 17 Quest Single Reflection ATR Accessory Fig 7. Access to Mirrors M1, M3 and M6 - Cover Plate Removed The grub screw (7) allows for rotation of the M6 mirror and the cap head screw (8) allows for tilt of the M6 mirror, as fitted to the main mirror frame assembly.
  • Page 18 To begin any alignment, first establish that there is a throughput of IR light radiation passing through the system from (S)ource to (D)etector with the Quest ATR Accessory installed correctly on it baseplate in the spectrometer sample compartment and with an ATR crystal puck assembly in position on the optical unit.
  • Page 19 Note: The following procedure can also be adopted if any Quest ATR Accessory to be used is ever found to be out of alignment when installed into a spectrometer system and there is no register of an energy throughput to the detector.
  • Page 20 Having followed steps 2) to 5) from the procedure above, 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 correct fine alignment procedure can now be followed starting with further rotation of mirror M6 as described from step 1) on page 16 of this instruction manual.

  • Page 21: Purging The Quest Atr Optical Unit

    Quest Single Reflection ATR Accessory 6. Purging the Quest ATR Optical Unit When the Quest ATR Accessory has been installed and aligned in the spectrometer there is an option for purging the Quest ATR optical unit if this is necessary.
  • Page 22 To help maintain a purged environment within the optical unit from introduction of a gas via the attached purge tubing, a pair of purge bellows (15) (P/N GS10707) have been supplied with the Quest ATR Accessory for attachment to the optical units two aperture ports (16).

  • Page 23: Fitting The Purge Bellows (P/N Gs10707)

    Accessory in position, measure the distance between the spectrometer source and detector bulkhead/side walls and the side end faces of the Quest ATR optical unit. (This is dimension “‘X”). 2. Using a sharp blade, cut lengths of the flexible purge bellows (15) which are equivalent to the measured length (“X”) allowing for an...

  • Page 24: Quest Atr Anvils And Clamp Anvil Arm Assembly

    Choice of Anvils and their Uses There are two different compression head anvils (17) that can be used with the Quest ATR Accessory when fitted to the clamp arm assembly (18). The anvil type and its uses are tabulated as follows:...

  • Page 25: Clamp Anvil Arm Assembly

    Fig 13. Anvil in Clamp Anvil Arm Assembly and in Storage Port Clamp Anvil Arm Assembly When using the Quest ATR Accessory, a liquid or solid sample is placed onto the crystal surface area of the flat ATR crystal puck assembly being used to obtain an ATR spectrum for the sample.
  • Page 26 User Manual Fig 14. Clamp Arm Assembly with Flat Anvil in Sampling Position If the clamp arm assembly is not required for sampling it can be rotated to a “parked” position to either the left or right side of the central post. As seen in the example image for Fig 13.

  • Page 27: Torque Limiter Screw Knob Assembly

    Quest Single Reflection ATR Accessory Torque Limiter Screw Knob Assembly The Quest ATR clamp arm assembly (18) is provided with a special built in torque limiter screw knob assembly (20). (See Figs 13. and 14.) For solid sampling, an appropriate anvil (17) is fitted in position. A solid...

  • Page 28: Sampling Using The Quest Atr Accessory

    8. Sampling Using the Quest ATR Accessory Important Note for Usage! The diamond, ZnSe, Ge and Si crystals in the Quest ATR crystal puck assemblies have a specific hardness and chemical resistance and should be treated accordingly. The crystals have been sealed into position to the stainless steel top plate mounting using Indium material.

  • Page 29: Collecting Atr Spectra Of Powder Samples

    Collecting a Background Spectrum 1. Choose a diamond, ZnSe, Ge or Si ATR crystal puck assembly to be used on the Quest ATR optical unit and clamp arm assembly. 2. Attach the Quest ATR optical unit to the installed Benchmark™...
  • Page 30 ATR crystal because of the chemical and structural resilience of diamond material. After cleaning (see Notes On Cleaning page 38), the Quest ATR Accessory is ready to accept a new sample for measurement.

  • Page 31: Collecting Atr Spectra Of Flat Solid Samples

    Quest Single Reflection ATR Accessory Collecting ATR Spectra of Flat Solid Samples When analyzing for a flat solid sample it is best to use the self levelling flat anvil (17) of the two anvil options, fitted to the clamp arm assembly (18).

  • Page 32: Collecting Atr Spectra Of Pellet/Bead Samples

    ATR crystal because of the chemical and structural resilience of diamond material. After cleaning (see Notes On Cleaning page 38), the Quest ATR Accessory is ready to accept a new sample for measurement.

  • Page 33: Collecting Atr Spectra Of Fiber Samples

    ATR crystal because of the chemical and structural resilience of diamond material. After cleaning (see Notes On Cleaning page 38), the Quest ATR Accessory is ready to accept a new sample for measurement.
  • Page 34 User Manual Note: When fitted, some movement of the self levelling flat anvil (17) pressing surface is allowable to adjust to the sample shape during compression. This movement enables even pressure to be applied across the sample contact area. 1. Collect a background spectrum as described in steps 1 to 4 (page 27).

  • Page 35: Collecting Atr Spectra Of Liquid And Paste Samples

    ATR crystal because of the chemical and structural resilience of diamond material. After cleaning (see Notes On Cleaning page 38), the Quest ATR Accessory is ready to accept a new sample for measurement.

  • Page 36: The Volatiles Cover (P/N Gs10825)

    Accessory is ready to accept a new sample for measurement. The Volatiles Cover (P/N GS10825) Included with the Quest ATR Accessory is a volatiles cover (21) (P/N GS10825). This is used when sampling volatile liquid samples for a prolonged containment and surface contact with the ATR crystal material from the crystal puck option fitted to the Quest ATR optical unit.
  • Page 37 Quest Single Reflection ATR Accessory the front of the optical unit, ensuring there is enough clearance of the anvil pressing surface from the top side of the volatiles cover (21) that has been placed into position over the crystal. The clamp arm assembly (18) will click correctly into the sampling position over the crystal area when turned towards the front.

  • Page 38: The Specular Reflectance Puck (P/N Gs10816)

    User Manual The Specular Reflectance Puck (P/N GS10816) The Quest ATR Accessory can be used for the spectral measurement of solid sample types such as flat surface films by the specular reflectance technique. A crystal puck assembly (22) that has no ATR...
  • Page 39 Alignment of Optics using the Specular Reflectance Puck When swapping over from use of a Quest ATR puck assembly to the specular reflectance puck (or vice versa), it should not be necessary to realign for the mirror settings in the optical unit. Any alignment of the...

  • Page 40: Notes On Cleaning

    Notes On Cleaning When cleaning a diamond, ZnSe, Ge or Si ATR crystal of the Quest ATR crystal puck assembly in preparation for a new sample, it is very important to take care to avoid damage to the crystal materials. As...
  • Page 41 In common and general usage, it will only be necessary to wipe and clean away at the top surface of any Quest ATR crystal puck between samples. If possible, try to avoid any solvent or cleaning solution materials from getting to the underside of the crystal puck.
  • Page 42 User Manual 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.
  • Page 43 Quest Single Reflection ATR Accessory 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.
  • Page 44 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.
  • Page 45 Quest Single Reflection ATR Accessory Datasheet 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 46: Quest Atr Accessory Part Identification List

    User Manual 9. Quest ATR Accessory “Bubble Numbers” Part Identification List (1) Optical unit fixing thumb screw to Benchmark™ baseplate. (2) Location slot of ATR crystal puck assemblies. (3) Location pin on top surface of the optical unit. (4) Magnetic catch for ATR crystal puck assemblies.

  • Page 47: Quest Atr Accessory Spare Parts

    P/N GS10807-X Quest ATR Diamond Extended Range Accessory (DLC Coated). Note: To purchase a Quest ATR Accessory with a specific coloured top surface, specify the appropriate letter for colour coding in place of ‘X ’after the part number when ordering. (See page 4.

  • Page 48: Quest Atr Technical Specifications

    User Manual 11. Quest ATR Technical Specifications ZnSe Diamond ATR Crystal ZnSe 45° Ge 45° Diamond 45° Si 45° Active Area 3.4 mm dia. 3.4 mm dia. 1.8 mm dia. 3.4mm dia Accessory 7,800 - 500 5,500 - 480 7,800 - 400 8,000 –...

  • Page 49: Quest Atr Serial Numbers

    Your Quest ATR Accessory will be provided with a serial number for identification of certain individual part assemblies. To help you, please use the grid below to fill in the serial number information of the Quest ATR Accessory parts you have received. If you need to contact...
  • Page 50 User Manual P/N GS10813 – Ge (AR coated) puck P/N GS10819 – Si (non-AR coated) puck P/N GS10826 – Diamond (AR coated) puck DLC P/N GS10827 – Diamond (extended range) puck DLC...
  • Page 51 Tel: 215 793 4044 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 River House, 97 Cray Avenue, Orpington Spain Kent BR5 4HE Teknokroma S.Coop C. Ltda...
  • Page 52 Brilliant Spectroscopy™ www.specac.com SPECAC INC. SPECAC LTD. 414 Commerce Drive River House, 97 Cray Avenue, Suite 175, Orpington Fort Washington, Kent BR5 4HE PA 19034, USA Tel: +44 (0) 1689 873134 Tel: 215 793 4044 Fax: +44 (0) 1689 878527 Fax: 215 793 4011 Registered No.

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