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Specac Silver Gate, User Manual

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Silver Gate™Evolution 
Single Reflection ATR System 

User Manual 

 
 
 

 

 
 
 

                                                                                 2I-10680 Issue 3

Summary of Contents for Silver Gate

Page 1: ...Silver Gate Evolution Single Reflection ATR System User Manual 2I 10680 Issue 3 ...

Page 2: ......

Page 3: ...Silver Gate Evolution Single Reflection ATR System User Manual 2I 10680 Issue 3 ...

Page 4: ...POLARIZER ROTATOR MOUNT P N GS12510 15 PURGING THE OPTICAL UNIT 16 FITTING THE PURGE BELLOWS P N GS10707 17 6 ANVIL OPTIONS 18 PELLET ANVIL P N GS10532 18 STAINLESS STEEL ANVIL P N GS10567 18 7 SAMPLING USING THE SILVER GATE ACCESSORY 19 GENERAL PINCIPLES 19 FEATURES OF THE BRIDGE AND CLAMP ANVIL ASSEMBLY 19 TORQUE LIMITER SCREW ASSEMBLY 20 QUICK LOCK AND RELEASE MECHANISM 21 STAY UP DEVICE 21 IMP...

Page 5: ...ND PASTE SAMPLES 29 NOTES ON CLEANING 33 8 SILVER GATE ATR BUBBLE NUMBER IDENTIFICATION LIST 34 9 SILVER GATE ATR ACCESSORY SPARE PARTS 35 10 SILVER GATE ATR TECHNICAL SPECIFICATIONS 36 11 SILVER GATE ATR SERIAL NUMBERS 37 Apr 2016 Specac Ltd All rights reserved Silver Gate and Benchmark are trademarks of Specac Ltd Other product names that may be mentioned herein may be trademarks of their respec...

Page 6: ...semblies A complete Silver Gate ATR system consists of an ATR flat or recessed crystal top plate assembly with a ZnSe or Ge crystal at 45 incident angle option fitted to an optical unit with a bridge and clamp anvil assembly This whole assembly is mounted into a spectrometer via a Benchmark type baseplate for correct positioning of the accessory to maximize for an optical throughput signal The ATR...

Page 7: ...assembly for solid or powder sample types although if the sample is small enough the recessed ATR crystal top plate assembly could be used instead When using the bridge and clamping mechanism for pressure application the compression head anvil does not rotate against the sample This ensures that heat is not generated by friction which may cause changes to the sample and the sample is not displaced...

Page 8: ...will include 1 Volatiles cover P N GS10503 1 Pair of purge bellows P N GS10707 1 Stainless steel flat anvil P N GS10567 1 Pellet anvil P N GS10532 With either optical unit assembly 1 ATR crystal top plate assembly choice of ZnSe Ge or Si flat or ZnSe Ge or Si recessed crystal top plate assembly Any additional ATR crystal top plates ordered with the accessory 1 Ball driver 3 0mm 1 Allen key 2 0mm 1...

Page 9: ... and two at the front with location pins and a fourth front central pillar into which the fixing thumb screw 1 of the Silver Gate optical unit is tightened Note It is normally best to install the Benchmark baseplate in the spectrometer first before locating the Silver Gate ATR accessory Fixing holes and studs in the Benchmark baseplate will vary dependant on the make and model of the spectrometer ...

Page 10: ...rystal Top Plate to the Optical Unit Six different versions of Silver Gate ATR crystal top plate assemblies can be fitted to the optical unit They are ZnSe flat crystal top plate assembly P N GS10683 1 Ge flat crystal top plate assembly P N GS10683 2 Si flat crystal top plate assembly P N GS10683 3 ZnSe recessed crystal top plate assembly P N GS10684 1 Ge recessed crystal top plate assembly P N GS...

Page 11: ...er Gate Evolution ATR System 9 Figure 2 Top view of Silver Gate ZnSe Flat ATR Crystal Top Plate Assembly Figure 3 Top view of Silver Gate ZnSe Recessed ATR Crystal Top Plate Assembly ATR Crystal ATR Crystal ...

Page 12: ...User Manual 10 Figure 4 Underside view of Silver Gate ZnSe Flat or Recessed ATR Crystal Top Plate Assembly Figure 5 Top view of Silver Gate Optical Unit without Bridge 2 4 5 3 6 7 ...

Page 13: ...urely in position To remove and swap over with any other ATR crystal top plate assembly just pull up on the ATR crystal top plate to release the magnetic catches Alignment With an ATR crystal top plate assembly in position on the optical unit and when the whole is installed in the spectrometer on an appropriate Benchmark baseplate the Silver Gate Accessory can be finely aligned The optical unit co...

Page 14: ... goes to zero while making any of the adjustments always bring it back with the same adjustment before proceeding further It is always best to start alignment from the output mirror the one nearest the detector In these instructions it is assumed M2 is the output mirror If your output mirror is M1 follow instructions substituting M1 with M2 and vice versa 1 Using the Ball driver tool in screw 8 of...

Page 15: ...ate thumb screws 7 5 If the Benchmark baseplate is mounted on a rail or is movable in the spectrometer move the Silver Gate ATR Accessory on the Benchmark baseplate to find the best position where the transmission is at a maximum Now firmly secure the Benchmark baseplate in this position Note In some spectrometers it may be necessary to remove the Silver Gate optical unit before securing the basep...

Page 16: ...Polarizer Specac P N GS12000 Series Polarizers can be fitted to the apertures 10 of the optical unit The polarizers push fit in these apertures and can be rotated to the desired angular orientation The polarizer will transmit at a maximum perpendicular component of the polarized light when it is mounted so that the notch slot in the polarizer holder ring is in the vertical plane Fitting the polari...

Page 17: ...ried out using any Benchmark baseplate compatible accessory particularly if there is limited space within a spectrometer sample compartment The standard aperture ports of the Benchmark baseplate compatible optical units as item 10 for the Silver Gate optical unit will accept a GS12000 Series polarizer To rotate this type of polarizer it must be removed from the aperture port and turned to align wi...

Page 18: ...lows 12 to the optical unit at the aperture ports 10 See Figure 9 The purge bellows grip fit around the circumference of the aperture ports and bridge any gap between the optical unit and the spectrometer sample compartment bulkheads from the source and to the detector If the gap distance between the optical unit and bulkhead is small the purge bellows can be cut to size It is best to cut all the ...

Page 19: ...llowing an additional 10mm for each Tip It is easier to cut the purge tube between the ridged grooves 3 Unscrew the Silver Gate Optical Unit fixing thumb screw 1 and remove the Silver Gate ATR Accessory from the sample compartment Note Fit a polarizer at this stage if required GS12000 Series or GS12510 Benchmark Compatible Accessory Polarizer Mount 4 Fit the flexible purge bellows 12 over both end...

Page 20: ...ed samples such as polymer beads Relatively soft irregular shaped samples can be used with this anvil on any of the Silver Gate ATR crystal top plate assemblies Figure 10 St Steel Flat Anvil P N GS10567 Figure 11 The stainless steel anvil P N GS10567 should be used generally for all solid and powder samples to bring the sample into good contact with the ZnSe or Ge crystal for any of the ATR crysta...

Page 21: ...oduced when the sample is in close contact with the ATR crystal so it is recommended to use the bridge and clamp anvil assembly 15 of the Silver Gate ATR Accessory on the optical unit In this way a load can be applied to the solid sample from an appropriate compression head anvil 13 fitted to the clamp head pressure pin 14 see Figure 12 to force the sample into good and close contact with the ZnSe...

Page 22: ...f the bridge see Figure 13 Figure 13 Silver Gate direction of T shaped Quick Lock Release knob 18 when bridge is open unlocked and closed locked With an appropriate anvil 13 fitted the torque limiter screw assembly knob 16 is turned in a clockwise fashion to provide a pre determined set pressure 50lbs load spread over the anvil face to the sample In operation the entire torque limiter screw assemb...

Page 23: ... either the flat or recessed ATR crystal top plate assembly there is no need to use the bridge and clamping assembly 15 with any anvil compression heads 13 so the bridge can stay open if desired see Figure 12 Important Note for Usage The ZnSe Ge and Si crystals in both the flat and recessed ATR crystal top plate assemblies have a specific hardness and chemical resistance and should be treated acco...

Page 24: ...ilver Gate optical unit with or without a bridge and clamp anvil assembly 2 Attach the Silver Gate optical unit to the installed Benchmark baseplate and fit the chosen ATR crystal top plate assembly to the optical unit 3 If using a Silver Gate bridge and clamp anvil assembly 15 on the Silver Gate optical unit then choose an appropriate compression head anvil 13 P N GS10567 or P N GS10532 see Figur...

Page 25: ... may scratch the crystal Only a small amount of load pressure should be needed to check for contamination It is not advisable to apply the maximum pressure loading Collecting ATR Spectra of Powder Samples When analyzing for a powder sample it is best to use a flat ATR crystal top plate assembly on a Silver Gate ATR accessory fitted with a bridge and clamp anvil assembly 15 The best anvil 13 to cho...

Page 26: ...le surface Continue rotation until the white cross on the black cover at the top of the torque knob assembly 16 ceases to rotate At this point a maximum load will be applied to the powder sample forcing it against the ATR crystal 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 f...

Page 27: ... flat ATR crystal top plate assembly on a Silver Gate ATR accessory fitted with a bridge and clamp anvil assembly 15 The best anvil 13 to choose would be the stainless steel anvil P N GS10567 See Figure 14 1 Collect a background spectrum as described in steps 1 to 4 page 21 2 Open the bridge 15 and position it past the stay up catch device 19 This allows for easier access to the ATR crystal surfac...

Page 28: ...8 and raising the bridge 15 up past the stay up catch device 19 8 Remove the flat solid sample carefully away from the ATR crystal avoid the possibility of scratching the ATR crystal surface and clean the ATR crystal and stainless steel anvil 13 surfaces After cleaning see Notes on Cleaning page 32 the Silver Gate ATR accessory is ready to accept a new sample for measurement Collecting ATR Spectra...

Page 29: ...diameter or less are not suitable for pressing using the concave recessed pellet anvil 13 Small pellet beads may have to be analysed by careful manipulation using the flat stainless steel anvil 13 instead Beware to avoid any point loading on the ATR crystal with a small pellet bead sample Continue rotation until the white cross on the black cover at the top of the torque knob assembly 16 ceases to...

Page 30: ...t of the stainless steel anvil 13 pressing surface level is allowed 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 21 2 Open the bridge 15 and position it past the stay up catch device 19 This allows for easier access to the ATR crystal surface area t...

Page 31: ...e anvil 13 before undoing the quick lock release screw 18 and raising the bridge 15 up past the stay up catch device 19 8 Remove the fiber sample carefully away from the ATR crystal avoid the possibility of scratching the ATR crystal surface and clean the ATR crystal and stainless steel anvil 13 surfaces After cleaning see Notes on Cleaning page 32 the Silver Gate ATR accessory is ready to accept ...

Page 32: ...plied 20 can be placed over the liquid to contain it during the analysis See Figure 16 Figure 15 Silver Gate ATR Accessory Optical Unit and Recessed ZnSe ATR Top Plate Assembly without Bridge and Clamp Anvil Assembly Figure 16 As Figure 15 but with Volatiles Cover 20 over the Recessed ZnSe ATR Top Plate Assembly 20 ...

Page 33: ...dge in the open unlocked position past the stay up catch device 19 Alternatively the bridge and clamp anvil assembly 15 can be removed completely from the bridge hinge support block 20 by unscrewing a thumb nut 21 for the hinge pin and sliding the hinge pin out of the bridge and support block See Figures 17 and 18 Figure 17 Silver Gate Hinge Block 20 and Thumb Nut 21 which is unscrewed for removal...

Page 34: ...e 15 up showing detail of the stay up catch 19 and stay up support rod 22 For analyzing a liquid or a paste 1 Collect a background spectrum as described in steps 1 to 4 page 21 2 If the Silver Gate ATR Accessory is fitted with a bridge and clamp anvil assembly 15 open the bridge and position it past the stay up catch device 19 This allows for easier access to the ATR crystal surface area to positi...

Page 35: ...asurement Notes on Cleaning When cleaning either a ZnSe Ge or Si ATR crystal of the Silver Gate ATR crystal top plate assemblies in preparation for a new sample it is very important to take care to avoid damaging the crystal materials Always wear gloves to protect yourself and the ATR crystal material Solvents such as water methanol and acetone are suitable to use Avoid the use of halogenated solv...

Page 36: ... 7 Optical unit front cover plate thumb screw 8 Optical unit mirror rotation cap head screw 9 Optical unit mirror tilt grub screw 10 Optical unit aperture port 11 Optical unit purge port tube fitting 12 Purge bellows P N GS10707 13 Anvil stainless steel P N GS10567 pellet P N GS10532 14 Clamp head pressure pin for anvil 15 Bridge and clamp anvil assembly 16 Torque limiter screw assembly knob 17 Br...

Page 37: ...stal top plate assembly P N GS10684 1 Silver Gate Evolution ZnSe recessed ATR crystal top plate assembly P N GS10684 2 Silver Gate Evolution Ge recessed ATR crystal top plate assembly P N GS10684 3 Silver Gate Evolution SI recessed ATR crystal top plate assembly P N GS10532 Pellet anvil P N GS10567 Stainless steel anvil P N GS10503 Volatiles cover P N GS10707 Purge bellows Silver Gate Evolution AT...

Page 38: ... ZnSe glued into anodized aluminium top plate Ge glued into anodized aluminium top plate Si glued into anodized aluminium top plate Applied Force From Bridge Anvil 50 lbs 50 lbs 50 lbs Typical Light Throughput When Aligned Between 20 and 55 Transmission Between 20 and 40 Transmission Between 20 and 45 Transmission Depth of Penetration 2 0µm For Sample of Refractive index 1 5 1000cm 1 0 7µm For Sam...

Page 39: ...ry it may be necessary to provide the serial number of the item to identify for replacement parts Silver Gate Evolution Part Number and Description Serial Number P N s GS10681 and GS10682 1 optical unit and top plate surface without bridge and clamp P N s GS10681 and GS10682 2 optical unit and top plate surface without bridge and clamp P N GS10683 1 ZnSe flat ATR crystal top plate P N GS10683 2 Ge...

Page 40: ...User Manual 38 Notes ...

Page 41: ...Silver Gate Evolution ATR System 39 Notes ...

Page 42: ...User Manual 40 Notes ...

Page 43: ...ystems eng co jp Website www systems eng co jp Spain Teknokroma S Coop C Ltda Barcelona Tel 93 674 8800 Fax 93 675 2405 email comercial teknokroma es Switzerland Portmann InstrumentsAG Biel Benken Tel 061 726 6555 Fax 061 726 6550 email info portmann instruments ch Website www portmann instruments ch USA SPECAC INC 414 Commerce Drive Suite 175 Fort Washington PA 19034 USA Tel 215 793 4044 Fax 215 ...

Page 44: ...SPECAC INC 414 Commerce Drive Suite 175 Fort Washington PA 19034 USA Tel 215 793 4044 Fax 215 793 4011 SPECAC LIMITED River House 97 Cray Avenue Orpington Kent BR5 4HE Tel 44 0 1689 873134 Fax 44 0 1689 878527 Registered No 1008689 England ...

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