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Summary of Contents for Pike MIRacle ATR
- Page 1 Installation and User Guide MIRacle Single Reflection Horizontal ATR Accessory...
- Page 2 This publication may contain or reference information and products protected by copyrights or patents and does not convey any license under the patent rights of PIKE Technologies, Inc. nor the rights of others. PIKE Technologies, Inc. does not assume any liability arising out of any infringements of patents or other rights of third parties.
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Page 3: Table Of Contents
Contents Introduction MIRacle ATR Accessory MIRacle Pressure Clamp Options MIRacle Universal Plate Options Installation Accessory Adjustment Performance Verification Sampling Procedures Configuration for Liquid Sampling Configuration for Solid Sampling Pressure Clamp Tip Attachments Micrometer Pressure Clamp High-Pressure Clamps High-Pressure Clamp Installation... -
Page 4: Introduction
Introduction The PIKE Technologies MIRacle™ is a patented Universal Sampling Accessory designed for single- or multi-reflection attenuated total reflectance (ATR) and specular reflectance measurements with FTIR spectrometers. The accessory features a unique optical design (US.PAT: 5,965,889 and 6,128,075), which provides exceptional sensitivity and IR throughput. The single-reflection sampling plate of the accessory has a 1.8 mm round crystal surface allowing reliable analysis of small samples. -
Page 5: Miracle Atr Accessory
MIRacle ATR Accessory Figure 3. MIRacle base optics assembly with purge tubes* * The MIRacle base optics assembly has the crystal plate and purge tubes attached to the base. Some base optics assemblies may appear different (such as adjustment screw locations and mounting scheme). -
Page 6: Miracle Universal Plate Options
Plate Installation The MIRacle accessory has been aligned and tested in the PIKE Technologies facility to ensure that it performs to specifications. However, some variation in optical alignment can occur from spectrometer to spectrometer. To allow for this difference, there are four alignment screws provided on the MIRacle base optics assembly for fine-tuning once the accessory is installed in the spectrometer. -
Page 7: Accessory Adjustment
Accessory Adjustment The MIRacle accessory may not require any alignment when installed. However, should you choose to fine-tune the accessory, refer to this figure and follow these steps: 1. Display the live interferogram on the spectrometer monitor and using the thumbscrews on the left and right side of the accessory (angle adjustment), adjust the mirrors until the highest throughput is achieved. -
Page 8: Performance Verification
2. Place the MIRacle accessory in the instrument per installation steps described on page 4. 3. Collect a spectrum of the MIRacle ATR using the same collection parameters as used to collect the background spectrum. The following are the % transmission values the accessory should achieve with different crystal... - Page 9 ZnSe Crystal Plate, Throughput Figure 5. MIRacle ATR throughput for the ZnSe crystal plate Diamond/ZnSe Crystal Plate, Throughput Figure 6. MIRacle ATR throughput for the diamond/ZnSe crystal plate PN 350-025004-09 P a g e...
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Page 10: Sampling Procedures
The spectrum of the required sample is obtained by ratioing a scan with a sample in place to a scan with no sample on the face of the crystal. The crystal mount is located on the base unit. The MIRacle ATR can be used for all types of samples (liquids, pastes, soft pliable films, powders and solids). -
Page 11: Configuration For Solid Sampling
material and discoloration of the metal plate can occur. Once the measurement has been made, remove the sample from the crystal and clean the surface of the crystal and the surrounding plate area with a suitable solvent. NOTE: The MIRacle high-pressure clamps have the ability to swing sideways for ease of accessing the crystal surface for cleaning. -
Page 12: Pressure Clamp Tip Attachments
Pressure Clamp Tip Attachments Swivel Tip Flat Tip Concave Tip The success of an ATR measurement depends upon the quality of the contact between the sample and the crystal. Since there is an infinite number of sample shapes and types, a single configuration of the sample press tip may not be adequate. -
Page 13: Micrometer Pressure Clamp
Micrometer Pressure Clamp The micrometer clamp assembly consists of the base which attaches directly to the accessory top plate and the “r” shaped arm with control knobs for raising and lowering the sample press. The clamp itself is a stainless steel barrel with the integrated micrometer screw at the top and the spring-loaded plunger at the bottom. -
Page 14: High-Pressure Clamps
High-Pressure Clamps The high-pressure clamps consist of the base which attaches directly to the accessory’s top plate, the stainless steel pressure tip arm and the pressure control knob with built in slip-clutch mechanism. A removable anvil is located underneath the pressure module. This anvil is positioned in the center of the crystal plate and provides direct pressure to the sample. -
Page 15: Atr Spectrum
The ATR Spectrum ATR spectra are similar to transmission spectra. A careful comparison of ATR spectra and transmission spectra reveals that the intensities of the spectral features in an ATR spectrum are of lower absorbance than the corresponding features in a transmission spectrum and especially in the high wavenumber (short wavelength) region of the spectrum. -
Page 16: Atr Correction
ATR Correction If an ATR spectrum representative of a transmission spectrum is desired, the ATR spectrum must be processed with the ATR correction program available on your spectrometer software. An example of the effect of this correction on a spectrum is shown in the following example for polystyrene. The middle spectrum is the original ATR spectrum of polystyrene. -
Page 17: Liquid Samples
Liquid Samples One minute, 4 cm resolution spectra of a dilute detergent solution and distilled water were collected using the MIRacle with diamond crystal. These samples were simply applied directly onto the MIRacle diamond ATR crystal for analysis. The red spectrum is the detergent solution and the blue spectrum is that for distilled water. A spectral subtraction can be applied to obtain the spectrum of the detergent component. -
Page 18: Useful Equations
Useful Equations The depth of penetration gives us a relative measure of the intensity of the resulting spectrum and is expressed by the following equation: λ 2π ( n sin θ – n ) Where λ is the wavelength of light, n is the refractive index of the crystal, n is the refractive index of the sample and θ... -
Page 19: Germanium
Germanium Germanium (Ge) has been used extensively in the past as a higher refractive index material for samples that have a high refractive index, such as carbon filled samples. The down side of using Ge is the high refractive index produces a relatively weaker spectral absorbance compared to ZnSe or diamond. Silicon Silicon is hard and brittle. -
Page 20: Specifications
MIRacle ATR crystal. Apply only room temperature samples to MIRacle 3- and 9-reflection ATR plates. Please contact PIKE Technologies if you wish to place samples of a higher temperature on the crystal surface. Heated MIRacle plates are also available and can be heated up to 130 °C (60 °C for diamond). -
Page 21: Precautions
Precautions Mirrors In order to provide the maximum transmission in the infrared, with the minimum spectral interferences, the mirrors used in this device are uncoated (bare) aluminum on a glass substrate. Since the coatings are soft, care must be taken to avoid damage. Normally, these mirrors will not need cleaning, since they are contained within the housing of the accessory. -
Page 22: Replacement Parts And Options
025-4000 Reconditioned Single Reflection Diamond/ZnSe Crystal Plate NOTE: To use this option please call PIKE Technologies to get a return material authorization (RMA) number to send your existing crystal plate to us for restoration to like new condition. HEATED CRYSTAL PLATES... - Page 23 PRESSURE CLAMPS 025-3020 MIRacle High-Pressure Clamp 025-3035 MIRacle Confined Space Clamp 025-3050 Micrometric, Low-Pressure Clamp 076-6025 Digital Force Adapter for High-Pressure Clamp OTHER 025-3053 Micrometer Controlled Press Tips Assortment 025-3099 High-Pressure Clamp Tip Assortment 025-3098 High-Pressure Tip Mount 026-5012 Flow-Through Attachment, sample volume 100 µL 026-5013 Liquids Retainer and Volatiles Cover Set 026-3051...
- Page 24 6125 Cottonwood Drive · Madison, WI 53719-5120 · (608) 274-2721 (TEL) · (608) 274-0103 (FAX) info@piketech.com · www.piketech.com...
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