Installation and User Guide

MIRacle Single Reflection

TM

Horizontal ATR Accessory

The information in this publication is provided for reference only. All
information contained in this publication is believed to be correct and
complete. PIKE Technologies, Inc. shall not be liable for errors contained herein
nor for incidental or consequential damages in connection with the furnishing,
performance, or use of this material. All product specifications, as well as the
information contained in this publication, are subject to change without notice.
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.
This document contains confidential or proprietary information of PIKE
Technologies, Inc. Neither this document nor the information herein is to be
reproduced, distributed, used or disclosed, either in whole or in part, except as
specifically authorized by PIKE Technologies, Inc.
PIKE Technologies, Inc. makes no warranty of any kind with regard to this
material including, but not limited to, the implied warranties of merchantability
and fitness for a particular purpose.
Copyright 1991-2018 by PIKE Technologies, Inc., Madison, WI 53719. Printed in
the United States of America. All world rights reserved. No part of this
publication may be stored in a retrieval system, transmitted, or reproduced in
any way, including but not limited to, photocopy, photograph, magnetic or
other record, without the prior written permission of PIKE Technologies, Inc.

Address Comments to:

PIKE Technologies, Inc.

6125 Cottonwood Drive
Madison, WI 53719

Phone (608) 274-2721

Fax (608) 274-0103
E-mail [email protected]
Web Site www.piketech.com

Jan. 1, 2018
 Contents
Introduction 2
MIRacle ATR Accessory 3
MIRacle Pressure Clamp Options 3
MIRacle Universal Plate Options 4
Installation 4
Accessory Adjustment 5
Performance Verification 6
Sampling Procedures 8
Configuration for Liquid Sampling 8
Configuration for Solid Sampling 9
Pressure Clamp Tip Attachments 10
Micrometer Pressure Clamp 11
High-Pressure Clamps 12
High-Pressure Clamp Installation 12
Crystal Cleaning 12
ATR Spectrum 13
ATR Correction 14
Liquid Samples 15
Solid Samples 15
Useful Equations 16
Materials 16
Zinc Selenide 16
Germanium 17
Silicon 17
Diamond 17
Specifications 18
Effects of Temperature 18
Precautions 19
Mirrors 19
SAFETY 19
Replacement Parts and Options 20

PN 350-025004-10
P a g e |1
Introduction
The PIKE Technologies MIRacle™ is a patented Universal Sampling Accessory designed for single or
multiple 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. Solid materials can be put
into intimate physical contact with the sampling area through high-pressure clamping, yielding high-
quality, reproducible spectra.

ATR crystal plates come in several configurations, including ZnSe, Ge, Si or diamond. The first three
options are suitable for analysis of liquids, semi-liquid materials and pliable solids. The Si or diamond
configurations should be used when working with reactive samples and/or abrasive solid materials that
need to be pressed hard against the crystal. Single reflection ATR works very well for the analysis of
relatively strong absorbing substances (e.g. polymers, rubber, paint chips, fibers, etc.). Highly absorbing
samples, such as black rubber, are best analyzed using the Ge plate due to its lower depth of penetration.
Acidic samples are best handled with Ge, Si or diamond crystal plates. For samples with relatively lower
absorption characteristics or when trace elements are present, the 3- and 9-Reflection ATR Plates are also
available in most crystal materials. Also, the MIRacle Specular Reflection Plate provides even more
flexibility for 45° specular reflection work without the need to change the accessory base.

The compact design of the accessory employs a transfer mirror to direct the infrared beam to one end of
an IR transmitting ATR crystal. A second mirror directs the beam emitted from the other end of the
MIRacle plate to the detector built into your FTIR spectrometer. The MIRacle features a universal
sampling plate design that eliminates the need for separate trough and flat plates, such as normally
required in ATR for handling liquid and solid samples, respectively. The accessory can be equipped with
a wide choice of compression clamps including micrometer controlled, high-pressure, rotating high-
pressure and digital readout high-pressure. Included as standard are the base optics assembly with
purge tubes specific to your FTIR spectrometer model, purge tubing attachments and adjustment
wrench set. Add to this your choice of MIRacle universal plate(s) and pressure clamp(s), all of which are
easily interchangeable.

Sampling Area Crystal Plate

Pressure Tip

Figure 1. High-Pressure Clamp Figure 2. Base Optics

PN 350-025004-10
P a g e |2
 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).

The purge tubing kit, wrench set, pressure clamp and tips are packed separately in the carrying case. The
purge tubing kit is not included with some models equipped with recognition bases. The flat tip is
attached to the sample clamp assembly, and the flat and swivel tips are included with the packaging.

MIRacle Pressure Clamp Options

Digital Meter with Digital High-Pressure Clamp High-Pressure Clamp Confined Space Clamp Micrometer Clamp

PN 350-025004-10
P a g e |3
NOTE: Tip of swivel tips and 3-reflection plates for Micrometer clamp are made of
(white) plastic; Swivel tip for high-pressure clamps are stainless steel. Depending
upon specific clamp, the pressure tips may appear different than the picture.

MIRacle Universal Plate Options

Single Reflection 3-Reflection Plate 9-Reflection Specular Reflection

Crystal Plate (Includes 7.8 mm swivel tip) Trough Plate 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. The following is
the procedure for accessory installation and final alignment.

1. The MIRacle accessory fits into the sample compartment of the FTIR spectrometer. Your MIRacle is
set to an appropriate configuration to fit the sample compartment of the FTIR instrument you
specified. Before inserting the accessory into the sample compartment, ensure that your
spectrometer is aligned. If the instrument is not aligned, follow the manufacturer’s instructions for
maximizing the interferogram signal (the IR energy throughput) of your FTIR spectrometer. In order
to locate the accessory in the correct position, simply place the entire accessory into the FTIR
sample compartment with the PIKE MIRacle label facing the front and line up the base plate
provided with the holes/pins in your FTIR Spectrometer.

2. Fasten the accessory onto the FTIR sample compartment base plate using the captive screw(s)
located on the MIRacle base plate (some accessories may have two mounting screws or a mounting
screw/pin combination, depending on spectrometer configuration).

3. Tighten the captive mounting screw (with flat head screwdriver or by hand) to firmly position the
accessory base onto the FTIR sample compartment base plate. The MIRacle accessory is now ready
for optical alignment.

PN 350-025004-10
P a g e |4
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. To do this, turn the screws one at a time slightly and check the signal. If it increases,
reverse turn until the maximum signal is obtained.

2. Insert the enclosed hex wrench in the two height adjustment screws on the top of the accessory.
Adjust the screws one at a time until the highest throughput is obtained.

3. Repeat the entire procedure two or three times to fine-tune the accessory.

NOTE: For some side focus FTIR models, both thumbscrews are located on the right side of the MIRacle
base optics assembly.

This is a one-time alignment procedure that optimizes the MIRacle to work with an individual optical
bench. Once completed, the alignment does not have to be repeated unless the accessory adjustments
have been moved or it has been placed in a different FTIR instrument. You are now ready to verify the
MIRacle optical throughput performance.

Height adjustment

Angle adjustment

Figure 4. Fine-tuning the MIRacle accessory

PN 350-025004-10
P a g e |5
Performance Verification
1. With the accessory removed from the sample compartment, collect an open beam background
spectrum.

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
configurations at 1000 cm-1 (with the exception of the Si value which is shown at 2000 cm-1).

ZnSe Single Reflection ATR Plate Greater than 22%T

Ge Single Reflection ATR Plate Greater than 25%T

Diamond w/ZnSe lens Single Reflection ATR Plate Greater than 25%T

ZnSe 3-Reflection ATR Plate Greater than 12%T

Diamond w/ZnSe lens 3-Reflection ATR Plate Greater than 12%T
Specular Reflection Plate Greater than 20%T

Diamond w/ZnSe lens 9-Reflection ATR Plate Greater than 6%T

The MIRacle ATR throughput spectra appear different and show different spectral features depending
upon the crystal material. One notable feature is the spectra range cut-off (where IR throughput goes to
zero) at the long wavelength end of the spectrum (near 400 cm-1).

In the spectrum shown for the ZnSe crystal plate the long wavelength cut-off is about 520 cm-1. Also
shown in this spectrum is that the IR throughput is about 32% at 1000 cm-1.

A feature in the diamond ATR crystal plates and present in the spectrum shown on the following page is
known as the diamond phonon broad IR absorbance bands, which appear between 2600 and 1900 cm-1.
This is a normal absorbance present in all diamond spectra. This feature ratios well in a typical sample
spectrum. It does, however, reduce the signal-to-noise ratio (SNR) in this spectral region.

If your accessory does not meet this minimum transmission level, please contact PIKE Technologies.
Before calling, please record the serial number located on the label on the back of the MIRacle base
optics assembly.

NOTE: IR throughput performance of your accessory will decrease slowly over time as the lens surface is
exposed to the environment and due to normal wear from cleaning the ATR surface. Contact PIKE
Technologies for information about MIRacle crystal plate reconditioning services when throughput drops
below a usable level.

PN 350-025004-10
P a g e |6
 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 350-025004-10
P a g e |7
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).

Configuration for Liquid Sampling

The crystal plate assembly of the MIRacle single reflection ATR features a round plate design, with a
1.8 mm sampling area, located in the center (6.0 mm for 3-reflection plates). The sample must be in
intimate contact with the sampling area in order to obtain an FTIR spectrum. For routine sampling, place
a drop of your sample on the ATR crystal and collect data. Care is required when removing the sample
from the crystal. It is desired that the sample be removed without scratching the surface of the crystal.

Bridge
Volatiles
Cover

Retainer
Dish

Liquids Retainer Liquids Retainer with Volatiles Cover

An optional liquids retainer and volatiles cover are available for quickly-evaporating liquid samples. For
volatile liquids, the liquid retainer with volatiles cover reduces the amount of evaporation of the sample
on the surface of the crystal. To use, place the retainer disk over the ATR crystal. Place the U-shaped
bridge over the retainer disk. Apply pressure to the U-shaped bridge using the pressure clamp. Fill the
reservoir of the liquid retainer with the volatile liquid. Slide the volatiles cover between the retainer disk
and the U-shaped bridge. Liquids retainer may be used with the high-pressure clamp only.

NOTE: Some crystals used in the accessory are made of fairly brittle materials (such as ZnSe, Si, or Ge).
Scratches on the surface of the crystal will result in a reduction in the throughput of the accessory.

Remove the sample gently with a non-abrasive cotton tissue and rinse with solvent. For more thorough
cleaning, the crystal plate should be cleaned with an appropriate mild solvent such as isopropyl alcohol
or a stronger solvent, such as acetone. Cotton swabs are highly recommended for ease of cleaning
without scratching the soft ATR surface. Sometimes “carry over” may occur from one sample to another
due to incomplete cleaning of a prior sample from the face of the crystal.

PN 350-025004-10
P a g e |8
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.

IMPORTANT: Samples should not be left in contact with the crystal for an extended period
of time since some samples may degrade the crystal material and discoloration of the metal
plate can occur.

NOTE: The MIRacle high-pressure clamp has the ability to swing sideways for ease of accessing the
crystal surface for cleaning.

Configuration for Solid Sampling

For measurements of soft, pliable films and select solid samples, the sample is placed onto the surface
of the crystal. Since the ATR effect only takes place very close to the surface of the crystal, an intimate
contact has to be made by the sample on the ATR crystal surface. This is achieved by using the pressure
clamp ordered with your MIRacle system. Mount the pressure clamp to the backside of the accessory
using the two alignment dowel pins on top of the MIRacle base and fasten using the two captive
thumbscrews on the clamp frame. With the sample in place on the crystal, lower the pressure tip so that
it is in contact with the sample. With the micrometer clamp or digital readout high-pressure clamp, it is
possible to achieve reproducible sampling by applying the same amount of pressure to your samples.
This is done by using the same settings on the micrometer screw or by using the electronic digital
display, respectively. However, in most cases, it is recommended to apply the maximum pressure
allowed to ensure the best contact and highest sampling sensitivity. The maximum force applied by the
micrometer pressure clamp is 8 pounds (>2000 psi). The maximum force applied by the high-pressure
clamps is 40 pounds (>10,000 psi). The high-pressure clamps have the additional advantage of a slip
clutch mechanism to avoid overtightening.

CAUTION: Care must be used in operating the pressure clamps since the pressure device may slide the
sample over the crystal. If the sample contains grit or abrasive materials, the sample motion may
damage the surface of the crystal while pressure is being applied. Ensure that the sample remains
stationary while applying load to the clamp. In addition, softer ATR materials, such as ZnSe, need to be
handled with care when running hard or sharp sample types. Do not apply the maximum pressure to
these types of samples on softer ATR plates to avoid scratching or denting.

PN 350-025004-10
P a g e |9
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. For this reason, the MIRacle pressure clamp is designed to
accept three different tip attachments, providing the best possible configuration for any given sample.
In addition, the 3-reflection ATR plates are provided with a special plastic swivel tip matching its 6-mm
diameter crystal size.

The swivel tip features an end cap mounted onto a small ball joint. Such design allows the press tip to
move and adjust its position to the shape of the sample and maintain the sample position parallel to the
crystal surface. This tip allows for better positioning and optimal contact of thin materials with the ATR
crystal surface. The swivel tip is used with irregularly-shaped samples, films and semi-rigid polymers.

The flat tip attachment is a flat-tipped cone and it is used when analyzing thin films, fibers, small
particles, rubber samples and other elastic polymers. The flat tip may also be used for powdered
samples.

The concave tip was developed specifically to work with granules, large beads and polymer pellets.
The tip features a concave surface, which prevents the sample from escaping from underneath the
press. It also forces the spherical samples to stay in the center of the crystal assuring maximum IR signal
strength.

IMPORTANT: Do not use the concave tip for powdered samples or samples which do
not completely protect the concave edges of the steel tip from pressing against the
crystal - this willdamage the ATR crystal.

PN 350-025004-10
P a g e | 10
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. A spring is located between the shaft of the micrometer screw and the plunger. The spring
tension can be adjusted by changing the position of the micrometer screw. This adjustment allows
application of higher or lower pressure to the sample placed on the accessory’s sampling plate. The
numbers on the scale of the micrometer screw serve as reference (they do not indicate the actual
pressure applied to the sample). The actual pressure per square inch (psi) depends on the size of the tip
attached to the press and the spring tension. Listed below are the approximate pressures calculated for
the square edge stainless steel tip (diameter 0.125").

Micrometer Setting Pressure (psi)

3.0 408
2.0 530
1.0 693
0.0 815

Lighter pressures should be used for soft, flexible samples. Higher pressures are necessary for hard
polymers, bids, granules, etc. (please see also the note on selection of pressure clamp tips on page 10).
The following is a short procedure outlining proper use of the MIRacle micrometer controlled sample
clamp (PN 025-3029):

1. Select the appropriate tip and attach it to the press.

2. Position the sample on the accessory plate.

3. Set the micrometer screw to 2.0.

4. Lower the press barrel with the control knobs until the edge of the sampling tip touches the lower
brass end of the barrel.

5. Collect the sample spectrum.

Some FTIR spectrometers offer a “spectrum preview” data collection mode. If available, you can
experimentally determine the best pressure for your particular sample by observing the intensity of the
spectrum while adjusting the micrometer screw.

NOTE: The spring in the clamp assembly is not compressed until the micrometer screw is set to 3.5. For
this reason, always keep the micrometer setting between 3.5 and 0.

PN 350-025004-10
P a g e | 11
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. The pressure clamp module rides up and down
on a lead screw located in the clamp column, with its position adjusted by the control knob. The control
knob features a ratchet-type clutch mechanism that controls the maximum allowable pressure and
protects the crystal from overtightening.

High-Pressure Clamp Installation

1. Position the clamp on the two dowel pins located on the top plate of the MIRacle accessory. Please
note that the top plate extends approximately 1/4" beyond the MIRacle base. The clamp mount
provides a space to accommodate for this extension. Before the clamp can be fully mounted on the
pins, the plate extension and the groove in the clamp mount must be perfectly aligned.

2. Press the clamp down until the pins fully engage. Using a hex driver, tighten the hex screws so the
clamp is firmly attached to the accessory base.

3. As with the micrometer pressure clamp, the high-pressure clamps are provided with three
pressure tips; swivel, flat and concave. However, the swivel tip for the micrometer clamp is
made of plastic whereas the one for the high-pressure clamp is made of metal due to the higher
sampling forces involved.

4. The clamp is now ready for use.

The high-pressure clamp model is able to swing to the side for ease of cleaning. The slip clutch knob is
used for applying pressure to the sample without overtightening. A detent holds the pressure clamp tip
in place directly over the crystal.

Crystal Cleaning
The solvent used for cleaning your crystal is determined by the sample that was analyzed. In all cases it
is best to attempt to clean the crystal with the mildest solvent possible. For most cases, the preferred
solvent is isopropyl alcohol. If a stronger solvent is required, acetone may be used. In all cases when
using solvents, inspect the materials safety data sheet associated with the solvent you are using and
comply with any recommended handling procedures. Apply the solvent to the crystal with a cotton swab
and gently remove using a cotton swab or non-abrasive wipe. Repeat this procedure until all traces of
the sample have been removed. Under no circumstances should softer crystal materials (ZnSe, Ge) be
rubbed with paper products such as Kleenex® or Kimwipes®. Many paper products are abrasive and
could cause scratching of the softer crystal surfaces.

CAUTION: Do not submerge the crystal plate or allow liquid to flow over the top of the
crystal plate. This will damage sensitive optics.

PN 350-025004-10
P a g e | 12
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. The intensity of the ATR spectrum is relative to the
penetration depth of the evanescent wave into the sample. This depth is dependent upon the refractive
index of the crystal and the sample, and upon the wavelength of the IR radiation.

The relatively thin depth of penetration of the IR beam into the sample creates the main benefit of ATR
sampling. This is in contrast to traditional FTIR sampling by transmission where the sample must be
diluted with IR transparent salt, pressed into a pellet or pressed to a thin film, prior to analysis to
prevent totally absorbing IR bands.

A comparison of transmission vs. ATR sampling results for a thick polymer sample is shown below where
the sample is too thick for high-quality transmission analysis (lower blue spectrum). In transmission
spectroscopy, the IR beam passes through the sample and the effective path length is determined by the
thickness of the sample and its orientation to the directional plane of the IR beam. Clearly in this
example the sample is too thick for transmission analysis because most of the IR bands are totally
absorbing. However, simply placing the thick sample on the ATR crystal and applying pressure generates
a high-quality spectral result (upper red spectrum) ‒ identified by library search as a polybutylene
terephthalate. The total analysis time for the thick polymer by ATR was less than one minute.

Thick Polymer by ATR

Thick Polymer by Transmission

Figure 7. Thick polymer sample FTIR spectrum collected by ATR (red) and transmission (blue).

PN 350-025004-10
P a g e | 13
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 in your spectrometer software. 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. The lower spectrum is the transmission spectrum of polystyrene.
Clearly the IR bands around 3000 cm-1 in the ATR spectrum are weaker relative to the IR bands at longer
wavelength.

However, in the upper red spectrum after ATR correction, the relative IR band intensities are very similar
to those from the polystyrene run by transmission.

Polystyrene, ATR-corrected

Polystyrene, ATR, original spectrum

Polystyrene, 1.5 mil. film, by transmission

Figure 8. ATR-corrected polystyrene spectrum.

PN 350-025004-10
P a g e | 14
Liquid Samples

One minute, 4 cm-1 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.

Detergent Solution
Distilled H20

Figure 9. Liquid detergent and distilled water spectra.

Solid Samples
For the analysis of solid samples the pressure clamp for the MIRacle is required. The sample is placed
face down onto the diamond crystal and force is applied to make intimate contact onto the ATR crystal.
The MIRacle accessory enables positioning of the sample to a feature area to ensure that the spectrum
collected is taken from the desired location on the sample.

PN 350-025004-10
P a g e | 15
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
dp =
2π ( n1 sin2 θ – n 22 ) 1/2
2

Where λ is the wavelength of light, n1 is the refractive index of the crystal, n2 is the refractive index of
the sample and θ is the effective angle of incidence.

Depth of penetration in microns as a function of crystal material is shown in the table below. The
penetration depth is calculated for a sample with a refractive index of 1.5 at 1000 cm-1. Also the safe pH
range of samples for use with each material is listed.

Materials
-1 Refractive Depth of
MIRacle Hardness Cuttoff cm , pH Range
Application 2 Index @ Penetration
Crystal Plate kgf/mm Spectral Range -1 of Sample
1000 cm @ 45°, µ
Ideal for hard samples,
Diamond/ZnSe 5700 525 2.4 2.00 1–14
acids or alkaline

When you need full mid-IR

Diamond/KRS-5 5700 250 2.4 2.00 1–14
spectral range

General purpose and

Ge 550 575 4.0 0.66 1–14
carbon filled or rubber

Excellent for far-IR spectral 8900-1500,

Si 1150 3.4 0.85 1–12
measurement 475-40
General purpose ATR
ZnSe 120 520 2.4 2.00 5-9
crystal
NOTE: Quoted spectral range also depends upon the FT-IR spectrometer configuration of source,
beamsplitter, detector and other components.

Zinc Selenide
Zinc Selenide (ZnSe) is the preferred replacement for KRS-5 for all routine applications. Its useful spectral
range is less at the low frequency end than that of KRS-5, but the mechanical strength of this rigid, hard
crystalline material is superior. Although a general-purpose material, it has limited use with strong acids
and alkalies. The surface becomes etched during prolonged exposure to extremes of pH (the acceptable
pH range is 5-9).

Note: Complexing agents, such as ammonia and EDTA, will erode its surface because of the formation
of complexes.

PN 350-025004-10
P a g e | 16
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 disadvantage of using Ge is the high
refractive index produces a relatively weaker spectral absorbance compared to ZnSe or diamond.

Silicon
Silicon (Si) is hard and brittle. It is chemically inert and only strong oxidizers affect it. Si is well suited for
applications requiring temperature changes as it withstands thermal shock better than other ATR
materials. It is also the hardest crystal material offered except for diamond, which makes it well suited
for abrasive samples that might otherwise scratch softer crystal materials. Typically, Si crystal is totally
absorbing below 1500 cm-1, limiting its usefulness in the mid-IR range.

Diamond
Diamond is one of the most rugged optical materials. It can be used for analysis of a wide range of
samples, including acids, bases, and oxidizing agents. Diamond is scratch and abrasion resistant. Its
disadvantage is the cost and the intrinsic absorption from approximately 2300 to 1800 cm-1, which limits
its usefulness in this region (5% transmission).

PN 350-025004-10
P a g e | 17
Specifications
ATR Crystal Choices Diamond/ZnSe, diamond/KRS-5, Ge, ZnSe, Si
Crystal Plate Mounting User-changeable plates
Crystal Plate Mount Stainless steel
Angle of Incidence 45 degrees, nominal
Crystal Dimensions, Surface 1.8 mm (single reflection), 6.0 mm (multiple reflection)
Pressure Device Rotating, continuously variable pressure; click stop at maximum.
Load cell sensor for precise and reproducible pressure control.
Digital Force Adapter (option)
Attaches directly to MIRacle clamp. Digital readout.
Maximum Pressure 10,000 psi (single reflection)
Sample Access 55 mm, ATR crystal to pressure mount
Heating Options Ambient to 60 or 130 °C maximum
Accuracy +/- 0.5%
Sensor Type 3 wire Pt RTD (low drift, high stability)
Digital or digital with PC control (unlimited ramps, automated
Temperature Control
data collection, USB interface)
Input Voltage 90-264 VAC, auto setting, external power supply
Operating Voltage 2.5 A/24 VDC/50 W
Specular Reflection Option Optional, 45 degree nominal angle of incidence
Accessory Dimensions (W x D x H) 104 x 103 x 210 mm (excludes FTIR baseplate and mount)

Effects of Temperature
The PIKE Technologies MIRacle utilizes a metallic gasket to seal the crystal to its mount. This sealing
mechanism allows some flexibility and hot samples may be placed on the crystal without damaging the
crystal or seal. However, it is recommended that the temperature difference between the sample and
the crystal be no more than 30 °C. So for a crystal at room temperature, the sample may be at a
temperature of up to 50 °C. Do not exceed sample temperature greater than 60 °C when using the
single reflection diamond 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).

PN 350-025004-10
P a g e | 18
Precautions
Mirrors

In order to provide maximum transmission in the infrared, with 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. If they do need cleaning, they may be gently wiped with
a lint-free, abrasive-free cloth, such as lens tissue, or with a camel hairbrush. Under no circumstances
should the mirrors be rubbed with paper products such as “Kleenex” since this will scratch the mirror
surface resulting in reduced IR throughput.

SAFETY

Caution should be used when handling and using ATR crystals since some of the materials can be
hazardous. Specifically, zinc selenide is a heavy metal material and should be handled with this in mind.
If the crystal is broken or pulverized, the dust may be harmful by inhalation, ingestion or skin
absorption.

PN 350-025004-10
P a g e | 19
Replacement Parts and Options

The following replacement parts and options are available. If you do not see required items on this list,
please contact PIKE.

ADDITIONAL CRYSTAL PLATES

025-2018 ZnSe Performance Crystal Plate
025-2058 Ge Performance Crystal Plate
025-2098 Si Performance Crystal Plate
025-2028 Diamond/KRS-5 Performance Crystal Plate
025-2027 Diamond/KRS-5 HS Performance Crystal Plate
025-2107 Diamond/ZnSe HS Performance Crystal Plate
025-2108 Diamond/ZnSe Performance Crystal Plate
025-2118 3-Reflection Diamond/ZnSe Performance Crystal Plate
025-2120 3-Reflection Diamond/ZnSe Performance Crystal Plate, Trough
025-2038 3-Reflection ZnSe Performance Crystal Plate
025-2218 9-Reflection Diamond/ZnSe Performance Crystal Plate, Trough
025-2208 Specular Reflection Performance Plate

RECONDITIONED CRYSTAL PLATES

025-3010 Reconditioned Single Reflection ZnSe Crystal Plate
025-3040 Reconditioned Single Reflection Ge Crystal Plate
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.

HEATED CRYSTAL PLATES

025-4018 Heated ZnSe Performance Crystal Plate
025-4058 Heated Ge Performance Crystal Plate
025-4108 Heated Diamond/ZnSe Performance Crystal Plate

NOTE: ZnSe and Ge heated plates may be operated to 130 °C. Diamond has limited range to 60 °C.
Heated plates require PIKE Temperature Controller.

LIQUID JACKETED CRYSTAL PLATES

025-2014 Liquid Jacketed ZnSe Crystal Plate
025-2054 Liquid Jacketed Ge Crystal Plate
025-2094 Liquid Jacketed Si Crystal Plate
025-2104 Liquid Jacketed Diamond/ZnSe Crystal Plate

PN 350-025004-10
P a g e | 20
TEMPERATURE CONTROLLERS FOR HEATED CRYSTAL PLATES
076-1420 Digital Temperature Control Module, PC Control
076-1220 Digital Temperature Control Module

PRESSURE CLAMPS
025-3025 MIRacle Performance High-Pressure Clamp
025-3027 MIRacle Performance Confined Space Clamp
025-3029 Performance Micrometric, Low-Pressure Clamp
076-6025 Digital Force Adapter for High-Pressure Clamp
076-6028 Digital Force Adapter for High-Pressure Confined Space 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 Volatiles Cover for Performance Plates
026-5010 Liquids Retainer for Performance Plates

SEALED HIGH-PRESSURE CLAMP

025-6020 Sealed High-Pressure Clamp

025-6108 Diamond/ZnSe Plate for Sealed Clamp
025-6018 ZnSe Plate for Sealed Clamp
025-6058 Ge Plate for Sealed Clamp

Figure 10. The Sealed High-Pressure Clamp for the MIRacle Single Reflection ATR accessory allows the clamp/crystal
plate assembly to be removed from the MIRacle base mounted in the spectrometer to a protective environment for
sample loading and handling. Typical applications include studies of toxic or chemically aggressive solids and
powders. Dedicated Sealed Sample Chamber Clamp crystal plates, available in diamond, ZnSe or Ge, must be
ordered separately.

PN 350-025004-10
P a g e | 21
6125 Cottonwood Drive · Madison, WI 53719-5120 · (608) 274-2721 (TEL) · (608) 274-0103 (FAX)
[email protected] · www.piketech.com