This document provides an overview of Attenuated Total Reflectance (ATR) Fourier Transform Infrared (FTIR) spectroscopy. It discusses how ATR addresses challenges with traditional transmission FTIR sampling methods, such as difficulties preparing homogeneous solid and liquid samples of a consistent thickness. The document describes how ATR uses an internal reflection element to produce an evanescent wave that interacts with the sample. It explains that ATR provides faster, more reproducible sampling compared to transmission by avoiding issues with sample thickness. Finally, it summarizes that ATR spectroscopy has revolutionized solid and liquid FTIR sampling through improved speed, reproducibility, and consistency between users.
PerkinElmer: Nano-Composites Characterization by Differential Scanning Calori...PerkinElmer, Inc.
Nanocomposites are usually comprised of organic polymer composites with inorganic nanomaterial fillers or building blocks. This combination increases the physical properties of the final nanocomposite product. Rigidity, thermal stability, dielectric strength, ductility, and elastic limits are expanded due to the special properties that nanoscale objects have compared to the traditional bulk fillers and bulk fibers. The uniqueness of nanoscale materials is the large surface area to weight ratio. This single nano characteristic leads to a dramatic increase in the interfacial area compared to traditional filler.
Thermal analytical techniques that are used to characterize nanocomposite formulations during development, processing, and final acceptance testing are: Differential Scanning Calorimetry (DSC, HyperDSCTM), Thermogravimetry (TGA), Dynamic Mechanical Analysis (DMA), and the hyphenated technique Thermogravimetry-Gas Chromatography-Mass Spectrometry (TGA-GC-MS), are used to measure nanocomposites. These measurements help ensure that the nanocomposite manufacturing process is stable, reproducible, and reliable. This poster concentrates on the formulation and end product validation through Differential Scanning Calorimetry (HyperDSCTM) characterization.
Study the effect of thin film thickness on the optical features of (IR5 laser...TELKOMNIKA JOURNAL
The linear optical features such as (transmittance T, absorbance A, the effective length 퐿푒푓푓, absorption coefficient 훼 and refractive index 푛 ) for the thin films samples of (3x10-3 mol/l of (IR5) laser dye, 0.02 gm of (CdS) nanoparticles and 0.04 gm of pp polymer) had been studied at different values of film thickness in one time and at different number of Yb:GdVO4 laser pulses. The non-linear optical features in terms of transmittance difference Δ푇푝−푣, non-linear refractive index 푛2, non–linear phase shift Δ훷표 non-linear absorption coefficient 훽 and minimum normalized transmittance 푇(푍) have been computed in relation to obtained normalized transmittance data from setup of Z-scan with open and closed apertures, calculated for (3x10-3 mol/l of (IR5) laser dye, 0.02 gm of (CdSe) nanoparticles and 0.04 gm of (pp) polymer) thin films at different values of film thickness at in one time and at different Yb:GdVO4 laser pulses. Thick films causes in deleting the non-linear effects generated by different layers. The (CdSe) nanoparticles leads to an absorption shifting of the wavelengths to lengthier wavelengths of red shift. So, this can be used in selecting the nanoparticles and medium with applicable exciting wavelengths. The film thickness and the laser pulses have the main effects in consolidating the Non-linear optical features.
High-Sensitivity HydrophoneBased on Fiber Grating Laser And Acorrugated Diaph...IJRESJOURNAL
ABSTRACT: In this work, we present afiber optic hydrophones based on dual-frequency fiber grating lasers and a corrugated diaphragm. The laser is employed as sensing element and an elastic corrugated diaphragm is used to translate acoustic pressure P intolateral point loadNon the laser cavity. Experimental result shows the fiber laser hydrophone has a working bandwidth over 1 kHz with sub100 μPa/Hz1/2minimum detectable pressure at 1 kHz
Improving Advanced Lithography Process Defectivity with a Highly Retentive 5n...Entegris
Semiconductors require ever increasing purity in fluids that come in contact with the devices to reduce the defectivity during the manufacturing process. Defect control is extremely critical and continues to be one of biggest challenges in lithography processes for integrated device manufacturers (IDMs) as the critical dimension (CD) size shrinks [1]. Any defect could result in an unusable device, resulting in a financial loss for the IDMs. Particularly in 193nm lithography processes, there have been widespread occurrences of various defects in the coated films, and many factors could play a role in defect formation. For example, photoresist and BARC coating defects could be affected by the dispense process, cleanliness of the materials, and filtration process.
Particle removal filters are used in almost every process step where a liquid comes in contact with a wafer. Implementation of polymer membrane-based microfiltration in the photochemical manufacturing process effectively improves the cleanliness of the materials. Furthermore, in today’s state-of-the art semiconductor fabs, an extra filtration step at the point of dispense on the coater module is adopted to further minimize coating defects by providing particle/bubble-free photochemical dispense on the wafer.
With the continuous demands for defect reduction and high productivity, Entegris has developed a new, highly retentive 5nm rated asymmetric ultrahigh molecular weight polyethylene (UPE) filter to address these demands particularly in advanced lithography processes. The purpose of this application note is to provide data to show the performance of 5nm asymmetric UPE filters and its effectiveness of reducing the wafer defects for various lithographic processes.
PerkinElmer: Nano-Composites Characterization by Differential Scanning Calori...PerkinElmer, Inc.
Nanocomposites are usually comprised of organic polymer composites with inorganic nanomaterial fillers or building blocks. This combination increases the physical properties of the final nanocomposite product. Rigidity, thermal stability, dielectric strength, ductility, and elastic limits are expanded due to the special properties that nanoscale objects have compared to the traditional bulk fillers and bulk fibers. The uniqueness of nanoscale materials is the large surface area to weight ratio. This single nano characteristic leads to a dramatic increase in the interfacial area compared to traditional filler.
Thermal analytical techniques that are used to characterize nanocomposite formulations during development, processing, and final acceptance testing are: Differential Scanning Calorimetry (DSC, HyperDSCTM), Thermogravimetry (TGA), Dynamic Mechanical Analysis (DMA), and the hyphenated technique Thermogravimetry-Gas Chromatography-Mass Spectrometry (TGA-GC-MS), are used to measure nanocomposites. These measurements help ensure that the nanocomposite manufacturing process is stable, reproducible, and reliable. This poster concentrates on the formulation and end product validation through Differential Scanning Calorimetry (HyperDSCTM) characterization.
Study the effect of thin film thickness on the optical features of (IR5 laser...TELKOMNIKA JOURNAL
The linear optical features such as (transmittance T, absorbance A, the effective length 퐿푒푓푓, absorption coefficient 훼 and refractive index 푛 ) for the thin films samples of (3x10-3 mol/l of (IR5) laser dye, 0.02 gm of (CdS) nanoparticles and 0.04 gm of pp polymer) had been studied at different values of film thickness in one time and at different number of Yb:GdVO4 laser pulses. The non-linear optical features in terms of transmittance difference Δ푇푝−푣, non-linear refractive index 푛2, non–linear phase shift Δ훷표 non-linear absorption coefficient 훽 and minimum normalized transmittance 푇(푍) have been computed in relation to obtained normalized transmittance data from setup of Z-scan with open and closed apertures, calculated for (3x10-3 mol/l of (IR5) laser dye, 0.02 gm of (CdSe) nanoparticles and 0.04 gm of (pp) polymer) thin films at different values of film thickness at in one time and at different Yb:GdVO4 laser pulses. Thick films causes in deleting the non-linear effects generated by different layers. The (CdSe) nanoparticles leads to an absorption shifting of the wavelengths to lengthier wavelengths of red shift. So, this can be used in selecting the nanoparticles and medium with applicable exciting wavelengths. The film thickness and the laser pulses have the main effects in consolidating the Non-linear optical features.
High-Sensitivity HydrophoneBased on Fiber Grating Laser And Acorrugated Diaph...IJRESJOURNAL
ABSTRACT: In this work, we present afiber optic hydrophones based on dual-frequency fiber grating lasers and a corrugated diaphragm. The laser is employed as sensing element and an elastic corrugated diaphragm is used to translate acoustic pressure P intolateral point loadNon the laser cavity. Experimental result shows the fiber laser hydrophone has a working bandwidth over 1 kHz with sub100 μPa/Hz1/2minimum detectable pressure at 1 kHz
Improving Advanced Lithography Process Defectivity with a Highly Retentive 5n...Entegris
Semiconductors require ever increasing purity in fluids that come in contact with the devices to reduce the defectivity during the manufacturing process. Defect control is extremely critical and continues to be one of biggest challenges in lithography processes for integrated device manufacturers (IDMs) as the critical dimension (CD) size shrinks [1]. Any defect could result in an unusable device, resulting in a financial loss for the IDMs. Particularly in 193nm lithography processes, there have been widespread occurrences of various defects in the coated films, and many factors could play a role in defect formation. For example, photoresist and BARC coating defects could be affected by the dispense process, cleanliness of the materials, and filtration process.
Particle removal filters are used in almost every process step where a liquid comes in contact with a wafer. Implementation of polymer membrane-based microfiltration in the photochemical manufacturing process effectively improves the cleanliness of the materials. Furthermore, in today’s state-of-the art semiconductor fabs, an extra filtration step at the point of dispense on the coater module is adopted to further minimize coating defects by providing particle/bubble-free photochemical dispense on the wafer.
With the continuous demands for defect reduction and high productivity, Entegris has developed a new, highly retentive 5nm rated asymmetric ultrahigh molecular weight polyethylene (UPE) filter to address these demands particularly in advanced lithography processes. The purpose of this application note is to provide data to show the performance of 5nm asymmetric UPE filters and its effectiveness of reducing the wafer defects for various lithographic processes.
Study of Linear and Non-Linear Optical Parameters of Zinc Selenide Thin FilmIJERA Editor
Thin film of Zinc Selenide (ZnSe) was deposited onto transparent glass substrate by thermal evaporation technique. ZnSe thin film was characterized by UV-Visible spectrophotometer within the wavelength range of 310 nm-1080 nm. The Linear optical parameters (linear optical absorption, extinction coefficient, refractive index and complex dielectric constant) of ZnSe thin film were analyzed from absorption spectra. The optical band gap and Urbach energy were obtained by Tauc’s equation. The volume and surface energy loss function of ZnSe thin film were obtained by complex dielectric constant. The Dispersion parameters (dispersion energy, oscillation energy, moment of optical dispersion spectra, static dielectric constant and static refractive index) were calculated using theoretical Wemple-DiDomenico model. The oscillation strength, oscillator wavelength, high frequency dielectric constant and high frequency refractive index were calculated by single Sellmeier oscillator model. Also, Lattice dielectric constant, N/m* and plasma resonance frequency were obtained. The electronic polarizibility of ZnSe thin film was estimated by Clausius-Mossotti local field polarizibility. The non-linear optical parameters (non-linear susceptibility and non-linear refractive index) were estimated.
International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.
Additive manufacturing (AM) offers a few major benefits to biomedical applications. To improve the knowledge on AM possibilities, Sirris is organizing two different masterclasses. The first will address the technology, materials used and applications, with experts in the matter explaining all relevant aspects.
FT-IR & Phase Behavior Studies of Polymer-Surfactant InteractionsDavid Scheuing
Presented to American Oil Chemist's Society meeting - 2005. Reviews interactions between cationic water-soluble polymers and anionic micelles. Discusses application of FT-IR to monitor morphology of adsorbed layers formed by these systems on Ge surfaces.
Study of Linear and Non-Linear Optical Parameters of Zinc Selenide Thin FilmIJERA Editor
Thin film of Zinc Selenide (ZnSe) was deposited onto transparent glass substrate by thermal evaporation technique. ZnSe thin film was characterized by UV-Visible spectrophotometer within the wavelength range of 310 nm-1080 nm. The Linear optical parameters (linear optical absorption, extinction coefficient, refractive index and complex dielectric constant) of ZnSe thin film were analyzed from absorption spectra. The optical band gap and Urbach energy were obtained by Tauc’s equation. The volume and surface energy loss function of ZnSe thin film were obtained by complex dielectric constant. The Dispersion parameters (dispersion energy, oscillation energy, moment of optical dispersion spectra, static dielectric constant and static refractive index) were calculated using theoretical Wemple-DiDomenico model. The oscillation strength, oscillator wavelength, high frequency dielectric constant and high frequency refractive index were calculated by single Sellmeier oscillator model. Also, Lattice dielectric constant, N/m* and plasma resonance frequency were obtained. The electronic polarizibility of ZnSe thin film was estimated by Clausius-Mossotti local field polarizibility. The non-linear optical parameters (non-linear susceptibility and non-linear refractive index) were estimated.
International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.
Additive manufacturing (AM) offers a few major benefits to biomedical applications. To improve the knowledge on AM possibilities, Sirris is organizing two different masterclasses. The first will address the technology, materials used and applications, with experts in the matter explaining all relevant aspects.
FT-IR & Phase Behavior Studies of Polymer-Surfactant InteractionsDavid Scheuing
Presented to American Oil Chemist's Society meeting - 2005. Reviews interactions between cationic water-soluble polymers and anionic micelles. Discusses application of FT-IR to monitor morphology of adsorbed layers formed by these systems on Ge surfaces.
Application Note: Simple Method of Measuring the Band Gap Energy Value of TiO...PerkinElmer, Inc.
The measurement of the band gap of materials is important in the semiconductor, nanomaterial and solar industries. This note demonstrates how the band gap of a material can be determined from its UV absorption spectrum.
Natural ageing of stabilized and unustabilized ldpe films used as greenhouses...eSAT Journals
Abstract
This article focuses on the study of both stabilized and unstabilized low-density polyethylene films aged under natural weathering in the middle of Morocco (Sidi Kacem city). The study was undertaken on three samples for each LDPE films: a new sample taken as reference; another exposed to outdoor weathering for one year; and a sample exposed for two years.
The outdoor exposure effects were followed by analysis of the total reflection Fourier transform infrared spectroscopy (ATR-FTIR). This technique provides information on the main chemical functions and evaluates the internal causes of natural ageing of our samples. The infrared spectra show the formation of hydroperoxides -O-OH, carbonyls >C=O, aliphatic esters R-(CO)-O-R, ether R-O-R, vinyl C=C, vinylidene >C=CH2 and trans-vinylene RHC=CRH in the amorphous regions. These compounds lead to initiate the mechanism of photo-oxidation of the unstabilized LDPE samples. Therefore, the increase in the formation of oxidation products into the aged samples (LDPEUS) indicates an accelerated degradation of these latter on climatic factors (UV, O2, humidity, rain ...). The UV stabilizer (free radicals scavengers) added to the formulation of LDPE films can delay the attack of the amorphous phase and prevent the formation of compounds that can cause and accelerate photo-oxidation. The results obtained by the infrared have been confirmed by observing the morphology of the samples with scanning electron microscopy technology (SEM).
Keywords: LDPE, Photo-oxidation, Natural ageing, UV stabilizer, ATR-FTIR, SEM
Computationally Efficient Methods for Sonar Image Denoising using Fractional ...CSCJournals
Sonar images produced due to the coherent nature of scattering phenomenon inherit a multiplicative component called speckle and contain almost homogeneous as well as textured regions with relatively rare edges. Speckle removal is a pre-processing step required in applications like the detection and classification of objects in the sonar image. In this paper computationally efficient Fractional Integral Mask algorithms to remove the speckle noise from sonar images is proposed. Riemann- Liouville definition of fractional calculus is used to create Fractional integral masks in eight directions. The use of a mask incorporated with the significant coefficients from the eight directional masks and a single convolution operation required in such case helps in obtaining the computational efficiency. The sonar image heterogeneous patch classification is based on a new proposed naive homogeneity index which depends on the texture strength of the patches and despeckling filters can be adjusted to these patches. The application of the mask convolution only to the selected patches again reduce the computational complexity. The non-homomorphic approach used in the proposed method avoids the undesired bias occurring in the traditional homomorphic approach. Experiments show that the mask size required directly depends on the fractional order. Mask size can be reduced for lower fractional orders thus ensuring the computation complexity reduction for lower orders. Experimental results substantiate the effectiveness of the despeckling method. The different non reference image performance evaluation criterion are used to evaluate the proposed method.
Phillips - A brief discussion of conventional sputtering and energetic Conden...thinfilmsworkshop
http://www.surfacetreatments.it/thinfilms
A Brief Discussion of Conventional Sputtering and Energetic Condensation for Superconducting cavity applications (Larry Phillips - 25')
Speaker: Larry Phillips - JLab | Duration: 25 min.
Abstract
The history of niobium films produced by conventional magnetron sputtering and energetic condensation will be discussed in terms of their impact on SRF cavity performance.
A brief overview of current R&D in the energetic condensation of niobium films for this application will also be discussed.
1. F T- I R S P E C T R O S C O P Y
T E C H N I C A L
FT-IR Spectroscopy
Attenuated Total Reflectance (ATR)
N O T E
Sample in contact
with evanescent wave
To Detector
Infrared ATR
Beam Crystal
Introduction many cases some form of sample Key Features
Mid-Infrared (IR) spectroscopy preparation is required in order
Faster sampling
is an extremely reliable and to obtain a good quality spectrum.
Traditionally IR spectrometers Improving sample-to-sample
well recognized fingerprinting reproducibility
method. Many substances can have been used to analyze solids,
be characterized, identified and liquids and gases by means of Minimizing user-to-user spectral
transmitting the infrared radia- variation
also quantified.
tion directly through the sample. Higher quality spectral databases
One of the strengths of IR spec- Where the sample is in a liquid for more precise material verification
troscopy is its ability as an ana- and identification
or solid form the intensity of the
lytical technique to obtain spectra spectral features is determined by
from a very wide range of solids, the thickness of the sample and
liquids and gases. However, in typically this sample thickness
w w w. p e r k i n e l m e r. c o m
2. cannot be more than a few tens of thoroughly with about 350 mg of thickness or pathlength. A constant
microns. Figure 1 displays a typical ground KBr. The mixture is now pathlength is highly desirable when
IR transmission spectrum. transferred to a die that has a barrel performing quantitative analyses.
diameter of 13 mm (Figure 2). This is
The technique of Attenuated Total Overall, sample preparation is easier
then placed in a suitable press and
Reflectance (ATR) has in recent for liquid transmission studies
pressed (evacuation is optional) at
years revolutionized solid and when compared to solid transmis-
around 12,000 psi for one to two
liquid sample analyses because sion sampling but both suffer from
minutes. Re-crystallization of the
it combats the most challenging inevitable reproducibility issues
KBr results in a clear glassy disk
aspects of infrared analyses, given the complexity of the sample
about 1 mm thick. This disk is now
namely sample preparation and preparation methods. In addition,
ready to be analyzed by transmission.
spectral reproducibility. preparation can be very messy and
time consuming and is further com-
Issues surrounding plicated by difficulties in getting
traditional transmission sample to matrix ratios correct and
homogenous throughout the sample.
sample preparation
The materials involved are fragile and
The two most common forms of hydroscopic and the quality of meas-
sample preparation for solids both urements can be adversely affected if
Evacuable KBr Die
involve grinding the material to a handled or stored incorrectly. The
fine powder and dispersing it in a Figure 2. Potassium bromide 13 mm die.
technique of Attenuated Total
matrix. The ground material can be Reflectance addresses these issues.
dispersed in a liquid to form a mull.
The most commonly used liquid is
Principles of ATR
mineral oil (nujol). Typically no
more than 20 mg of solid is ground An attenuated total reflection
and then one or two drops of nujol accessory operates by measuring
are used to create a paste which is the changes that occur in a totally
then spread between two Mid-Infra- internally reflected infrared beam
red transparent windows e.g. NaCl, when the beam comes into contact
KBr, CaF2. The sample is now ready Figure 3. Sealed (l) and demountable (r) with a sample (indicated in Figure 4).
liquid cells. An infrared beam is directed onto
to be placed in the spectrometer for
analysis by transmission. an optically dense crystal with a
Liquids are traditionally analyzed
high refractive index at a certain
Potassium bromide (KBr) is prob- as thin films in cells (Figure 3), a cell
angle. This internal reflectance
ably the most widely used matrix consists of two IR transparent win-
creates an evanescent wave that
material. Between 1 and 3 mg of dows. A Teflon® spacer is generally
extends beyond the surface of the
ground material needs to be mixed used to produce a film of the desired
crystal into the sample held in con-
tact with the crystal. It can be easier
to think of this evanescent wave as
a bubble of infrared that sits on the
surface of the crystal. This evanes-
cent wave protrudes only a few mic-
rons (0.5 µ - 5 µ) beyond the crystal
surface and into the sample. Conse-
quently, there must be good contact
between the sample and the crystal
surface. In regions of the infrared
spectrum where the sample absorbs
energy, the evanescent wave will be
attenuated or altered. The attenuated
Figure 1. A Mid-Infrared spectrum of Hexene. energy from each evanescent wave
2
3. is passed back to the IR beam, which deformable materials, and also with Germanium has a much better work-
then exits the opposite end of the fine powders but many solids give ing pH range and can be used to
crystal and is passed to the detector very weak spectra because the con- analyze weak acids and alkalis.
in the IR spectrometer. The system tact is confined to small areas. The Germanium has by far the highest
then generates an infrared spectrum. effects of poor contact are greatest refractive index of all the ATR
at shorter wavelengths where the materials available which means
For the technique to be successful,
depth of penetration is lowest. that the effective depth of pene-
the following two requirements must
tration is approximately 1 micron.
be met: The issue of solid sample/crystal
For most samples this will result
contact has been overcome to a great
• The sample must be in direct in a weak spectrum being produced,
extent by the introduction of ATR
contact with the ATR crystal, however, this is an advantage when
accessories with very small crystals,
because the evanescent wave or analyzing highly absorbing materi-
typically about 2 mm across. The
bubble only extends beyond the als; carbon black filled rubbers are
most frequently used small crystal
crystal 0.5 µ - 5 µ. typically analyzed using Germanium
ATR material is diamond because it
• The refractive index of the crys- ATR accessories.
has the best durability and chemical
tal must be significantly greater inertness. These small area ATR crys- Diamond is by far the best ATR crys-
than that of the sample or else tal top-plates generally provide only a tal material because of its robustness
internal reflectance will not oc- single reflection but this is sufficient, and durability. The original purchase
cur – the light will be transmitted given the very low noise levels of cost is obviously higher than that of
rather than internally reflected in PerkinElmer’s modern FT-IR spec- other crystal materials available, but
the crystal. Typically, ATR crystals trometers. Much higher pressure with over the instrument’s lifetime re-
have refractive index values be- limited force can now be generated placement costs should be minimal.
tween 2.38 and 4.01 at 2000 cm-1. onto these small areas. A much The same cannot be said of Zinc
It is safe to assume that the majority smaller area of contact is now re- Selenide or Germanium, both of
of solids and liquids have much quired in comparison to the HATR which can scratch and break with
lower refractive indices. units. As a result, spectra can be improper use.
obtained from a wide variety of
ATR accessories As with all FT-IR measurements, an
solid materials including minerals.
infrared background is collected, in
The traditional ATR design in which
this case, from the clean ATR crystal.
a thin sample was clamped against Crystal materials The crystals are usually cleaned
the vertical face of the crystal has and cleaning by using a solvent soaked piece of
been now been replaced by a hori-
There are a number of crystal mate- tissue. Typically water, methanol or
zontal design. In horizontal ATR
rials available for ATR. Zinc Selenide isopropanol are used to clean ATR
(HATR) units, the crystal is a paral-
(ZnSe) and Germanium are by far crystals. The ATR crystal must be
lel-sided plate, typically about 5 cm
the most common used for HATR checked for contamination and carry
by 1 cm, with the upper surface ex-
sampling. Zinc Selenide is a rela- over before sample presentation,
posed (Figure 4). The number of
tively low cost ATR crystal material this is true for all liquids and solids.
reflections at each surface of the
and is ideal for analyzing liquids
crystal is usually between five and
and non-abrasive pastes
ten, depending on the length and
and gels but it is not
thickness of the crystal and the angle Sample in contact
particularly robust with
of incidence. with evanescent wave
a working pH range of
When measuring solids by ATR, it 5-9. ZnSe scratches quite
is essential to ensure good optical easily and so care must
To Detector
contact between the sample and the be taken when cleaning
crystal. The accessories have devices the crystal. It is recom- Infrared ATR
Beam Crystal
that clamp the sample to the crystal mended that lint free
surface and apply pressure. This tissue is used. Figure 4. A multiple reflection ATR system.
works well with elastomers and other
w w w. p e r k i n e l m e r. c o m 3
4. Analyzing liquids After the crystal area has been The strongest bands here extend
After the crystal has been cleaned cleaned and the background col- beyond 20% T with relatively little
and an infrared background has lected, the solid material is placed force applied; the force gauge is
been collected, the liquid is simply onto the small crystal area (Figure 6). registering 80 N. A lot more pres-
poured onto the crystal (Figure 5). Experience has shown that ideal sure would need to be applied when
The whole crystal must be covered if results from powder samples have analyzing high density polymers and
performing a quantitative or qualita- been achieved by placing just coatings on metal surfaces. Once the
tive analysis. The crystal is recessed enough sample to cover the crystal user is satisfied with the spectrum
into the metal plate to retain the area. The sample height should not shown in this ‘Preview Mode’, the
sample. Pastes and other semi-solid be more than a few millimeters. data is then collected in the normal
samples are readily measured by manner. The force should not be
Once the solid has been placed on the
spreading them on the crystal. Hori- adjusted when co-adding the final
crystal area, the pressure arm should
zontal ATR units are often used for spectrum. Unlike transmission
be positioned over the crystal/sample
quantitative work in preference to measurements, ATR sampling does
area. When using the Spectrum 100
transmission cells because they are not produce totally absorbing
Series’ Universal ATR accessory,
easier to clean and maintain. spectral bands because the effective
the pressure arm locks into a precise
path-length is controlled by the
position above the diamond crystal
crystal properties thereby minimiz-
(Figure 7). Force is applied to the
ing sample re-preparation time.
sample, pushing it onto the dia-
mond surface. After the spectrum has been col-
lected, which should typically take
no more than 32 seconds, the user
must return to the ‘Preview Mode’.
This mode is now used to check
that the crystal area is clean before
placing the next sample on the cry-
Figure 5. Using a pipette to add a liquid stal. A 100% T line with no spectral
sample to a ZnSe HATR trough plate.
features (Figure 9) should be seen if
the crystal is clean, if spectral fea-
Analyzing solids tures are seen, the crystal should
Solids are generally best analyzed be cleaned again using a solvent
Figure 7. Applying pressure to a solid sample
on the single reflection ATR acces- on the Universal diamond ATR top-plate. soaked tissue. The next sample can
sories; diamond being the preferred be placed on the crystal area once
choice for most applications because the 100% T line has been displayed
PerkinElmer’s revolutionary and the sampling steps are repeated.
of its robustness and durability.
Spectrum™ FT-IR software utilizes
a ‘Preview Mode’ which allows the
Conclusion
quality of the spectrum to be
monitored in real-time while fine ATR is an IR sampling technique that
tuning the exerted force. It is good provides excellent quality data in
practice to apply pressure until the conjunction with the best possible
strongest spectral bands have an reproducibility of any IR sampling
intensity which extends beyond technique. It has revolutionized IR
70% T, namely from a baseline at solid and liquid sampling through:
100% T down to 70% T. Good
• Faster sampling
sample/crystal interface contact has
been achieved once this rule has • Improving sample-to-sample
been satisfied. This is very easy to reproducibility
achieve with soft samples and fine • Minimizing user to user spectral
Figure 6. Placing a powder sample onto the
Universal diamond ATR top-plate. powders, this is shown in Figure 8. variation
4