FTIR Series Accessories

Transcription

1 Fourier Transform Infrared Spectrophotometers FTIR Series Accessories C03-E005J

2 FTIR Accessories Overview Selection of Optional Accessories Shimadzu's FTIR instruments have simple optics to give an attachment having complicated optics its full play. In FTIR, which ensures exceptionally high wavenumber accuracy, even a single-beam instrument provides satisfactory spectra, which means that the reference sample and the unknown sample can be measured individually; the net result is that, in FTIR, only one piece of attachment or accessory is useful enough. In dispersive IR, by contrast, attachments and accessories must be used as a pair. This is a great advantage from an economic viewpoint. Most of the attachments and accessories are designed so that samples may be measured without preparation. Shown to the right is a flow chart for selecting attachments and accessories. The results of FTIR analysis depend greatly on the type of attachment and accessory used in analysis. IRPrestige-2 IRAffinity-

3 Rubbers Pyrolysis Powders Paper, cloth, yarns Films, plastics Thinner than 00 µm Dissolve in solvent Solids Grind Coating films on metals Thicker than µm Mix with KBr powder Thinner than µm Coating films on resins Type of Sample Semiconductors Surface measurement Liquids Oil content measurement Nonvolatile organic solvents Volatile organic solvents Aqueous solutions Extract solutions Rapid measurement Above 0% in concentration Below 0% in concentration Difference spectrometry Evaporate solvent Gases Concentration % order ppm order Micro/trace samples Liquids Solids µl order Below several handreds of µm Above several hundreds of µm

4 Total reflectance method Liquid film method Nujol method KBr pellet method Total reflectance method Diffuse reflectance method Total reflectance method Total reflectance method Transmission method Film method SiC sampler ATR accessories (Black rubbers requires Ge prism) Demountable cell Demountable cell KBr die + hydraulic press + vacuum pump, or mini hand press Single-reflection ATR DRS-8000A... Mix with KBr powder ATR accessories ATR accessories Film holder... Use grid polarizer for study of molecular orientation Demountable cell... Evaporate the solvent to obtain the film DRS-8000A + SiC sampler Total reflectance method Specular reflectance method Reflection absorption spectrometry KBr pellet method Diffuse reflectance method Total reflectance method Specular reflectance method Film holder Total reflectance method Single-reflection ATR... Measurement to a depth of /5 of the wavelength with a KRS-5 prism and to /0 with a Ge prism SRM-8000A, VeeMAXllA RAS-8000A,... Use of a grid polarizer enhances sensitivity about two times VeeMAXllA KBr die + hydraulic press + vacuum pump, or mini hand press DRS-8000A ATR accessories... Measurement to a depth of /5 of the wavelength with a KRS-5 prism and to /0 with a Ge prism SRM-8000A,... Convert a reflection spectrum into the absorption VeeMAXllA spectrum by the Kramers-Kronig method Single-reflection ATR (Ge prism) Quartz cell... Detection limit is ppm level with 0 µm optical path Liquid film method Solution method Total reflectance method Liquid film method Demountable cell Fixed thickness cell, sealed liquid cell ATR-8200HA, Single-reflection ATR Demountable cell with KRS-5 window Solution method Total reflectance method Fixed thickness cell ATR-8200HA, Single-reflectionATR... The sample solution is supplied dropwise on prism and measured after evaporating the solvent Diffuse reflectance method DRS-8000A... The sample solution is supplied dropwise on KBr powder and measured after evaporating the solvent 5 cm/0 cm gas cell Gas cell with long pathlength Total reflectance method Infrared microscopy Total reflectance method Single-reflection ATR AIM Applicable to transmission, reflection, and ATR methods Single-reflection ATR

5 Shimadzu Accessory Line-up. Options from Shimadzu Remarks Page Single Reflection Type Attenuated Total Reflection MIRacle XX with Diamond, ZnSe, Ge prism 8 Attachment Integral with Sample Compartment GladiATR XX with Diamond prism 9 Horizontal Type Attenuated Total Reflection Attachment Integral with Sample Compartment HATR with ZnSe prism 0 Attenuated Total Reflection Attachment ATR-8000A ATR with KRS-5 prism Attenuated Total Reflectance Measurement Horizontal Type Attenuated Total Reflection Attachment Single-Reflection Horizontal Attenuated Total Reflection Attachment ATR-8200HA ATR-8200H MIRacleA MIRacle MIRacleA MIRacle DuraSampllR II (Diamond ATR) See page 4 with ZnSe prism with ZnSe prism with Ge prism DuraScope with Diamond prism 5 Specular Reflectance Attachment SRM-8000A SRM Incident Angle: 0 7 Reflectance Measurement Reflection Absorption Spectrometry Attachment RAS-8000A RAS Incident Angle: 70 to 75 8 Grid Polarizer GPR Variable Incident Angle Reflectance Attachment VeeMAX II A VeeMAX II Incident Angle: 30 to Diffuse Reflectance Measurement Diffuse Reflectance Attachment SiC Sampler DRS-8000A DRS Automatic Diffuse Reflectance Attachment DRS-800ASC Automatic Infrared Microscope AIM-8800 Type Type XX XX 26 Micro Sample Measurement ATR Objective Mirror Sampling Kit Diamond Cell C Diamond Cell B ATR-8800M with Ge prism Micro Vise Holder Reflection-Type Beam Condenser RBC Automatic Sampler Diffuse Reflectance Attachment DRS-800ASC Accessories for Automated Measurement Auto Sampler for Transmission Measurement ASC-8000T Sample Switcher Purge Control Kit Purge Control Kit Dry Air Supply Unit PCK-894 PCK-2 50Hz 60Hz

6 Remarks Page External Detector / Optional Detector External light Beam Switching Kit MCT Kit Cassette (Sample Holder) Magnetic-Type Film Sample Holder Universal Clip Holder Transmission Measurement EZ-Clip 3 EZ-Clip cm Gas Cell XX 0 cm Gas Cell XX 36 Gas Cell Long Pathlength Gas Cell Mini Hand Press Evacuable Die for KBr Pellets MHP Micro Die for 2 mm dia. KBr Pellets Pellet Measurement Micro Die for 5 mm dia. KBr Pellets Hydraulic Press SSP-0A Vacuum Pump SA8-3M Magnetic-Type Pellet Holder Agate Mortar and Pestle KBr Crystal (00 g) Demountable Cell Sealed Liquid Cell XX XX 40 Cells for Liquid Samples Fixed Thickness Cell XX 4 Sample Cell for Oil Content Determination Crystal Polishing Kit See page Others Far Infrared Kit NIR Set Upload Type Diffuse Reflectance Attachment UpIR A NIR Measurement NIR Integrating Sphere IntegratIR A Heating Transmission Cell Infrared Microscope AIM XX 46 IRsolution Agent Mapping Program Optional Software Macro Platform 3D Display Program PLS Quantitation Software Curvefitting (Peak split) Software

7 Attenuated Total Reflectance Measurement Attenuated Total Reflection Method The Attenuated Total Reflection (ATR) method, also called Multiple Internal Reflectance (MIR) method, is a versatile and powerful technique for infrared absorption spectrophotometry. This method is popular not only in FTIR but also in conventional dispersive IR, because it is not necessary to chemically treat, or machine, the samples. Measurement is made without destroying the samples. FTIR instruments, which ensure far higher sensitivity than dispersive lr instruments, dramatically widen the scope of application scope of the attenuated total reflection method; hence, a wide variety of attachments have been developed for this application. Shimadzu also provides a variety of ATR attachments. Principle The sample is held in contact with a prism made of highly refractive material, which transmits infrared rays; infrared rays are made incident on this sample at an angle larger than the critical angle (angle that induces total reflection). The light that is totally reflected by the interface between the sample and the prism is measured to obtain an infrared spectrum. Though it is called "total reflection", the light travels through the thin surface layer of the sample, as shown in the figure below, and therefore, the spectrum obtained is similar to that obtained from a very thin slice of the same sample. Prism Sample Sample Prism lnfrared rays Sample Requirements for Measurements by the ATR Method The sample must be placed in close contact with the surface of the prism. This method is applicable to soft rubber or plastic samples, solid samples with a flat surface, liquid samples, and powder samples. The prism has a higher refractive index than the sample. lt is necessary to use a prism having an appropriate refractive index. Penetration Depth of IR Light (Sample thickness) Infrared light can penetrate to a depth expressed by the next equation: Example of Penetration Depth Sample refractive index of.5 Material Refractive index (,000 cm - ) Incident angle Penetration depth 4,000 cm - 2,000 cm -,000 cm cm - λ dp= 2π (sin 2 θ-n2 2 ) 2 ZnSe/KRS-5/Diamond µm.0 µm 2.0 µm 5.0 µm 0.28 µm 0.55 µm. µm 2.8 µm where, θ : lncident angle n2: (Refractive index of sample) / (Refractive index of prism) λ : Wavelength in prism λ : λ, λ : Wavelength in air, n : Retractive in order of Prism n When θ= 45 and n2 = 0.5, therefore, 0 µm (,000 cm - ) dp corresponds to 3.8 µm and 5 µm dp (2,000 cm - ) to.6 mm. The ATR method provides spectra of surface layers without actually slicing them. Since the measurable depth (thickness) differs with the wavelength of the light, the ATR method give spectra of a little different shape though the peak wavenumbers are the same. Material Refractive index (,000 cm - ) Incident angle Penetration depth 4,000 cm - 2,000 cm -,000 cm cm µm 0.6 µm.2 µm 3.0 µm Germanium µm 0.33 µm 0.66 µm.7 µm µm 0.25 µm 0.5 µm.3 µm The software program for correcting for penetration depth, incorporated in the IRPrestige-2, IRAffinity-, FTIR-8000 Series further widens the application field of the ATR method. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 7

8 Attenuated Total Reflectance Measurement Single Reflection Type Attenuated Total Reflection Attachment Integral with Sample Compartment MIRacle 0 ( XX) This is a single reflection type horizontal attenuated total reflection attachment. Samples are measured by pressing them against an approximately.5 mm-diameter prism that is positioned horizontally. The prism materials available are diamond (with ZnSe support element), ZnSe, and Ge. This ATR attachment supports the measurement of liquid samples and solid samples such as plastics, fibers, films, and powders. Use the diamond or Ge prism to measure acidic or alkaline samples. Use the Ge prism to measure samples with a high refractive index, such as black rubber. The measurement wavenumber range is 4, cm - for diamond and ZnSe and 4, cm - for Ge. MIRacle 0 is a dedicated accessory for IRAffinity- that incorporates an automatic accessory recognition function. It cannot be used with IRPrestige-2 or the FTIR-8000 Series. Measurable Samples Film Paper Rubber Molded plastic Surface coating Liquid and gel samples Powder Notes Toxic hydrogen selenide may be generated if strongly acidic samples are measured using the ZnSe prism. Measure samples between ph 5 and 9. Use the diamond or Ge prism to measure acidic samples to approximately ph 2. Note, however, that measuring samples more acidic than this may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. The following power supply is required if a pressure sensor is attached: 90 to 264 V AC adaptor, 0.5 VA power consumption MIRacle 0 Part Names and Options and Maintenance Parts ZnSe prism plate for MIRacle 0 Ge prism plate for MIRacle 0 Diamond prism plate for MIRacle 0 Pressure sensor MIRacle 0 diamond prism MIRacle 0 ZnSe prism MIRacle 0 Ge prism MIRacle 0 diamond prism with pressure sensor MIRacle 0 ZnSe prism with pressure sensor MIRacle 0 Ge prism with pressure sensor Standard Content MIRacle 0 main unit Prism plate (Select diamond, ZnSe, or Ge.) Sample clamp (Select clamp with or without pressure sensor.) Adaptor for liquid samples IR Spectrum of ABS Resin 8

9 Single Reflection Type Attenuated Total Reflection Attachment Integral with Sample Compartment GladiATR 0 ( XX) This is a single reflection type horizontal attenuated total reflection attachment. Samples are measured by pressing them against a mm diamond prism that is positioned horizontally. An optional Ge prism is available. This ATR attachment supports the measurement of liquid samples and solid samples such as plastics, fibers, films, and powders. Use the optional Ge prism to measure samples with a high refractive index, such as black rubber. As the prism is made of diamond only, the measurement wavenumber range is 4, cm - and 4, cm - for the Ge prism. GladiATR 0 is a dedicated accessory for IRAffinity- that incorporates an automatic accessory recognition function. It cannot be used with IRPrestige-2 or the FTIR-8000 Series. Measurable Samples Film Paper Rubber Molded plastic Surface coating Liquid and gel samples Powder Notes Measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. The following power supply is required if a pressure sensor is attached: 90 to 264 V AC adaptor, 0.5 VA power consumption MIRacle 0 Part Names and GladiATR 0 diamond prism GladiATR 0 diamond prism with pressure sensor Standard Content GladiATR 0 main unit Diamond prism plate Sample clamp (Select clamp with or without pressure sensor.) Adaptor for liquid samples IR Spectrum of Lactose Powder Options and Maintenance Parts Ge prism plate for GladiATR 0 Diamond prism plate for GladiATR 0 Pressure sensor FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 9

10 Attenuated Total Reflectance Measurement Horizontal Type Attenuated Total Reflection Attachment Integral with Sample Compartment HATR 0 ( ) Samples are measured by pressing them against a prism that is positioned horizontally. The prism is made of ZnSe, and an optional Ge prism is also available. This ATR attachment supports the measurement of liquid samples and flat solid samples such as films, rubbers, and flat plastics. It is not suitable for powder samples or very small samples. Use the optional Ge prism to measure samples with a high refractive index, such as black rubber. HATR 0 is a dedicated accessory for IRAffinity- that incorporates an automatic accessory recognition function. It cannot be used with IRPrestige-2 or the FTIR-8000 Series. Features Two separate prisms for solid and liquid samples are supplied as standard. The prism is easy to install and remove, making cleaning and replacement of the prism simple. The measurement wavenumber range is 4, cm - for the ZnSe prism. It supports the measurement of liquid samples between ph 5 and 9. The measurement wavenumber range is 4, cm - for the Ge prism. It supports the measurement of samples with a high refractive index and acidic or alkaline samples. Note, however, that measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. Number of reflections: 0 Prism dimensions: 80 mm 0 mm For details about the chemical resistance of the prisms, see the table at the end of this guide. Measurable Samples Film Paper Rubber Notes Standard Content Flat plastic Surface coating on flat metal Liquid and gel samples Toxic hydrogen selenide may be generated if strongly acidic samples are measured using the ZnSe prism. Measure samples between ph 5 and 9. Use the Ge prism to measure acidic samples to approximately ph 2. Note, however, that measuring samples more acidic than this may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. HATR 0 main unit ZnSe prism for solid samples, 45 incident angle ZnSe prism for liquid samples, 45 incident angle Sample clamp IR Spectrum of Ethanol Options and Maintenance Parts ZnSe prism plate for solid samples, 45 incident angle, for HATR 0 Ge prism plate for solid samples, 45 incident angle, for HATR 0 ZnSe prism plate for liquid samples, 45 incident angle, for HATR 0 Ge prism plate for liquid samples, 45 incident angle, for HATR

11 Attenuated Total Reflection Attachment ATR-8000A ( ) ATR-8000 ( ) In the ATR-8000 series, the incident angle is changeable in three steps of 30, 45, and 60, so that measurement can be made to different depths. Combined with the program to correct for the penetrating depth of the infrared rays (which is a weak point of the ATR method because it differs depending on the wavenumber), this feature provides spectra that are highly comparable to those given by another method. QuickStart ATR-8000A includes the automatic accessory recognition function. Features It is not necessary to adjust the position of the prism when a new sample is set. The sample holder is held at one point; hence, the prism is under minimized force. 25 times reflection (with an incident angle of 45 ) ensures high sensitivity. Maximum sample size: 40 mm 5 mm, 0 mm thick The measurement wavenumber range is 4, cm - for the KRS-5 prism. The measurement wavenumber range is 4, cm - for the Ge prism. It supports the measurement of samples with a high refractive index and strongly acidic or alkaline samples. Note, however, that measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism holder. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. to detector ATR-8000 Prism Measurable Samples Film Paper Rubber Flat plastic Surface coating on flat metal Optics of ATR-8000 Standard Content Attenuated Total Reflection Attachment ATR prism (KRS-5) Sample holder Hex key wrench PhiIlips screwdriver set Prisms Material KRS-5 Ge Refractive Index (000 cm - ) With holder () Without holder () Note: Prisms without a holder are recommended as supplies, while those with a holder are recommended when prisms of different materials are purchased. ATR Spectrum of PET (KRS-5 prism) 45 (52) 2 (48) Dimensions of Prism ATR Spectrum of PET, corrected for Penetration Depth FTIR Series Accessories Fourier Transform Infrared Spectrophotometers

12 Attenuated Total Reflectance Measurement Horizontal Type Attenuated Total Reflection Attachment ATR-8200HA ( ) ATR-8200H ( ) The principle is the same as the ATR Since the prism can be placed horizontally, powder or liquid samples, which cannot be analyzed with the ordinary ATR attachment, can be readily measured. QuickStart ATR-8200HA includes the automatic accessory recognition function. Features Prisms for liquid samples and for solid samples are provided as standard. The prism is mounted and dismounted by one-touch operation, which ensures easy exchange of samples. ZnSe prisms are very chemically stable and ensure high mechanical strength. The measurement wavenumber range is 4, cm - for the ZnSe prism. It supports the measurement of samples between ph 5 and 9. The measurement wavenumber range is 4, cm - for the Ge prism. It supports the measurement of samples with a high refractive index and strongly acidic or alkaline samples. Note, however, that measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. Number of reflections: 0 Prism dimensions: 80 mm 0 mm For details about the chemical resistance of the prisms, see the table at the end of this guide. Measurable Samples Film Paper Rubber Flat plastic Surface coating on flat metal Liquid and gel samples to detector ATR-8200H Sample Prism Optics of ATR-8200H FTIR Spectrum of Oil Notes Toxic hydrogen selenide may be generated if strongly acidic samples are measured using the ZnSe prism. Measure samples between ph 5 and 9. Use the Ge prism to measure acidic samples to approximately ph 2. Note, however, that measuring samples more acidic than this may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. Standard Content Spectrum of Edible Oil The prism for liquid samples is fixed in the bottom of a boat-shaped groove, as shown in the above figure, so that liquid, powder or gel samples can be easily measured. The indentation to accept the sample is accessible from above to ensure ease when replacing samples and cleaning the prism. FTIR Spectrum of PVDC Sheet Horizontal Type Attenuated Total Reflection Attachment ZnSe prism for solid samples, 45 incident angle ZnSe prism for liquid samples, 45 incident angle Gripper ( ) Prisms ZnSe prism for solid samples, 45 incident angle ZnSe prism for liquid samples, 45 incident angle Ge prism for solid samples, 45 incident angle Ge prism for liquid samples, 45 incident angle Spectrum of PVDC Sheet The prism for solid samples permits easy measurement of film and other solid samples, with operation being the same as that for the regular ATR. A gripper is fixed to hold the sample in close contact with the prism surface, which enables highly reliable spectra. 2

13 Single Reflection Type Attenuated Total Reflection Attachment MIRacle A (ZnSe prism) ( ) (Ge prism) ( ) MIRacle (ZnSe prism) ( ) (Ge prism) ( ) This is a single reflection type horizontal attenuated total reflection attachment. Samples are measured by pressing them against an approximately 2 mm-diameter prism. As the prism is small and positioned horizontally, liquid samples can be measured by dripping a few drops of the sample onto the prism. This ATR attachment also supports the measurement of solid samples such as plastics, fibers, films, and powders. Use the Ge prism to measure samples with a high refractive index and strongly acidic or alkaline samples. MIRacle A incorporates an automatic accessory recognition function. Features The small prism supports the measurement of solid sample fragments or small volumes of liquid samples. The measurement wavenumber range is 4, cm - for the ZnSe prism. It supports the measurement of samples between ph 5 and 9. The measurement wavenumber range is 4, cm - for the Ge prism. It supports the measurement of samples with a high refractive index and strongly acidic or alk aline samples. Note, however, that measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. The ZnSe prism plate and Ge prism plate can be interchanged. Number of reflections: Prism diameter: approx. 2 mm For details about the chemical resistance of the prisms, see the table at the end of this guide. MIRacle ZnSe Prism Plate Measurable Samples Film Paper Rubber Molded plastic Surface coating Liquid and gel samples Powder Notes Toxic hydrogen selenide may be generated if strongly acidic samples are measured using the ZnSe prism. Measure samples between ph 5 and 9. Use the diamond or Ge prism to measure acidic samples to approximately ph 2. Note, however, that measuring samples more acidic than this may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. Spectrum of EVA (Ethylene Vinyl Acetate) pellet Standard Content MIRacle main unit Prism plate (Select ZnSe or Ge.) Sample clamp (high-pressure clamp) Adaptor for liquid samples Options and Maintenance Parts ZnSe prism plate Ge prism plate To use the old model MIRacle/MIRacle A ( /92/95/96), purchase one of the replacement prisms below. The prism plate shape and the sample clamp have been changed. In addition to the prism plate, the set contains parts to measure liquid samples and an instruction manual. Replace the sample clamp with a high-pressure clamp as well. To replace the prism plate again, purchase a prism plate listed in the table at the left. New-type ZnSe prism set for replacement New-type Ge prism set for replacement High-pressure clamp FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 3

14 Attenuated Total Reflectance Measurement DuraSamplIR II (Diamond ATR) This is a single-reflection ATR system that presses an approximately 2 mm diameter diamond prism tightly against the sample. The diamond prism allows the analysis of hard samples. The fit between the sample and prism is extremely good, making it convenient for liquids, solids, powders, fibers and film samples. With System I (High-Pressure Device type), the sample is pressed tightly against the prism by the clamper accessory while adjusting the clamping pressure. With System H (ViewIR type), the sample can be observed as it is being clamped. System I is also available with a pressure sensor included. ZnSe and KRS-5 support elements are available to support the diamond prism. The measurement wavenumber range is up to 4, cm - for ZnSe and 4, cm - for KRS-5. The pressure sensor cannot be added later. If it will be needed, please include it when purchasing the system. Exterior of System I (High-Pressure Device Type) Measurable Samples Film Paper Rubber Molded plastic Surface coating Liquid and gel samples Powder Notes Measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. The following power supply is required if a pressure sensor is attached: 00 V AC, 50/60 Hz, 00 VA Exterior of System I (with pressure sensor) DuraSamplIR II Part Names and DuraSamplIR II A System I (ZnSe support element) DuraSamplIR II A System I (ZnSe support element, with pressure sensor) DuraSamplIR II A System I (KRS-5 support element) DuraSamplIR II A System I (KRS-5 support element, with pressure sensor) DuraSamplIR II A System H (ZnSe support element) DuraSamplIR II A System H (KRS-5 support element) The systems above include an automatic accessory detection feature. DuraSamplIR II System I (ZnSe support element) DuraSamplIR II System I (ZnSe support element, with pressure sensor) DuraSamplIR II System I (KRS-5 support element) DuraSamplIR II System I (KRS-5 support element, with pressure sensor) DuraSamplIR II System H (ZnSe support element) DuraSamplIR II System H (KRS-5 support element) Exterior of System H (ViewIR Type) Metal Plate Diamond Prism Optional and Standard Parts DuraDisk (ZnSe support element) DuraDisk (KRS-5 support element) DuraDisk (Ge/Ge) The DuraDisk is the section where the diamond prism and the support element are joined together (the cylindrical metal section shown in the photo of the System I exterior). DuraDisks can be replaced by the customer. Infrared Light ZnSe or KRS-5 Support Element DuraSamplIR II Optics 4

15 DuraScope ( ) As with the DuraSamplIR, this is a single-reflection diamond ATR, where measurements are conducted by pressing the sample against the approximately 2 mm diameter diamond prism. A micro CCD camera is provided directly below the diamond prism to allow the observation of the contact status between the sample and prism on a video monitor. The built-in pressure sensor indicates the pressure being applied to the prism. Apart from solid samples such as plastics, film or powders, liquid samples can be also analyzed by being dropped onto the prism surface. ZnSe and KRS-5 support elements are available to hold the diamond prism. The measurement wavenumber range is 4, cm - for ZnSe and 4, cm - for KRS-5. Video Monitor Measurable Samples Film Paper Rubber Molded plastic Surface coating Liquid and gel samples Powder DuraScope Notes Measuring strongly acidic samples below ph 3 may result in corrosion of the prism or prism plate. Consult your Shimadzu representative. For details about the chemical resistance of the prisms, see the table at the end of this guide. The following power supply is required: 00 V AC, 50/60 Hz, 00 VA DuraScope Part Names and DuraScope (ZnSe support element) DuraScope (KRS-5 support element) Options and Maintenance Parts DuraDisk (ZnSe support element) DuraDisk (KRS-5 support element) DuraDisk (Ge/Ge) The DuraDisk comprises an integral diamond prism and support element. A DuraDisk with a Ge prism is also available to measure high-refractive-index samples. The DuraDisk can be replaced by the customer. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 5

16 Reflectance Measurement Specular Reflectance Method FTIR measurement by the specular reflectance method provides three types of information shown below: 2 The incident light passes through the sample layer and is reflected by the substrate: the spectrum given is similar to that obtained by the transmission method. Measurement of thin film on a metal plate is a typical example of this method. The incident light is reflected by the surface of the sample: the reflection spectrum is obtained, which can be converted into absorption spectrum through the use of the Kramers-Kronig analysis method. Transmitted light cannot be detected. 3 The above mentioned two types of information are mixed: the spectrum given is the sum of the transmission spectrum and the reflection spectrum. When the sample has a uniform thickness, the two reflection light beams interfere with each other, and the sample thickness can be obtained from the interference pattern. The measurement of a epitaxiai layer of a semi-conductor sample is a typical application of this method. Sample Metal substratum.reflection Absorption Spectroscopy Metal substratum Thin film IR rays IR rays Thin film IR rays The Reflection Absorption Spectroscopy (RAS) method permits high-sensitivity measurement of a thin film sample on a metal substrate. This method has recently come to be applied to the measurement of very thin (a few tens of angstroms thick) samples, e.g. organic LB films (Langmuir-Brodgett's Iayers), and to the determination of molecular orientation. When a polarized Iight beam is made incident on a metal substrate, as shown below, it is changed in phase when reflected by the metal surface.. 2. In vertical polarization, the vectors of the polarized light are opposite to each other. Therefore, no stationary waves are produced on the substrate, and interaction with the film material is not detected. ln parallel polarization, the vectors of the polarized Iight meet at a point to produce stationary waves, which interact with the film and are absorbed. The intensity of this absorption is dependent on the incident angle: the larger the incident angle, the higher the intensity of absorption. The optimum incident angle is different with the type of sample and the wavelength of the peak under study. In many cases, an incident angle between 70 and 80 is used. 2.Conversion of Reflection Spectra into Absorption Spectra A reflection spectrum, which provides information on the optical properties of the sample, must be converted into the absorption spectrum to be informative about the chemical structure of the sample. The Kramers-Kronig analysis method is quite convenient in that it is useful to convert a reflection spectrum into an absorption spectrum: it is not necessary to shave or slice the sample. In the example (2) shown below, when the ø is sufficiently small, each element of the complex refractive index of a material may be expressed as: -R Reflectance value n= () +R-2 Rcosθ Absorption coefficient where, R: Reflectance value θ: phase shift when the light is reflected. The θ for the wavenumber vg may be calculated from the following Kramers-Kronig equation: θ(νg)= -2 Rsinθ k= +R-2 Rcosθ 2νg π 0 The θ can be obtained from the reflectance value R, and substituting that θ in the equation (2) gives the absorption coefficient k. Performing this calculation for all the wavenumbers will give the absorption spectrum. Examples of Applications In R(ν) ν 2 νg 2 Since a reflection spectrum can be converted into the absorption spectrum through Kramers-Kronig analysis, Absorption spectrum can be obtained without shaving or slicing the sample, provided that the sample has a smooth surface. lt is not necessary to use an ATR prism or a costly attachment. 2 Kramers-Kronig analysis method is especially effective for infrared microscopy, where it is virtually impossible to slice the sample. dν (2) (3) Vertical polarization Parallel polarization Metal plate Metal plate Reflection of Light on MetaI Substratum 6

17 Specular Reflectance Attachment SRM-8000A ( ) SRM-8000 ( ) The specular reflectance measurement method is an old method to obtain reflection lr spectra. The SRM-8000 series permits not only measurement of reflection spectra, but also measurement of absorption spectra through the combined use of the Kramers-Kronig analysis method. This attachment provides absorption spectra of solids, such as high polymers, without using a prism, which is required in the ATR method. QuickStart SRM-8000A includes the automatic accessory recognition function. Features Easy sample setting. Kramers-Kronig conversion software provides IR spectra without sample preparation. The incident angle is 0 on average. Measurable Samples Coatings on flat metal surfaces with µm order. Flat plastic sheet. SRM-8000 Sample Specular reflectance attachment Standard mirror, mm Sample mask, 5 mm dia. Hex key wrench Phillips screwdriver to detector Optics of SRM-8000 Specular Reflectance Spectrum of the Inner Wall of Aluminum Can Specular Reflectance Spectrum of PMMA after Kramers-Kronig Conversion FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 7

18 Reflectance Measurement Reflection Absorption Spectrometry Attachment RAS-8000A ( ) RAS-8000 ( ) The reflection absorption spectrometry method is used only in FTIR. When a vertically polarized light and a horizontally polarized light are made incident on a metal substrate, the lights are changed in the respective phase. In the case of vertically polarized light, the phase change is about π, irrespective of the incident angle, and, hence, the vectors of the reflected light interact destructively with each other; the stationary waves produced have almost zero amplitude - no absorption of the sample is detected. In the case of horizontally polarized light, the amount of phase change varies continuously from zero (for 0 incident angle) to π (for 90 ). The amplitude of the stationary waves produced also changes with the incident angle: when a high incident angle is selected, the stationary waves will have a high amplitude and the interaction of the light beam and the sample will be high, resulting in a high detecting sensitivity. This method permits high-sensitivity measurement of thin films on metals having a high reflectance. Combined use of a grid polarizer further enhances the sensitivity. A grid polarizer ( ) is not included in the standard content of the RAS-8000 series but is available as an option. QuickStart RAS-8000A includes the automatic accessory recognition function. Incident light RAS-8000 Reflected light Stationary wave Features Easy sample setting. The incident angle is selectable between 70 and 75. Vertical polarization Parallel polarization Standard Content Principle of Reflection Absorption Spectrometry Reflection absorption spectrometry attachment Standard mirror Sample mask, 8 mm dia. Sample mask, 5 mm dia. Sample mask, 25 mm dia. Light beam mask, 3 3 mm Light beam mask, 5 5 mm Light shielding plate* Hex key wrench PhiIIips screwdriver * Attaching the light shielding plate raises the mean incident angle of the light beam from 70 to Sample 20 Light shield plate Mask (at wedge) Optics of RAS-8000 Relationship Between Spectrum of Fluorine Film on Hard Disk, Peak Area and Film Thickness (calibration curve) 8

19 Grid Polarizer GPR-8000 ( ) A grid is precisely produced on the substrate by the photographic technique. The grid polarizer enhances the sensitivity of the RAS-8000 Reflection Absorption Spectroscopy Attachment. Degree of polarization: 99% (at 0 µm), 95% (at 3 µm) Quenching ratio: 48: (at 0 µm), 23: (at 3 µm) Effective area: 25 mm dia. Angle scale: 360, 0 increments Material of substrate: KRS-5, 2 mm thick Measurement wavenumber range: 5,000 to 350 cm - Notes This grid polarizer cannot be used with the VeeMax II Series. GPR-8000 Spectrum of Elongated Polyethylene Film Red: Parallel polarization Black: Vertical polarization Spectrum of Elongated Polyethylene Film (Enlarged) Red: Parallel polarization Black: Vertical polarization FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 9

20 Reflectance Measurement Variable Incident Angle Reflectance Attachment VeeMAX II A ( ) VeeMAX II ( ) On this attachment, the incident angle can be varied within the range 30 to 80. Large samples can be measured as they are since the measurement position exits the sample compartment. An optional ATR prism and polarizer can be attached. VeeMAX II A is equipped with an accessory recognition function. Features Incident angle can be varied within the range 30 to 80. Measurement is possible by merely placing the measurement surface of the sample face down. A polarizer can be used to perform high-sensitivity measurement of thin films and measure the orientation of polarized light. A single-reflection ATR prism can also be attached. Exterior of VeeMAX II and Optional Polarizer Measurable Samples Coatings on flat metal surfaces Flat plastic sheet Attaching the optional ATR prism allows measurement of the following samples: Film, paper, rubber, plastic, fluid, gel samples Standard Content VeeMAX II Sample mask set Gold-coated mirror VeeMAX II Optical System Options ZnSe prism plate for solid samples, 45 incident angle Ge prism plate for solid samples, 45 incident angle Sample clamp for VeeMAX KRS-5 polarizer for VeeMAX Liquid sample retainer for VeeMAX System Combinations Reflectance measurement in the range 30 to 80 can be handled on the VeeMAX II Series. When performing high-sensitivity reflectance measurement using a polarizer, purchase a VeeMAX II Series main unit and KRS-5 polarizer for the VeeMAX. The GPR-8000 cannot be used. When performing ATR measurement of solid and film samples, purchase a VeeMAX II Series main unit, prism plate (45 ) for solid samples for VeeMAX, and sample clamp for VeeMAX. When performing ATR measurement of liquid samples, purchase a VeeMAX II Series main unit, prism plate (45 ) for solid samples for VeeMAX, and liquid retainer for VeeMAX. High-Sensitivity Reflection Spectrum of Hydroxylapatatite on Gold Plate and Fibrinogen Laminated Thin Film Exterior of VeeMAX II and Optional Polarizer 20

21 Diffuse Reflectance Measurement Diffuse Reflectance Spectroscopy In measurement of powder samples by the dispersive IR method, the KBr pellet method is often used. The powder sample is mixed with alkali halide powder, such as KBr, and briquetted into a pellet, which is then measured by the transmission method. This KBr pellet method is also used in FTIR, but the diffuse reflection spectroscopic method is easier to perform. As shown in the figure below, when a light beam is made incident on a powder sample, some part of the light is specularly reflected by the surface of the powder. The other part penetrates into the sample and is transmitted and reflected repeatedly, and then emerges out of the sample as a diffuse reflected (scattered) light. This diffuse reflected light is informative of the IR spectrum of the powder sample. Incident light Applications The diffuse reflectance spectroscopic method is applicable to any sample that can be pulverized. It also permits using, as the diluting substance, diamond powder or the like, which is not applicable to the KBr pellet method. This method is also applicable to detection of substances dissolved in a volatile solvent, such as fractions of liquid chromatography. LC effluent is made to drop on KBr powder, the mobile phase is removed by evaporation, and then the fraction is analyzed with the FTIR instrument equipped with a diffuse reflectance attachment. Remove mobile phase through evaporation Diffuse reflected light Specularly reflected light Diffuse reflectance attachment HPLC fraction KBr powder Detector Interferometer FTIR Reflection Within Powder Sample FTIR Analysis of HPLC Fractions Diffuse reflected light, which has been repeatedly transmitted within the powder sample, gives a spectrum similar to ordinary transmission spectrum. The spectral intensity is not completely proportional to the concentration of the compounds under study: those components which are detected as rather low intensity absorption bands are detected at higher intensity because the light beam is transmitted repeatedly in the sample. It is necessary, therefore, to compare diffuse reflected spectra with ordinary transmission spectra or to convert them with the Kubelka-Munk equation. f= (-R) 2 /2R = K/S where, K: absorption coefficient S: scattering coefficient R: reflection index (sample power spectrum/dilution power spectrum) Since it is very difficult to measure absolute reflection indices, diffuse reflection indices, which are the values relative to the reflection of KBr or KCI powder having no absorption in the IR region, are generally used. The spectra thus obtained are Kubelka-Munk converted to have intensities proportional to concentration. The result is spectra useful for quantitative determination. IRPrestige-2, IRAffinity- and FTIR-8000 Series incorporates the Kubelka-Munk conversion function as a standard feature. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 2

22 Diffuse Reflectance Measurement Diffuse Reflectance Attachment DRS-8000A ( ) DRS-8000 ( ) The method of diffuse reflectance spectrometry is one of the most popular FTIR application methods of application of FTIR. lt features high-energy throughput and simple operation. The Shimadzu FTIR Series incorporates, as standard, the Kubelka-Munk conversion functions, essential to diffuse reflectance spectrometry for correcting the light scattering by the KBr powder. QuickStart DRS-8000A includes the automatic accessory recognition function. Features The small measuring light beam (.8.8 mm) ensures reliable analysis of small samples. The attachment is a drawer type, which ensures easy replacing. The standard data processing functions include the Kubelka-Munk conversion functions as standard. DRS-8000 Standard Content Diffuse reflectance attachment Sample holder 2 mm ID cup Sample holder 4 mm ID cup Aluminum cup holder* Standard mirror Ground glass mirror Sample holding rod Hex key wrench Phillips screwdriver * Holder for disposable sample cup. Disposable sample cups are available as extra. To detector Sample Optics of DRS-8000 Options Sample cup, 50 pieces per set, aluminum, 6 dia..5 deep (mm) Sample die for aluminum cup SiC sampler Diffuse Reflectance Spectrum of Lactose Diffuse Reflectance Spectrum of Lactose After Kubelka-Munk Conversion 22

23 SiC Sampler ( ) In diffuse reflectance spectrometry, it is necessary to pulverize the sample and mix the powder with KBr powder. When the SiC sampler is used, the operation is simplified as follows: Diluent such as KBr powder is not required. The solid sample is ground with SiC emery paper and the sample powder on the emery paper is directly analyzed with the DRS (The SiC has a hardness of 9.0 and is quite chemically stable.) New emery paper is used as reference. Standard Content Holding rod Sample holder SiC emery paper (#320) SiC emery paper (#400) sheets 00 sheets SiC Sampler Supplies SiC emery paper (#320), 00 sheets SiC emery paper (#400), 00 sheets Sample holder that can be directly installed to the DRS-8000 Sticker type SiC emery paper Solid sample Construction of SiC Sample Diffuse Reflectance Spectrum of Plastic Products Obtained with SiC Sampler FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 23

24 Diffuse Reflectance Measurement Automatic Diffuse Reflectance Attachment DRS-800ASC ( ) Having the same optics as the DRS-8000, the DRS-800ASC accepts 24 samples to permit automated measurement. Features One-touch connection to the FTIR Series, which has the control capability as standard. With no external control unit required, the DRS-800ASC is very compact. Controlled by Labsolutions IR or IRsolutions software. Manual control to reduce the frequency of opening the lid of the sample compartment is possible, resulting in higher analytical productivity. Use of the disposable sample cups ensures easy exchange of samples. Notes When this attachment is used on IRPrestige-2, the ASC cable ( ) and Power unit ( ) is required. When this attachment is used on IRAffinity-, the ASC cable ( ) is required. The BASIC software is required separately for the HYPER-IR model. DRS-800ASC Standard Content Automatic diffuse reflectance attachment Sample holder, 24-sample type Standard mirror Sample cup Die Tweezers Sample handling rod Hex key wrench Phillips screwdriver 2 set 200 pair To detector Sample Supplies Sample holder, 24-sample type Sample cup, aluminum, 6 dia..5 deep (mm) Optical Diagram of DRS-800ASC Sample stage 24

25 Micro Sample Measurement Measurement of Micro Samples FTIR ensures such a high sensitivity as to permit reliable measurement of micro samples. There are three popular devices to measure micro samples: single-reflection ATR, beam condenser and infrared microscope. The objects of measurement are classified as the selected small part of the sample and a small part of a sample of uniform composition; measurement is made in either the reflection mode or transmission mode. These may be tabulated as follows: Single-reflection ATR Measurement ATR only mode Selection of the part to be Not possible measured Minimum measurable About 00 µm size Detector Installation Detctor of the FTIR (Measurement wavenumber range is limited by prism) Sample compartment of the FTIR Transmission mode As shown in the figures, both in the beam condenser and the IR microscope, the IR light beam from the interferometer is condensed by the optics and made incident on the sample. The light beam from the sample is expanded to the original size and condensed on the detector, and then measured with the detector. The measurement principle of measurement is the same as that of ordinary samples, but in the case of micro samples, it is important to take the sample thickness into due consideration. In measurement of 50 mm thick yarn samples, for example, if measurement is made without reducing the thickness, the detector signal will be saturated-resulting in deformed absorption bands. It is necessary to compress the sample using a diamond cell or the like. Ordinary glass lenses are used for visual observation, while reflection mirrors must be used for lr measurement. Reflection-type beam condenser Transmission only Not possible About 200 µm lr microscope Transmission/reflection/ATR Selection by aperture after observation in visual mode About 0 µm Dedicated MCT detector Detector of (Measurement wavenumber range the FTIR is limited by the MCT detector.) Sample compartment External installation of the FTIR To detector X-Y-Z stage Aperture Reflecting objective Autome sample Condenser mirror Sample Beam Condenser MCT detector Entrance for IR beam from the FTIR main Infrared Microscope (Transmission mode) IR light from interferometer Reflection mode Infrared microscopy is effectively used in reflection mode. As shown in the figure, the IR light from the interferometer is condensed by the reflecting objective and made incident on the sample, and the reflected light travels back to the same objective to be sensed by the detector. The paths for the incident light beam and the reflected light beam are switched by the wedge mirror. Though the measurement principle is the same as that of the samples of ordinary sizes, since the measurement is made on a very small area, specular reflection often occurs, resulting in abnormal peaks. The optics for visual observation and for lr rays are the same as that for the transmission mode. ATR mode microscopy Infrared Microscope (Reflection mode) The Attenuated Total Reflection (ATR) method is effectively used for samples that are opaque to IR rays, as well as for IR microscopy. It is especially effective for analysis of foreign materials on the resin surface and measurement of samples with curved surfaces. As shown in the figure, a semicircular prism is placed at the focus of the reflecting objective, and the light totally reflected by the interface of the sample and prism is measured to obtain the IR spectrum. IR beam ATR (Ge) prism Sample Schwarzchild reflecting objective mirrors. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 25

26 Micro Sample Measurement Automatic Infrared Microscope AIM-8800 Type ( for 20V, -93 for 220V, -94 for 240V, -34 for CE, 230V) Type 2 ( for 20V, -97 for 220V, -98 for 240V, -35 for CE, 230V) The AIM-8800 is used with the FTIR Series, and is installed to the right of the instrument. This infrared microscope features ideal, bright optics and a state-of-the-art MCT detector, enabling high-sensitivity detection of micro samples to enhance the full potential of the FTIR. In addition, the numerous advanced functions, such as auto aperture setting and auto focusing, greatly simplify the analysis of micro samples. The microscope may remain attached to the instrument during ordinary measurement, so switching to microscopic measurement from ordinary measurement is no more than a touch away. (Note: The AIM-8800 cannot be installed on the FTIR-800.) IRAffinity- Infrared Microscope System Features Ideal optical system, employing a state-of-the-art MCT detector for high-sensitivity analysis. Auto aperture, auto centering and auto X-Y stage functions simplify determination of the analysis location. Auto focus brings image in clear focus with one mouse-click. Up to 0 samples and 2 background measurement sites can be stored in memory. Stage movement, aperture setting and focusing, as well as switching between transmission / reflection and measurement / observation modes are all performed via the PC screen. Control is also possible using the microscope's key-board. 300 PC Printer CRT Key Board Relative Positioning of IRAffinity- and Microscope Monitor 700 mm Specifications Optics MCT detector (Glass dewar type) Signal-to-noise ratio Electrically activated aperture Motor-driven X-Y sample stage Microscope keyboard Operation PC control 5 Cassegrain objective 5 Cassegrain condenser mirrors Wavelength range : Wavelength range (near-infrared) (Note ) Type : cm - 0,000 to 3,800 cm - Type 2 : cm - With liquid nitrogen monitoring system Transmission mode, aperture size 50 mm, 8 cm -, 60 repeat scans 2600: or higher (Type ), 2000: or higher (Type 2) XYθ directional drive. Setting of XY direction increments is µm over Sample surface, and increments in θdirection (numerical entry possible). Minimum setting value : 3 µm Positioning range : X axis : 70 mm; Y axis : 30 mm Resolution. µm pitch Sample thickness : Reflection mode : < = 40 mm Transmission mode : < = 0 mm Measuring mode selection / XY stage operation (speed variable in 4 steps) / manual focusing / illumination control Measuring mode selection / XY stage operation /auto centering / manual focusing / auto focusing / illumination control / aperture setting / aperture preview / measurement position and aperture setting recording (0 sample positions, 2 background positions) Adhesive on Metal (measurement of part enclosed in blue in photo on right) Note : Near-infrared measurement is possible only when the NIR Set is mounted on IRPrestige-2 Note 2: When connecting to a PC-type FTIR-8000 Series, IRAffinity- and IRPrestige-2 the PC for operating the FTIR main unit is also used for operating the AIM When connecting to a non-pc-type FTIR-8000 Series, the PC must be purchased separately. Contact us for details on parts required for connecting the FTIR to the AIM Spectrum of Adhesive on Metal 26

27 ATR Objective Mirror ATR-8800M ( ) A semicircular prism made of ZnSe is used. x 5 magnification; 30 incident angle, and single reflection. The prism is a slide type and permits switching between visual observation mode and IR measurement mode. Features Small prism enables focusing and measurement of even small samples. Measurement range of 5,000 to 700 cm - Maintenance Parts Replacement Ge prism Other Optional for Microscope Aluminum reference mirror KBr window plate CaF2 window plate Visible objective lens (x0) Visible objective lens (x20) Infrared polarizer (Infrared polarizer and holder are required.) Visible polarizer Remarks 3 mm dia. 3 mm dia. 2 mm thick 3 mm dia. 2 mm thick Infrared polarizer holder Infrared polarizer (STJ-00) Please contact us for details. ATR-8800M ATR Objective Mirror Spectrum of Adhesive on Fiber Sampling Kit ( ) This kit is for pretreating samples for microscope measurement. It comprises a set of tweezers, roller knife, needles, scissors, replacement blades and replacement needles. Standard Content Tweezers (straight) Tweezers (curved) Roller knife Needle (straight) Needle (bent) Needle holder Scissors Replacement blades (pack of 5) Replacement needles (pack of 5) Exclusive case Sampling Kit FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 27

28 Micro Sample Measurement Diamond Cell This pressurized cell thinly compresses samples with a certain degree of thickness or minute samples placed on a microscope's stage to perform transmission measurement as they are. This cell is applicable to a variety of samples including drugs, rubber and plastic. Two types of cells are available, Diamond Cell C using an artificial diamond and Diamond Cell B using a natural diamond. Spectrum of Single Fiber Red: Diamond cell used Black: Diamond cell not used Notes Diamonds exhibit slight absorption in the range 3,000 to,500 cm -. Diamonds are hard but brittle and may crack depending on the sample and method of use. Diamond Cell C ( ) A pressurized cell-enabling microscopic measurement of minute, thinly compressed samples as they are. Applicable for analysis of drugs, rubbers, plastics, polymers, etc. The Diamond Cell B noted above employs a natural diamond, and is therefore relatively expensive. This Diamond Cell, on the other hand, uses an artificial diamond, so is less expensive and, further, employs a thinner and larger diameter window (.6 mm). Although its strength is slightly inferior to the natural diamond, it is adequate for compressing nearly all samples. Features Large-size diamond provides.6 mm diameter window Large diameter window allows measurement even when placed in standard sample compartment Measurement possible by merely placing on infrared microscope stage Standard Content C plate C screws Holder with diamond window for C Case 3 2 Diamond Cell C Options and Maintenance Parts C plate C screws (pack of 3) Holder with diamond window for C Diamond Cell B ( ) This attachment is used to compress a micro sample into a thin plate, which is then directly measured by infrared microscopy. This method is applicable to various types of samples, such as pharmaceuticals, rubbers, plastics, and polymers. Features Use of the Type II diamond cell allows measurement to be made over the entire wavenumber range. Even thick samples can be measured in the transmission mode, with a high sensitivity. Micro samples are made flat, so that high sensitivity is obtained during measurement. Measurement is made with the diamond cell placed on the stage as it is. Adjustment for sample thickness is made with a precision screw. Cells with a cell plate of lower-cost material are also applicable. Combined use with an infrared microscope is recommended. Diamond Cell B Standard Content Diamond cell Holder with compression cap O ring pair set Options and Supplies Diamond cell for spare CaF2 window, a pair KBr window, a pair

29 Micro Vise Holder ( ) This holds various types of samples for microscopy. It ensures positive holding of samples of a difficult shape or measurement of a sample at a user-selectable angle. Measurement with a polarizer, with the sample under tensile load, provides information on the molecular orientation. Sizes of Holdable Samples Tensile load Gripped load Within approx. width of 20 mm Film of length 4 to 54 mm (excluding grip allowance) Max. approx. length 40 mm Approx. width 40 mm Standard Content Micro vise holder Holding fixture 2 Micro Vise Holder Reflection-Type Beam Condenser RBC-8000 ( ) This beam condenser is especially useful for transmittance measurement of micro samples. Features Since no lenses are used, measurement can be made over the entire wavenumber region of the FTIR instrument. Combined use with an ultramicro cell, 0.05 mm optical path, permits transmission measurement of 2 to 3 µl of liquid samples. The light beam is reduced to /5 (about.8.8 mm). Standard Content RBC-8000 reflection-type beam condenser Sample holder, with X-Y-Z stage Pellet sample holder Hex key wrench Phillips screwdriver W-Y-Z stage Sample Optical Diagram of RBC-8000 RBC-8000 FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 29

30 Accessories for Automated Measurement Automating the Operation The technique of Fourier Transform Infrared Spectrophotometry (FTIR) is now extensively used in various fields for R&D and industrial purposes. Since samples measured by infrared spectrophotometry are mostly chemically stable and can be measured without pretreatment, it is fairly easy to automate the measurement of many samples. Automating the measurement saves labor and ensures high analytical productivity. Automating the FTIR Measurement One of the most important methods to automate the operation of the FTIR main is to utilize a computer system. Combination of a computer and the program, described below, provides automation of sample loading and unloading, measurement, data processing, and presentation of the analytical results. The photo to the right shows the ASC connector (supplied as standard), which is used to export the control signals to an automatic sample changer. The software incorporated in the FTIR can control the automatic sample changer via a pair of the ASC connectors. Operation by Automated Sequence The operation must be carried out in the sequence programmed to be most appropriate for the particular type of samples under study. The Shimadzu FTIR-8000 Series instruments (except FTIR-8000PC Series) incorporate, as standard, the SPECTROMACRO software, which permits flexible programming through simple procedures. As for the FTIR-8000PC Series, the optional BASIC software has the same functions as SPECTROMACRO. IRPrestige-2, IRAffinity- and FTIR-8400S (IRsolution model) can be controlled from the software. ASC Connector 30

31 Automatic Diffuse Reflectance Attachment DRS-800ASC ( ) This attachment automates measurement of up to 24 samples. For details, refer to page 24. Auto Sampler for Transmission Measurement ASC-8000T ( ) This attachment accepts up to 8 samples for measurement in the transmission mode. Features The control is made by the standard control signals from the FTIR main, meaning no external controller is required. The attachment is easily installed in the standard sample compartment. A holder for a 3 mm dia. pellet is provided. Use of the window-plate option enables measurement in the Nujol method. DRS-800ASC Notes When this attachment is used on IRPrestige-2, the ASC cable ( ) and Power unit ( ) is required. When this attachment is used on IRAffinity-, the ASC cable ( ) is required. The BASIC software is required separately for the HYPER-IR model. Standard Content ASC-8000T main Pellet holder Fixing spring Tweezers pair Options KRS-Window set (with a set of window holder) Film holder (9 pcs. as a set) ASC-8000T Sample Switcher 2 ( ) All the Shimadzu FTIR Series spectrophotometers are single-beam type. This attachment allows any one of them to be operated in the "quasi double-beam mode" by switching two samples during measurement. Features Two cassettes for liquid cells or pellet holders are provided. In the case of the FTIR Series, the optional BASIC software is necessary for the "quasi double-beam mode (except FTIR-8200PC / 8300 / 8400 / 8400S / 8700 / 8900, IRAffinity-, IRPrestige-2. Accessories That Can Be Used Evacuable die for KBr pellets Sealed liquid cell Magnetic pellet holder Diamond cell Sample holder for MHP- Mini Hand Press Fixed thickness cell Magnetic film holder 0 cm gas cell Sample Switcher 2 Accessories That Cannot Be Used 5 cm gas cell Notes When this attachment is used on IRPrestige-2, the ASC cable ( ) and Power unit ( ) is required. When this attachment is used on IRAffinity-, the ASC cable ( ) is required. The BASIC software is required separately for the HYPER-IR model. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 3

32 Purge Control Kit Purge Control Kit PCK-894 ( ) for IRAffinity-, FTIR-8400/8400S/8900 Series PCK-2 ( ) for IRPrestige-2 The FTIR Series uses a sealed interferometer to ensure high sensitivity and stability during measurement without using dry air. To eliminate the interference of carbon dioxide and water vapor, it is recommended to purge the interferometer, the sample compartment, the second sample compartment, etc. through a combined use of the purge control unit and the dry air supply unit or nitrogen gas. This kit is for adjusting the piping between the FTIR and purge gas source, piping sections along which purge gas flows and the purge gas flow rate. This kit contains the following parts: Flow path and flow rate controller Purge tube (0 m, 7 mm I.D., 0 mm O.D.) Exhaust parts Notes The purge control kit cannot be used with the DBX Ventilate the site when purging with nitrogen gas. PCK-2 Dry Air Supply Unit ( for 50 Hz line, 00 VAC) ( for 60 Hz line, 00 VAC) This unit is very easy to install: all you have to do is to connect pipes to the inlet and outlet of the unit. Also, the unit is quite compact and provided with casters so that it can be easily carried around. The noise of the air compressor is minimized by the use of sound-proofing materials. Note Dimensions: W400 D60 H60 mm Dry air supply capacity: 0 to 20L / min. Dry air: -7 C or lower in dew point. 32

33 External Detector / Optional Detector External Detector / Optional Detector A DLATGS detector or LiTaO3 detector is mounted as standard on the IRPrestige-2, IRAffinity- and FTIR-8000 Series. Some applications require use of a high-sensitivity MCT detector or external installation of a special optical system. Required Parts IRPrestige-2 IRAffinity- FTIR-8000 Series ) When Using the MCT Detector MCT Kit - Second sample compartment ) Cannot be used on the FTIR-800/8200/8500/8600. External Light Beam Switching Kit ( ) When Using an External Optical System External Light Beam Switching Kit External Light Beam Switching Kit Second sample compartment External Light Flux Extraction Kit This kit extracts infrared light from the right side of the IRPrestige-2, IRAffinity- and FTIR-8000 Series, and switches the light to externally installed accessories such as an infrared microscope. Also attached is a polystyrene film about 50 µm thick so that instrument validation can be filly automated based upon Japanese Pharmacopoeia, European Pharmacopoeia or ASTM. Note, however, that a separate standard sample must be prepared if traceability is required. This kit can be used on the FTIR-8300/8400/8400S/8700/8900, IRAffinity- and IRPrestige-2. Standard Content Switching mirror (with polystyrene film) External input signal connector set Exterior and Content of External Light Beam Switching Kit Notes Traceability is not provided for the polystyrene film. This kit cannot be used on the FTIR-800/800M/800A/8200/8200D/8200A/8500/8600 and FTIR-8200PC/8600PC. MCT Kit ( for IRPrestige-2) A high-sensitivity MCT detector is used when analyzing minute or dark samples, or performing measurement using a long pathlength gas cell. This kit is an MCT detector unit installed on IRPrestige-2 for switching between the standard DLATGS detector. Switching of detectors is performed automatically from IRsolution. It has a built-in liquid nitrogen monitor to cut off current flow when the detector element is not being cooled, thus protecting the MCT detector. The liquid nitrogen dewar is made of glass and does not require reevacuation. Specifications Detector Wavelength range Liquid nitrogen retention time Liquid nitrogen cooled MCT detector With glass dewar (approx. 300 ml) With liquid nitrogen monitor 5,000 to 650 cm - 8 hours (when liquid nitrogen is newly purchased) Notes This kit cannot be mounted at the same time as the NIR set. Liquid nitrogen is required when using the MCT detector. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 33

34 Transmission Measurement Accessories for Transmission Measurement Film samples can be measured easily if they are attached to the standard cassette or optional film holder. Cassette (Sample Holder) ( ) A cassette (sample holder) provided as standard on the FTIR can be used for options for attaching to cassettes for liquid and gas cells. However, with some accessories, there may be clearance between the cell and the cassette, which sometimes results in poor attachment reproducibility. Also, bending sometimes occurs when heavy accessories such as the 0 cm gas cell are attached. Use this optional cassette when performing measurement with such accessories with better reproducibility. This attachment cannot be used on the FTIR-800/800M/800A/ 8200/8200D/8200A/8500/8600 and FTIR-8200PC/8600PC. Features Little clearance Rigid Standard Content Cassette ASSY Maintenance Parts Cassette mounting screws Magnetic-Type Film Sample Holder ( ) Film samples are held between the stainless backplate (SUS 430) and rubber magnet for direct analysis. Standard Content Backplate (SUS430) Magnet sheet without hole Magnet sheet with 3 mm dia. hole Magnet sheet with 7 3 mm hole Magnet sheet with 7 9 mm hole Magnet sheet with 0 23 mm hole Dimensions of Magnetic-Type Film 34

35 Universal Clip Holder ( ) This holds a sample by one-touch operation through the use of a clip. A silicone rubber o-ring is used for positive contact and sample protection. Pressure nut Clip Features Applicable sample sizes range from 3 to 40 mm in diameter, and up to 3 mm thick. The pressure nut ensures easy measurement of mull samples. The rubber magnet and o-ring are used for positive holding of samples. Standard Content Universal clip holder Magnet base, 22 mm dia. Magnet base, 0 4 mm hole Spare O-ring O-ring Slide stopper Universal clip holder Magnet base Spare O-ring EZ-Clip3 ( ) This one-touch sample holder uses a clip exclusive for 3 mm dia. samples. An O-ring is located on the surface of the holder that contacts the sample to prevent damage to the sample. Features Thick samples (max. thickness 3 mm) also can be held. Diameter of light passage hole: 0 mm Standard Content EZ-Clip3 EZ-Clip25 ( ) This one-touch sample holder uses a clip exclusive for 25 mm dia. samples. An O-ring is located on the surface of the holder that contacts the sample to prevent damage to the sample. Features Thick samples (max. thickness 3 mm) also can be held. Diameter of light passage hole: 0 mm Standard Content EZ-Clip25 FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 35

36 Transmission Measurement Gas Cell Gas cells are used when measuring gas samples. Select the optical pathlength to suit the concentration of the component. Short Pathlength Gas Cells 5 cm Gas Cell ( XX) 0 cm Gas Cell ( XX) Used for measurement of gas samples or liquid samples of low boiling points. The cells are designed conic to make the inner volume smaller. The inner volumes of the 5 cm and 0 cm gas cells are 42 ml and 98mL, respectively. The last two digits of the catalog numbers show the material of the window plate, as listed below. Cell Window Plates NaCl KBr KRS-5 Type of Window Plate Last two digits of Spectrum of HCl Gas Long Pathlength Gas Cell A gas cell with a long pathlength is used when measuring low concentration gas samples. Inside a long pathlength gas cell, light repeatedly doubles back, which results in a long pathlength. There are two types of long pathlength gas cells, one with a sample compartment and the other with a second sample compartment. A regular MCT detector is used as the detector. The pathlength of long pathlength gas cells, gas cell material, window plate material, and detector must be selected according to the gas component, concentration, temperature, capacity, and other factors to be measured. When selecting a long pathlength gas cell, contact us so that you can select the appropriate cell. Dimensions of Long Pathlength Gas Cell to detector Pressure gauge Window Sample inlet / outlet pipe Optics of Long Path Cell 36

37 Pellet Measurement KBr Pellet Method With this method, powder samples are diluted with KBr powder to produce pellets for transmission measurement. On the FTIR, the light intensity is large, so measurement is possible using pellets made easily with the Mini Hand Press. When making regular 3 mm dia. pellets, the evacuable die for KBr pellets, hydraulic press and vacuum pump are used. Mini Hand Press MHP- ( ) This is a compact, inexpensive hand-driven press used to produce KBr pellets. A pellet produced in the frame is directly measured using the dedicated holder; this ensures exceptional simplicity of operation. No dies or vacuum pump are required. Standard Content 2 Mini Hand Press Pellet holder Upper and lower cylinder set Briquetting frame, 4 mm dia Pellet remover Pellet remover base * Parts other than Mini Hand Press are provided as maintenance parts. 2, 5 and 6 are shared for 4 and 3 mm dia. parts. Options and Maintenance Parts 4 mm dia. briquetting frame, 20 pieces 3 mm dia. briquetting frame, 0 pieces Upper/lower cylinder set 3 mm dia. briquetting frame, 20 pieces The following items are recommended for using MHP- KBr Crystal 00 g Agate Mortar and Pastle each Micro spatula Evacuable Die for KBr Pellets ( ) Used to prepare KBr pellets, 3 mm dia. The amount of KBr crystal necessary for one pellet is about 200 mg and the sample to 2 mg. Standard Content Base 2 Barrel 3 Spring 4 Plunger 5 Mandrel 6 Die frame 7 Pellet holder 8 Punching rod 9 Punching base 0 Plug Sieve 2 Exhaust port * Packet of one when ordering by this * * * The following items are recommended for producing pellets of high transmittance: SSP-0A Hydraulic Press SA8-3M Vacuum Pump KBr Crystal Agate Mortar and Pestle Micro spatula g each FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 37

38 Pellet Measurement Micro Die for 2 mm dia. KBr Pellets ( ) Micro Die for 5 mm dia. KBr Pellets ( ) Used in combination with the KBr die ( ), which is for 3 mm dia. pellets, to produce smaller pellets, 5 mm or 2 mm in diameter. Specify the diameter you require or the Cat. No. when placing an order. 4 Standard Content Mandrel for 2 mm dia. pellets Mandrel for 5 mm dia. pellets Die frame for 2 mm dia. pellets Die frame for 5 mm dia. pellets Tool Pellet holder Hydraulic Press SSP-0A ( ) Used for producing KBr pellets. The maximum pressure is 0 tf/cm 2. A high-precision pressure gauge is provided. Vacuum Pump SA8-3M ( ) This is a compact rotary vacuum pump, having a displacement capacity of 0 to 30 L/min., used for vacuum dehydration in production of KBr pellets. (00 VAC power is required.) 38

39 Magnetic-Type Pellet Holder ( ) 3 mm diameter pellets are held between the stainless backplate (SUS430) and rubber magnet for direct analysis. Agate Mortar and Pestle ( ) Used to prepare KBr pellets or samples for diffuse reflectance method. KBr Crystal (00 g) ( ) Used to prepare KBr pellets. Features a long storage life, thanks to its low hygroscopicity. FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 39

40 Cells for Liquid Samples Measurement Using Demountable Cells Demountable cells, sealed liquid cells, fixed thickness cells, etc. are useful for measurement of liquid samples. In quantitative analyses, it is necessary to know the thickness of the cell accurately. Interference patterns are often used for the thickness measurement. In transmission/reflection FTIR of thin films, an interference pattern as shown above is overlaid on the spectrum. The film thickness, t, is given by the next equation: M n= 2 n2 -sin 2 θ(ν-ν2) where ν and ν2 are the wavelengths of peaks or valleys, M is the degree of interference (number of the waves) between ν and ν2. When the refractive index (n) of the film is known and is uniform between the ν and ν2, the cell thickness may be obtained from the above equation. In practice, the cell is measured without any sample in it, and its thickness is obtained by substituting n = and θ = 0. Demountable Cell ( XX) This type of cell is used for qualitative analysis of less volatile liquid samples, Nujol mulls, or film samples. The cell is assembled and disassembled in each analysis run Type NaCl Demountable Cell KBr Demountable Cell KRS-5 Demountable Cell A pair of NaCl plates ( ) A pair of KBr plates ( ) A pair of KRS-5 plates ( ) Contents Metal holder ( ) 0.05 mm lead spacer ( ) set mm lead spacer ( ) 0sheets 0. mm lead spacer ( ) 0 sheets 0 sheets Sealed Liquid Cell ( XX) This type of cell is used for measurement of volatile liquid samples. The cell is assembled sandwiching a spacer of the desired thickness, a sample is injected into the cell, and then drawn out with a syringe. When it is necessary to prevent leaks of samples, the use of the fixed thickness cell is recommended Type Contents NaCI Sealed Liquid Cell A pair of NaCl plates, with and without hole ( ) Metal holder ( ) Gasket ( ) Lead cushion ( ) Rubber cushion ( ) PTFE stopper ( ) Syringe ( ) KBr Sealed Liquid Cell A pair of KBr plates, with and without hole ( ) KRS-5 Sealed Liquid Cell A pair of KRS-5 plates, with and without hole ( ) set mm lead spacer ( ) 4 sheets 2 pcs mm lead spacer ( ) 4 sheets 2 pcs. ( ) for KRS-5 2 pcs. 0. mm lead spacer ( ) 4 sheets 2 pcs. ( ) for KRS-5 pc. 0.5 mm lead spacer ( ) 4 sheets ( ) for KRS-5 40

41 Fixed Thickness Cell ( XX) This type of cell is used for quantitative measurement of liquid or volatile samples. The cell is assembled in the Shimadzu factory to have the customer-specified cell thickness. Matched pair of fixed thickness cells are also available. The last two digits of catalog numbers indicate the type of cell window plates, as shown in the table below: Example: The catalog number of the fixed thickness cell, 0. mm in thickness, KBr window plate, is Cell Window and Thickness Thickness mm 0.05 mm 0. mm 0.2 mm 0.5 mm.0 mm 2.0 mm 5.0 mm NaCl KBr KRS-5 Not available FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 4

42 Cells for Liquid Samples Sample Cell for Oil Content Determination This cell is used to quantitatively determine the concentration of oils extracted into carbon tetrachloride. Optional path length Capacity Type of cell 00 mm 50 mm 0 mm 5 mm 2 mm mm ml 9 ml 4 ml 2 ml 0.8 ml 0.4 ml a set of 2 Spacer ( ) is required Spacer ( ) is required Spacer ( ) is required Oil content cell holder Type ( ) Square cell holder ( ) Crystal Polishing Kit ( ) This kit is used for polishing an NaCl and KBr window plate. The kit contains a polishing plate, abrasive, chamois and rubber gloves. Note: Do not polish KRS-5 window plate. 42

43 Others Far Infrared Kit ( ) In the far infrared region up to 240 cm -, peaks of inorganic compounds and organometallic complexes are observed. The Far Infrared Kit is a Csl beam splitter mounted on the IRPrestige-2 for measuring spectra in the far infrared region. Using the Csl beam splitter enables spectra in the far infrared region up to 240 cm - to be measured. A standard light source and detector are used. Since the 500 cm - to 240 cm - region absorbs lots of moisture in air, purge the instrument with dry air or dry nitrogen gas, for example, before performing measurement. Also, store the Csl beam splitter in a desiccator when it is not in use since it is extremely sensitive to moisture. Feature Far Infrared Spectrum of Polyvihylidenchloride Measurement wavelength range 5000 cm - to 240 cm - Standard Content Csl beam splitter FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 43

44 NIR Measurement NIR Measurement Accessories for the IRPrestige-2 Accessories are available for easier and higher-sensitivity NIR measurement of a wide range of samples. Each accessory is equipped with the Automatic Accessory Recognition function. When the accessory is fitted to the sample compartment, the accessory type and its serial number are recognized automatically and the optimal measurement parameters are set. Applications and Accessories Multicomponent Quantitation of Liquid Samples The quantities of various components in liquid pharmaceuticals and foods are measured and controlled. For example, quantitation can be made of the quantities of components such as sugar and proteins when manufacturing soft drinks. In this case, the location and shape of each component peak will depend on temperature. Therefore, measurement is conducted at a constant temperature using a heating transmission cell system. Here, the PLS Quantitation Program will be required to create the calibration curves. Introduction to Near-Infrared (NIR) Analysis In the near IR regions, absorption due to molecular vibration appears. Therefore, substances can be identified by comparing spectral patterns, and quantitatively determined from the peak intensity. Absorbance is lower in the near IR region than in the mid IR region, so samples can be measured without dilution. The IRPrestige-2, which employs the Fourier transform method and offers spectra with high wavelength precision, is optimal for identifying substances by comparing spectral patterns. Samples contained in glass or thin plastic containers can be measured directly. It is also possible to analyze a sample using a probe. Thus, sample pretreatment is easy, and the near IR measurement is also suitable for measuring samples that cannot be easily unpacked. Near-Infrared Applications Near-Infrared is used for qualitative and quantitative analysis, just as with the mid-infrared. Its applications include quality inspections of raw materials received, and endpoint quantitations for reaction processes. Acceptance Inspections for Raw Materials (Qualitative) When determining whether the correct raw materials have been delivered based on the spectral shape, select accessories in accordance with the form of the raw materials. After measurement, pass/fail determinations and library searches can be conducted using the PharmaReport program. If the sample is a powder, use either diffuse reflection equipment UpIR A, near-infrared integrating sphere IntegratIR A, or a reflection-type fiber probe. For liquid samples, pastes, pellets, and cloths, use near-infrared integrating sphere IntegratIR A. For tablet samples (pharmaceuticals), use either near-infrared integrating sphere IntegratIR A or a reflection-type fiber probe. For diffuse reflection equipment UpIR A and near-infrared integrating sphere IntegratIR A, the sample is prepared, and the prepared sample is then placed in the measurement window for measurement. Measurement can be conducted as is with the sample placed in the test tube included, or left in a plastic bag. In the latter case, however, there may be a significant impact from the bag's interference fringe. If the reflection-type fiber probe is used, measurement is possible without sampling. The probe can be inserted directly into the sample, or measurement can be taken directly of a sample placed in a glass bottle or plastic bag. In the latter case, however, there may be a significant impact from the bag's interference fringe. Difference Between UpIR A and IntegratIR A Diffuse reflection equipment UpIR A and near-infrared integrating sphere IntegratIR A differ as shown below. The selection should be made on the basis of the experimental objective. Benefits of IntegratIR A. The peak strength is several times stronger than for UpIR A, and the obtained spectrum has a superior S/N ratio. 2. Good data is obtained when measuring powdered samples in plastic bags. 3. Measurements can be conducted of pellets, pastes, tablets, liquids and cloth samples. Benefits of UpIR A. Cost 2. Specialized for powdered sample analysis. 44

45 NIR Set ( ) This option is attached to the IRPrestige-2, enabling near-infrared measurement. Experiments are conducted via software that switches between the mid-infrared and the near-infrared. (Cannot be used with IRAffinity- or FTIR-8000 series.) Specifications Standard Contents Measurement Range: 2,500 cm - to 3,800 cm - Beam Splitter: Silicon-coated CaF2 Light Source: Tungsten iodine lamp Detector: InGaAs detector Product Name Beam Splitter Storage Box CaF2 Beam Splitter Upload Type Diffuse Reflectance Attachment UpIR A ( ) Powder samples can be placed on the sample stage for measurement. Pretreatment such as KBr dilution is unnecessary. Powders can be measured directly. Alternatively, directly set the sample contained in a plastic bag or glass bottle. Applications include qualitative or verification tests in acceptance inspections and quantitative analysis of components contained within samples. Specifications Measurement range: 0,000 to 3,800 cm - Accessory recognition function: Included Standard Accessories Options Product Name Product Name UpIR A Main Unit Test tube with screw cap (pack of 200) Gold-coated mirror for reference Sapphire window Test tube (pack of 6) Test tube holder Sample holder with sapphire window NIR Integrating Sphere IntegratIR A ( ) Pretreatment such as KBr dilution is unnecessary. Samples contained in a plastic bag or glass bottle can be measured. Applications include qualitative or verification tests in acceptance inspections and quantitative analysis of components contained within samples. Powders, tablets, liquids, pastes, fibers, plastic pellets and molded samples can be placed on the sample stage for measurement (reflectance measurement). A highly sensitive InGaAs detector is built-in. The IntegratIR installation kit ( for IRPrestige-2 CE model, or for other IRPresige-2 model) or External light beam switching kit must be purchased separately. Specifications Measurement range: 0,000 to 3,800 cm - Accessory recognition function: Included Standard Accessories Product Name IntegratIR A Main Unit Gold diffusion mirror with protective cap Options Spectrum of a tablet (antipyretic) Test tube (pack of 25) Product Name Test tube holder Test tube (pack of 25) FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 45

46 NIR Measurement Heating Transmission Cell ( ) Liquid samples contained in the 6-mm diameter test tube can be measured while they are being heated, or maintained at a constant temperature. Applications include multi-component quantitative analysis of liquid samples and tracing reactions and changes in the sample under heating. The temperature can be set from room temperature to 20 C. The set comprises a transmission cell for measurement under heating and a temperature controller. Specifications Measurement range: Accessory recognition function: Temperature range: Applicable test tube: Output: Power supply: Standard Accessories Product Name Heating Transmission Cell Holder Temperature Controller 6 50 mm test tube (pack of 500) 2,500 to 3,800 cm - Included Room temperature to 20 C (heater temperature) 6 mm dia. 50 mm 5A Max. 20/220 V selectable Results of measuring octanoic acid under heating (measured at 0 C intervals from 30 to 20 C). Increase in liberated OH (6,920 cm - ) caused by heating can be verified. Options Product Name 6 50 mm test tube (pack of 500) Infrared Microscope AIM-8800 ( XX) NIR measurements of microscopic parts of the sample can be made. By fitting the AIM-8800 to an IRPrestige-2 unit with the NIR set installed and using the high-sensitivity MCT detector, measurements can be conducted in the 0,000 to 3,800 cm - region. In order to use this accessory, the Light Beam Switching Kit, AIM Connection Kit ( ) and Video Capture device are required separately. The AIM-8800 will not work with notebook PCs. Specifications Measurement range (Note) : 0,000 to 3,800 cm - Equipped with an electrically powered aperture and stage PC control (measurement position memory function/ auto-centering/ auto focus etc). Can also be operated from the keyboard Note: If combined with an IRPrestige-2 unit with the NIR set installed. Options Product Name Mapping Program (IRsolution) Reflection spectrum of an electronic part. The thickness of the coating film was calculated to be 2.28 µm from the interference fringe. (refractive index.5) 50 %T /cm 46

47 Optional Software Wide Variety of Optional Programs A variety of optional software is available for IRsolution, the Windows-based FTIR control software that offers outstanding ease-of-operation and functionality. IRsolution features standard functionality that includes data processing functions, such as subtraction spectra and Kubelka-Munk transform functions, quantitative analysis functions, such as multi-point calibration curve and multi-regression methods, and spectral search functions. Adding optional software programs allows extending the range of applications even further. IRsolution Agent ( ) IRsolution Agent is a tool for managing data from IRsolution results in a database. This allows managing analytical data records over their entire life cycle, from creation (measurement), review, approval, storage, viewing, backup, and disposal. Compliant with FDA 2 CFR Part (electronic records and electronic signatures), this program provides security management and electronic signature functions for data stored and recorded in a database. Measurement data is automatically saved in a database to allow easy searching of target data at a later time. Spectral waveform data, peak detection tables, and other information stored in the database can be view directly. Note: Not compatible with data measured or analyzed using the mapping program. Mapping Program ( ) The mapping program captures microscope images and synthesizes them to create a visual image for large areas. It allows specifying the range, measurement interval, background position, and other mapping parameters on the synthesized image. Icons are provided for switching between transmittance and reflectance modes, and other microscope and mapping operations. Mapping modes include area mapping, linear mapping, and random mapping (a feature that automatically maps multiple desired measurement points specified in advance). In addition to normal mapping using transmittance or reflectance modes, microscope ATR mapping measurement is possible (ATR object mirror is optional). From the mapping data obtained, spectra can be extracted and functional group maps can be calculated for specific peaks. Data can be rendered in 3D, with contour lines, or as an overlay of spectra. Measurement Example of Area Mapping (area map of flux on a circuit board) FTIR Series Accessories Fourier Transform Infrared Spectrophotometers 47

48 Optional Software Macro Platform ( ) Macro Platform is a module to run Macro programs provided by Shimadzu on IRsolution software. Please contact your Shimadzu representative when you need an automatic measurement system with an automatic sample changer or to perform routine operation with repeated specified operations. 3D Display Program ( ) The 3D display program offers the following functionality. Changes the method of displaying datadata can be displayed in bird s eye view (3D), as an intensity distribution or using contour lines, as a spectral overlay, or rotated. 3D data processingchanges at specific wavenumbers can be isolated. Functions include data extraction, data points thinning, smoothing, zero-baseline, background correction, normalization, log conversion, first- or second-order derivative, and ATR correction. Creation of 3D data from spectraspectra measured at fixed intervals, such as by repeated measurements, can be arranged consecutively to create 3D data. Note: The 3D display program cannot control mapping measurements or AIM-8800 series infrared microscopes. PLS Quantitation Software ( ) PLS (Partial Least Squares) quantitation is a widely used Chemometrics method like the Multiple Linear Regression (MLR) method for quantitation of multicomponents.irsolution has PLS I and PLS II methods for PLS quantitation. IRsolution analyzes PLS calibration curves by calculating "Influence", "Residuals", "Scores", "Loadings", "Press Values", etc. Screen of PLS quantitation Curve-Fitting (Peak-Splitting) Software ( ) Usually, an IR band can consist of several overlapping peaks. Curvefitting (Peak split) software separates IR bands into individual component peaks. This software is good for many applications, such as analysis of a peak with hydrogen bond influences and analysis of hidden peaks overlapped with other peaks.curvefitting (Peak split) software separates the band with suitable curves from 6 types of curves such as Gaussian, Lorentian, Gaussian+Lorentian. Component peaks and a synthesized peak are displayed to evaluate the separation. Curvefitting (Peak split) result of peak ( cm - ) of ABS resin spectrum. Top : Target peak and specified peaks Bottom : Component peaks and a synthesized peak 48