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C103-E005H

FTIR Series Accessories

Sh i ma dzu F o u ri e r Tra n sfo r m In fra re d Spe c tro ph o to me te rs

F TI R Acc esso r i e s O v e r v iew

Se l e c t i o n o f O p tio n al A cc e s s ories
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 singlebeam 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.

Rubbers

Powders

Paper, cloth, yarns Films, plastics

Solids Coating films on metals

Coating films on resins

Semiconductors

Type of Sample

Oil content measurement Nonvolatile organic solvents Liquids Volatile organic solvents Aqueous solutions

Extract solutions IRPrestige-21

Gases

Concentration

Micro/trace samples

Liquids

IRAffinity-1

Solids

Total reflectance method Pyrolysis Liquid film method Nujol method KBr pellet method Total reflectance method Diffuse reflectance method Total reflectance method Thicker than 100m Thinner than 100m Dissolve in solvent Grind Thicker than 1 m Total reflectance method Transmission method Film method SiC sampler Specular reflectance method Total reflectance method Thinner than 1 m Mix with KBr powder Reflection absorption spectrometry KBr pellet method Diffuse reflectance method Total reflectance method Specular reflectance method Film holder Surface measurement Total reflectance method Total reflectance method

ATR-8000A, ATR-8200HA, Single-reflection ATR, etc. (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-8000A, ATR-8200HA, Single-reflection ATR, etc. ATR-8000A, ATR-8200HA, Single-reflection ATR, etc. Film holder .............. Use grid polarizer for study of molecular orientation Demountable cell .... Evaporate the solvent to obtain the film DRS-8000A, SiC sampler SRM-8000A, VeeMAX2A ATR-8200HA, .......... Measurement to a depth of 1/5 of the wavelength with a KRS-5 prism and to 1/10 with a Ge prism Single-reflection ATR RAS-8000A, ............ Use of a grid polarizer enhances sensitivity about two times VeeMAX2A KBr die + hydraulic press + vacuum pump (or mini hand press) DRS-8000A ATR-8200HA, .......... Measurement to a depth of 1/5 of the wavelength with a KRS-5 prism and to 1/10 with a Ge prism Single-reflection ATR SRM-8000A, ............ Convert a reflection spectrum into the absorption spectrum by the Kramers-Kronig method VeeMAX2A ATR-8200HA, Single-reflection ATR (Ge prism) Quartz cell .............. Detection limit is 1ppm level with 10 mm optical path

Liquid film method Rapid measurement Solution method Above 10% in concentration Below 10% in concentration Difference spectrometry Evaporate solvent Liquid film method Total reflectance method Solution method Diffuse reflectance method Total reflectance method

Demountable cell Fixed thickness cell, sealed liquid cell Demountable cell with KRS-5 or ZnSe window ATR-8200HA, Single-reflection ATR Fixed thickness cell DRS-8000A ............. The sample solution is supplied dropwise on KBr powder and measured after evaporating the solvent ATR-8200HA, Single-reflectionATR ............ The sample solution is supplied dropwise on prism and measured after evaporating the solvent 5cm/10cm gas cell Gas cell with long pathlength

% order ppm order order R Below several handreds of m Above several hundreds of m

Transmission method Total reflectance method Infrared microscopy Total reflectance method

Micro cell Single-reflection ATR AIM-8800 ................ Applicable to transmission, reflection, and ATR methods Single-reflection ATR
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Shi m adz u A c c e s s o r y L i n e - u p

1. Options from Shimadzu


Description Attenuated Total Reflection Attachment Horizontal Type Attenuated Total Reflection Attachment ATR-8000A ATR-8000 ATR-8200HA ATR-8200H MIRacleA MIRacle MIRacleA MIRacle DuraSampllR2 (Diamond ATR) DuraScope SRM-8000A SRM-8000 RAS-8000A RAS-8000 GPR-8000 VeeMAX2A VeeMAX2 DRS-8000A DRS-8000 DRS-8010ASC RBC-8000 Type 1 Type 2 ATR-8800M Attenuated Total Reflectance Measurement Single-Reflection Horizontal Attenuated Total Reflection Attachment P/N 206-62303-91 206-62303 208-97240-91 208-97240 208-97247-95 208-97247-91 208-97247-96 208-97247-92 See page 9 208-92184 208-92207 206-62304-91 206-62304 206-62302-91 206-62302 206-61550 208-977284-91 208-97284-92 206-62301-91 206-62301 200-66750 206-62308 206-62305 206-72500-92 206-72500-96 206-70450-91 208-92171 208-92236 200-66752 208-97206 208-97202 206-62308 206-63900 206-63663-92 206-62309 206-70170-91 206-71122-91 206-73512 206-72352-91 200-64185-01 200-64185-02 206-70125-92 206-72017-91 206-62306-01 206-62306 206-62307 206-17384 200-66754-11 208-97207 208-97208 208-97209 202-32006202-32007 200-66747-91 202-32010 202-32011 202-32012 200-64175 261-79017 200-66753-11 200-93508 202-34141 202-32000202-32001202-32002See page 32 202-32024 206-72016-91 206-72015-91 208-97271-91 208-97272-91 206-72751-91 206-72760-91 206-72716-91 206-73700206-21600-92 206-73738-91 206-72330-91 206-73737-91 206-72331-91 206-72333-91 Remarks with KRS-5 prism with ZnSe prism with ZnSe prism 8 with Ge prism 9 with Diamond prism Incident Angle: 10C Incident Angle: 70 to 75 C Incident Angle: 30 to 80 C 10 12 13 14 15 17 18 19 21 22 with Ge prism 23 24 25 Page 6 7

Single-Reflection Horizontal Attenuated Total Reflection Attachment Specular Reflectance Attachment Reflection Absorption Spectrometry Attachment Grid Polarizer Variable Incident Angle Reflectance Attachment Diffuse Reflectance Attachment Diffuse Reflectance Measurement SiC Sampler Automatic Diffuse Reflectance Attachment Reflection-Type Beam Condenser Automatic Infrared Microscope AIM-8800 ATR Objective Mirror Sampling Kit Diamond Cell C Diamond Cell B Micro Magnetic Sample Holder Micro Vise Holder Automatic Sampler Diffuse Reflectance Attachment Auto Sampler for Transmission Measurement Sample Switcher 21

Reflectance Measurement

Micro Sample Measurement

Accessories for Automated Measurement

DRS-8010ASC ASC-8000T PCK-8000 PCK-8730 PCK-8940 PCK-8941 PCK-21 50Hz 60Hz

27

Purge Control Kit Purge Control Kit

28

Dry Air Supply Unit External light Beam Switching Kit MCT Kit Second Sample Compartment (with MCT detector) Second Sample Compartment MCT Detector Cassette (Sample Holder) Magnetic-Type Film Sample Holder Universal Clip Holder EZ-Clip 13 EZ-Clip 25 5cm Gas Cell 10cm Gas Cell Gas Cell Mini Hand Press Evacuable Die for KBr Pellets Micro Die for 2mm dia. KBr Pellets Micro Die for 5mm dia. KBr Pellets Hydraulic Press Vacuum Pump Magnetic-Type Pellet Holder Agate Mortar and Pestle KBr Crystal (100g) Demountable Cell Sealed Liquid Cell Fixed Thickness Cell Sample Cell for Oil Content Determination Crystal Polishing Kit Far Infrared Kit NIR Set Upload Type Diffuse Reflectance Attachment NIR Integrating Sphere Fiber Coupler Reflective Fiber Probe Heating Transmission Cell Infrared Microscope IRsolution Agent Mapping Program Macro Platform 3D Display Program PLS Quantitation Software Curvefitting (Peak split) Software

28 29

External Detector / Optional Detector

SSU-8000MCT SSU-8000 MCTD-8000

30

31

Transmission Measurement

32

33

Long Pathlength Gas Cell MHP-1

34

Pellet Measurement

SSP-10A SA18-3M

35

36

38

Cells for Liquid Samples

39 40 42

Others

UpIR A IntegratIR A

NIR Measurement

43 44 45

AIM-8800

Optional Software

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A t t enuat ed Tot al R ef l ect ance M easurement

A t t enu at ed To t al R ef lect io n M et h o d
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.

Prin cip le
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 lnfrared rays

Sample

Prism Sample

R eq u iremen t s f or M easurement s by t he ATR M et hod


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.

Pen et rat io n D ept h of IR Light


Infrared light can penetrate to a depth expressed by the next equation:

( Sa m pl e t h i c k n e s s ) where,
1

dp=

2(sin2-n212) 2

: lncident angle n21: (Refractive index of sample) / (Refractive index of prism) : Wavelength

Examp le o f Pen et rat ion D ept h


Sample refractive index of 1.5
Material Refractive index (1,000 cm-1) Incident angle 4,000 cm-1 Penetration 2,000 cm-1 depth 1,000 cm-1 400 cm-1 Material Refractive index (1,000 cm-1) Incident angle 4,000 cm-1 Penetration 2,000 cm-1 depth 1,000 cm-1 400 cm-1 ZnSe/KRS-5/Diamond 2.4 45 60 1.2m 0.7m 2.4m 1.3m 4.8m 2.7m 12.0m 6.6m Germanium 4 45 0.7m 1.3m 2.7m 6.6m

When = 45 and n21 = 0.5, therefore, 10m (1000 cm-1) dp corresponds to 3.18m and 5m dp (2000 cm-1) to 1.6m. 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. The software program for correcting for penetration depth, incorporated in the IRPrestige-21, IRAffinity-1, FTIR-8000 Series further widens the application field of the ATR method.

30 1.2m 2.4m 4.8m 12.0m

60 0.5m 1.0m 2.0m 5.1m

A ttenuated R e f l e c t a n c e Me a s u re me n t

Attenuated To t al Reflection Attachment ATR-8000A (P/N 206- 62303- 91) ATR-8000 (P/N 206- 62303)
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.

to detector

60
Prism

45 30

Optics of ATR-8000

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. 45 times reflection (with an incident angle of 45) ensures high sensitivity. Standard software includes a program to correct for penetration depth. Maximum sample size: 40mm x 15mm, 10mm thick

Standard Con t ent


Description Attenuated Total Reflection Attachment ATR prism (KRS-5) Sample holder Hex key wrench PhiIlips screwdriver Quantity 1 1 1 set 1 1

ATR-8000

Prisms
Material KRS-5 Ge Refractive Index (1000cm-1) 2.37 4.0 With holder (P/N) 206-61560-01 206-61560-02 Without holder (P/N) 200-66125-01 200-66125-02
ATR Spectrum of PET (KRS-5 prism)

Note: Prisms without a holder are recommended as supplies, while those with a holder are recommended when prisms of different materials are purchased.

45

(52) 2 (48) 50 Dimensions of Prism 20

ATR Spectrum of PET, corrected for Penetration Depth

H o rizo n t al T yp e A t t enuat ed Tot al R ef lect ion At t achment A T R - 8200H A ( P/ N 2 0 8 - 9 7 2 4 0 - 9 1 ) A T R - 8200H ( P/ N 2 0 8 - 9 7 2 4 0 )


The principle is the same as the ATR-8000. 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.
Prism

Sample

F eat u res
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.
to detector Optics of ATR-8200H

St an d ard C o n t ent
Description 1 Horizontal Type Attenuated Total Reflection Attachment 2 ZnSe prism for solid samples, 45 incident angle 3 ZnSe prism for liquid samples, 45 incident angle 4 Gripper (P/N 208-97240-25) Quantity 1 1 1 1
ATR-8200H

The prism for liquid samples is fixed in the groove, as shown in the figure, so that liquid, powder, or gel samples may be easily measured. The dent to accept a sample is accessible from above to ensure ease when replacing samples and cleaning the prism.
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 Oil

The prism for solid samples permits easy measurement of film type and other solid samples, the operation being the same as that for the ATR-8000. A plate is fixed with screws to put the sample in close contact with the prism surface, which ensures high reliability of the spectra.
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.

FTIR Spectrum of PVDC Sheet

Prisms
Description 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 P/N 208-97240-03 208-97240-01 208-97240-13 208-97240-10

A ttenuated To t a l R e f l e c t a n c e M e a s u re me n t

Single-Ref lect ion Horizontal Attenuated Total Reflect io n Attachment MIRacleA ZnSe prism model (P/N 208-97247-95) MIRacle ZnSe prism model (P/N 208-97247-91) MIRacleA Ge prism model (P/N 208-97247-96) MIRacle Ge prism model (P/N 208-97247-92)
MIRacle is a single-reflection horizontal attenuated total reflection attachment which uses a 2 mm prism in diameter. Since the prism is placed horizontally, solid samples, such as plastics, fibers, films and powders, and liquid samples can be measured. QuickStart MIRacleA includes the automatic accessory recognition function.

Trough Insert Prism

to detector Thumb screw Optics of MIRacle

Features
Since the small prism is mounted, small solid samples and a bit of a liquid sample can be measured. The ZnSe prism can measure the wavenumber range from 5000 cm-1 to 650 cm-1. The Ge prism can measure the wavenumber range from 5000 cm-1 to 700 cm-1 and can be used for the measurement of high refractive index samples such as black rubber samples.

Standard Con t ent


Description Single-Reflection Horizontal Attenuated Total Reflection Attachment Single-Reflection HATR UniversaI plate (Selected prism, ZnSe prism or Ge prism) Pressure clamp Trough Insert Quantity 1 1 1 1
MIRacle

Prisms
Description Single-Reflection HATR Universal Plate, ZnSe prism Single-Reflection HATR Universal Plate, Ge prism P/N 208-97247-93 208-97247-94
ZnSe Prism Plate

Spectrum of EVA (Ethylene Vinyl Acetate) pellet

D u raSamp lIR2 ( D iamond A TR )


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 650 cm-1 for ZnSe and 400 cm-1 for KRS-5. The pressure sensor cannot be added later. If it will be needed, please include it when purchasing the system.
Metal Plate Diamond Prism

Infrared Light

ZnSe or KRS-5 Support Element

DuraSamplIR2 Optics

D u raSamp lIR2 Part N ames and P/N


Description DuraSamplIR2A System I (ZnSe support element) DuraSamplIR2A System I (ZnSe support element, with pressure sensor) DuraSamplIR2A System I (KRS-5 support element) DuraSamplIR2A System I (KRS-5 support element, with pressure sensor) DuraSamplIR2A System H (ZnSe support element) DuraSamplIR2A System H (KRS-5 support element) Description DuraSamplIR2 System I (ZnSe support element) DuraSamplIR2 System I (ZnSe support element, with pressure sensor) DuraSamplIR2 System I (KRS-5 support element) DuraSamplIR2 System I (KRS-5 support element, with pressure sensor) DuraSamplIR2 System H (ZnSe support element) DuraSamplIR2 System H (KRS-5 support element) P/N 208-92143-11 208-92144-11 208-92143-12 208-92144-12 208-92145-11 208-92145-12
Exterior of System I (High-Pressure Device Type)

The systems above include an automatic accessory detection feature.

P/N 208-92143-01 208-92144-01 208-92143-02 208-92144-02


Exterior of System I (with pressure sensor)

208-92145-01 208-92145-02

Op t io n al an d St andard Part s
Description DuraDisk (ZnSe support element) DuraDisk (KRS-5 support element) DuraDisk (Ge/Ge) P/N 208-92147 208-92148 208-92238

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.

Exterior of System H (ViewIR Type)

Attenuat ed To t a l R e f l e c t a n c e M e a s u re me n t

DuraScope

(P/N 208- 92184)


Video Monitor

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.

Description DuraScope (ZnSe support element)


DuraScope (KRS-5 support element)

P/N 208-92184 208-92207

DuraScope

Options for Du raSampllR II and D uraS cope


Description DuraDisk (ZnSe support element) DuraDisk (KRS-5 support element) DuraDisk (Ge/Ge) P/N 208-92144 208-92148 208-92238

The DuraDisk is the section where the diamond prism and the support element are joined together. A DuraDisk for the Ge prism for measuring high refractive index samples also is available. DuraDisks can be replaced by the customer.

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R ef l ect ance M easur em ent

Sp ecu lar R ef lect an ce M et h o d


FTIR measurement by the specular reflectance method provides three types of information shown below: 1 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 Metal substratum example of this method.
Thin film

2 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.
Sample

IR rays

IR rays

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. Metal substratum The measurement of a epitaxiaI layer of a semi-conductor Thin film sample is a typical application of this IR rays method.

1.R ef lect io n A b sorpt ion Spect roscopy


The Reflection Absorption Spectroscopy (RAS) method permits highsensitivity 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.

Vertical polarization Metal plate

Parallel polarization Metal plate

1. 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. 2. 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.

Reflection of Light on MetaI Substratum

2.C o n versio n o f R ef lect ion Spect ra int o Absorpt ion Spect ra


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 is sufficiently small, each element of the complex refractive index of a material may be expressed as: 1-R (1) n= Reflectance value 1+R-2Rcos Absorption coefficient k= -2Rsin 1+R-2Rcos (2) where, R: Reflectance value : phase shift when the light is reflected. The for the wavenumber vg may be calculated from the following Kramers-Kronig equation: (g)= 2g 0

InR() d 2g2

(3)

The can be obtained from the reflectance value R, and substituting that in the equation (2) gives the absorption coefficient k. Performing this calculation for all the wavenumbers will give the absorption spectrum.

Examp les o f A p plicat ions


Since a reflection spectrum can be converted into the absorption spectrum through Kramers-Kronig analysis, 1Absorption 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. 2Kramers-Kronig analysis method is especially effective for infrared microscopy, where it is virtually impossible to slice the sample.

11

R efl ectan ce M e a s u r e m e nt

Specular Ref lectance Attachment SRM-8000A (P/N 206- 62304- 91) SRM-8000 (P/N 206- 62304)
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.

Sample

to detector

Optics of SRM-8000

Features
Easy sample setting. Kramers-Kronig conversion software provides IR spectra without sample preparation. Description Specular reflectance attachment Standard mirror, 30 x 30 mm Sample mask, 15 mm dia. Hex key wrench Phillips screwdriver P/N 200-66123 206-18752-02 Quantity 1 1 1 1 1

SRM-8000

Specular Reflectance Spectrum of the Inner Wall of Aluminum Can

Specular Reflectance Spectrum of PMMA after Kramers-Kronig Conversion

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R ef lect io n A b sorpt ion Spect romet ry A t t ach men t R A S- 8000A ( P/N 2 0 6 - 6 2 3 0 2 - 9 1 ) R A S- 8000 ( P/N 2 0 6 - 6 2 3 0 2 )
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 , 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 (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 (P/N 206-61550) 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

Stationary wave

Reflected light Vertical polarization Parallel polarization

Principle of Reflection Absorption Spectrometry

Sample 20

Light shield plate

Mask (at wedge) Optics of RAS-8000

F eat u res
Easy sample setting. The incident angle is selectable between 70 and 75.

St an d ard C o n t ent
Description Reflection absorption spectrometry attachment Standard mirror Sample mask, 8 mm dia. Sample mask, 15 mm dia. Sample mask, 25 mm dia. Light beam mask, 3 x 3 mm Light beam mask, 5 x 5 mm Light shielding plate* Hex key wrench PhiIIips screwdriver P/N 200-66123 206-18752-01 206-18752-02 206-18752-03 206-18608-01 206-18608-02 Quantity 1 1 1 1 1 1 1 1 1 1

RAS-8000

* Attaching the light shielding plate raises the mean incident angle of the light beam from 70 to 75.

Relationship Between Spectrum of Fluorine Film on Hard Disk, Peak Area and Film Thickness (calibration curve)

13

R efl ectan ce M e a s u r e m e nt

Grid Polarizer GPR-8000 (P/N

206- 61550)

A grid is precisely produced on the substrate by the photographic technique. The grid polarizer enhances the sensitivity of the RAS8000 Reflection Absorption Spectroscopy Attachment. Degree of polarization: 99% (at 10 m), 95% (at 3 m) Quenching ratio: 148: 1 (at 10 m), 23:1 (at 3 m) Effective area: 25 mm dia. Angle scale: 360, 10 increments Material of substrate: KRS-5, 2 mm thick Measurement wavelength range: 5,000 to 350 cm-1

Note 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

14

Variab le In cid ent A ngle R ef lect ance A t t ach men t VeeM A X 2 A ( P/ N 2 0 8 - 9 7 7 2 8 4 - 9 1 ) VeeM A X 2 ( P/ N 2 0 8 - 9 7 2 8 4 - 9 2 )
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.

F eat u res
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 2 and Optional Polarizer

M easu rab le 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

St an d ard C o n t ent
Description VeeMAX 2 Sample mask set Gold-coated mirror P/N 208-97284-11 208-97271-13 Quantity 1 1 1
VeeMAX 2 Optical System

Op t io n s
Description 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 P/N 208-97284-21 208-97284-24 208-97284-14 208-97300-12 208-97300-28

Syst em C o mb in at ions
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

15

D i ffuse Ref l e c t a n c e M e a s u r e me n t

D i ffu s e R e f l ec tan ce S p ec tros c opy


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. 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= (1-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. The FTIR-8000 Series / IRPrestige-21 incorporates the Kubelka-Munk conversion function as a standard feature.

Incident light

Diffuse reflected light

Specularly reflected light

Reflection Within Powder Sample

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.
HPLC fraction Remove mobile phase through evaporation Diffuse reflectance attachment

KBr powder FTIR FTIR Analysis of HPLC Fractions

16

Interferometer

Detector

D if f u se R ef lect ance A t t achment D R S- 8000A ( P/N 2 0 6 - 6 2 3 0 1 - 9 1 ) D R S- 8000 ( P/N 2 0 6 - 6 2 3 0 1 )


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 KubelkaMunk 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.

Sample

to detector

F eat u res
The small measuring light beam (1.8 x 1.8mm) 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.

Optics of DRS-8000

St an d ard C o n t ent
Description 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 P/N Quantity 1 1 1 1 1 1 1 1 1

DRS-8000

206-61184-01 206-61184-02

* Holder for disposable sample cup. Disposable sample cups are available as extra.

Op t io n s
Description Sample cup, 50 pieces per set, aluminum, 6 dia. x 1.5 deep (mm) Sample die for aluminum cup SiC sampler P/N 201-52943 206-63950 200-66750
Diffuse Reflectance Spectrum of Lactose

Diffuse Reflectance Spectrum of Lactose After Kubelka-Munk Conversion

17

D i ffuse Ref l e c t a n c e M e a s u r e me n t

SiC Sampler

(P/ N 200- 66750)

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 DRS8000. (The SiC has a hardness of 9.0 and is quite chemically stable.) New emery paper is used as reference.

Sample holder that can be directly installed to the DRS-8000

Sticker type SiC emery paper

Standard Con t ent


Description Holding rod Sample holder SiC emery paper (#320) SiC emery paper (#400) P/N 208-92176 Quantity 1 2 100 sheets 100 sheets
Solid sample

Supplies
Description SiC emery paper (#320), 100 sheets SiC emery paper (#400), 100 sheets P/N 200-66751-01 200-66751-02

Construction of SiC Sample

SiC Sampler

Diffuse Reflectance Spectrum of Plastic Products Obtained with SiC Sampler

18

A u t o mat ic D if f use R ef lect ance A t t achment D R S- 8010A SC ( P/ N 2 0 6 - 6 2 3 0 8 )


Having the same optics as the DRS-8000, the DRS-8010ASC accepts 24 samples to permit automated measurement.

F eat u res
One-touch connection to the FTIR Series, which has the control capability as standard. With no external control unit required, the DRS-8010ASC is very compact. Controlled by the auto program incorporated as standard in the FTIR Series. The program is user-definable. 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.
Sample

to detector

N o t es
When this attachment is used on IRAffinity-1, the ASC cable (P/N 206-73433-91) is required. The BASIC software is required separately for the HYPER-IR model.

Optical Diagram of DRS-8010ASC

St an d ard C o n t ent
Description Automatic diffuse reflectance attachment Sample holder, 24-sample type Standard mirror Sample cup Die Tweezers Sample handling rod Hex key wrench Phillips screwdriver Quantity 1 2 1 set 200 1 1 pair 1 1 1

DRS-8010ASC

Su p p lies
Description Sample holder, 24-sample type Sample cup, aluminum, 6 dia. x 1.5 deep (mm) P/N 206-65234 201-52943

F o r co n n ect io n wit h FTIR main body, a cab le is req u ired.


Description Cable for IRPrestige-21, IRAffinity-1 Cable for FTIR-8400S P/N 206-73433-91 208-94914-02

Sample stage

19

M i cro S a m p l e M e a s u r e m e n t

M e a s u re me n t o f Micro S ample s
FTIR ensures such a high sensitivity as to permit reliable measurement of micro samples. There are two popular devices to measure micro samples: 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: Reflection-type beam condenser Transmission only Not possible About 200 m Detector of the FTIR lR microscope Transmission/reflection/ATR Selection by aperture after observation in visual mode About 10m Dedicated MCT detector (Measurement wavenumber range is limited by the MCT detector.) External installation

Measurement mode Selection of the part to be measured Minimum measurable size Detector

Installation

Sample compartment of the FTIR

Transmissio n 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 m 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.
IR light from interferometer to detector Aperture

MCT detector

Reflecting objective Autome sample Condenser mirror Entrance for IR beam from the FTIR main

X-Y-Z stage

Sample

Beam Condenser

Infrared Microscope (Transmission mode)

Reflection mo d e
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.
Infrared Microscope (Reflection mode)

ATR mode m icroscopy


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

Schwarzchild reflecting objective mirrors.

ATR (Ge) prism Sample

20

R ef lect io n - T yp e B eam C ondenser R B C - 8000 ( P/N 2 0 6 - 6 2 3 0 5 )


This beam condenser is especially useful for transmittance measurement of micro samples.

F eat u res
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 L of liquid samples. The light beam is reduced to 1/5 (about 1.8 x 1.8mm).

St an d ard C o n t ent
Description RBC-8000 reflection-type beam condenser Sample holder, with X-Y-Z stage Pellet sample holder Hex key wrench Phillips screwdriver Quantity 1 1 1 1 1

W-Y-Z stage

Sample

Optical Diagram of RBC-8000

RBC-8000

21

M i cro S a m p l e M e a s u r e m e n t

300

Automatic Inf rared Microscope AIM-8800 Type 1 (P/N 206-72500-92 for 120V, -93 for 220V, -94 for 240V, -34 for CE, 230V) Type 2 (P/N 206-72500-96 for 120V, -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-8100.)

450

340 PC

Printer CRT 340 150 Key Board 450 948 mm Relative Positioning of IRAffinity-1 and Microscope Monitor 700 IRAffinity-1 Infrared Microscope System Spectrum of Adhesive on Metal

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 10 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.

Specificatio n s
Optics MCT detector (Glass dewar type) Signal-to-noise ratio 15 x Cassegrain objective 15 x Cassegrain condenser mirrors Wavelength range : Type 1 : 5000-720cm-1 Type 2 : 5000-650cm-1 60 repeat scans 2600: 1 or higher (Type 1), 2000: 1 or higher (Type 2) Electrically activated aperture XY directional drive. Setting of XY direction increments is 1 m over Sample surface, and 1 increments in direction (numerical entry possible). Minimum setting value : 3 m Motor-driven X-Y sample stage Positioning range : X axis : 70mm; Y axis : 30mm Resolution. 1 m pitch Sample thickness : Reflection mode : < 40mm = Transmission mode : < 10mm = Microscope keyboard Operation PC control 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 (10 sample positions, 2 background positions)
Wavelength range (near-infrared) (Note 1) 10,000 to 3,800 cm-1 With liquid nitrogen monitoring system

Transmission mode, aperture size 50 m, 8cm-1

Adhesive on Metal (measurement of part enclosed in blue in photo on right)

(Note 1) Near-infrared measurement is possible only when the NIR Set is mounted on IRPrestige-21. Remarks: 1) When connecting to a PC-type FTIR-8000 Series, IRAffinity-1 and IRPrestige-21, the PC for operating the FTIR main unit is also used for operating the AIM-8800. When connecting to a non-PC-type FTIR-8000 Series, the PC must be purchased separately. 2) Contact us for details on parts required for connecting the FTIR to the AIM-8800.

22

A T R Ob ject ive M irror A T R - 8800M ( P/N 2 0 6 - 7 0 4 5 0 - 9 1 )


A semicircular prism made of ZnSe is used. x 15 magnification; 30 incident angle, and single reflection. The prism is a slide type and permits switching between visual observation mode and IR measurement mode.

F eat u res
Small prism enables focusing and measurement of even small samples. Measurement range of 5,000 to 700 cm -1

M ain t en an ce Part s
Description Replacement Ge prism P/N 206-70451-91

Ot h er Op t io n al f or M icroscope
Description Aluminum reference mirror KBr window plate CaF2 window plate Visible light objective lens (x10) Visible light objective lens (x20) Infrared polarizer (Infrared polarizer and holder are required.) Visible light polarizer Remarks P/N 13 mm dia. 206-90104 13 mm dia. x 2 mm thick 200-66752-04 13 mm dia. x 2 mm thick 200-66752-02 Manufactured by 208-92180-01 Kyowa Optical Co., Ltd. 208-92180-02 Infrared polarizer holder 206-81524 208-92014 Infrared polarizer (STJ-1001) Please contact us for details.

ATR-8800M ATR Objective Mirror

Spectrum of Adhesive on Fiber

Samp lin g K it

( P/ N 2 0 8 - 9 2 1 7 1 )

This kit is for pretreating samples for microscope measurement. It comprises a set of tweezers, roller knife, needles, scissors, replacement blades and replacement needles.

St an d ard C o n t ent
Description 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 Quantity 1 1 1 1 1 1 1 1 1 1

Sampling Kit

23

M i cro S a m p l e M e a s u r e m e n t

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.
Notes Diamonds exhibit slight absorption in the range 3,000 to 1,500 cm-1. Diamonds are hard but brittle and may crack depending on the sample and method of use.

Diamond Cell C

Diamond Cell C

( P/ N 208- 92236) 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 (1.6 mm). Although its strength is slightly inferior to the natural diamond, it is adequate for compressing nearly all samples. Large-size diamond provides 1.6mm diameter window Large diameter window allows measurement even when placed in standard sample compartment Measurement possible by merely placing on infrared microscope stage

Features

Standard Con t ent


Description C plate C screws Holder with diamond window for C Case Hex key wrench Quantity 1 3 2 1 1

Spectrum of Single Fiber Red: Diamond cell used Black: Diamond cell not used

Options and Maintenance Part s


Description C plate C screws (pack of 3) Holder with diamond window for C P/N 208-92172-01 208-92172-02 208-92236-01

Diamond Cell B

( P/ N 200- 66752) 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 Con t ent


Description Diamond cell Holder with compression cap O ring Quantity 1 pair 1 1 set

Options and Supplies


Description Diamond cell for spare CaF2 window, a pair KBr window, a pair P/N 200-66752-01 200-66752-02 200-66752-04

24

M icro M ag n et ic Sample H older


( P/N 2 0 8 - 9 7 2 0 6 ) This is exclusively used for IR microscopy. This holder allows samples to be held by a magnetic cover and loaded by one-touch operation without being dirtied. Samples are held between magnet sheets and placed on the microscope's stage. The sample slide is made of stainless steel, and has three holes, 5 mm dia., 13 mm dia. x 1 mm and 13 mm dia. x 2 mm. Samples of thickness up to 0.5 mm can be held.

Sample slide, made of stainless steel Silver mirror Same reflectivity as gold and harder than gold or aluminm. Magnetic cover with micro scale (10 m square) Convenient for measurement and positioning of samples Magnetic covers 13mm dia. and 5mm dia. are available for selective use

F eat u res
Fiber samples are easily loaded. Applicable to both reflection and transmission measurement modes. Provided with a micro scale (10 m square grid).

St an d ard C o n t ent
Description Stainless steel sample slide Magnetic cover (5 mm dia. hole) Magnetic cover (13 mm dia. hole) Magnetic cover (with micro 10 m scale) Quantity 1 1 1 1
Hole, 13mm dia. and 2mm thick Used for refelctometry or to accept a diamond window Hole, 13mm dia. and 1mm thick Hole, 5mm dia. Used for measurement of small samples Slit for fiber sample Used for measurement of monofilament samples, for example

M icro Vise H o lder

( P/ N 2 0 8 - 9 7 2 0 2 ) 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 o f H o ld ab le Samples
Within approx. width of 20 mm Film of length 14 to 54 mm (excluding grip allowance) Gripped load Max. approx. length 40 mm Approx. width 40 mm
Micro Vise Holder

Tensile load

St an d ard C o n t ent
Description Micro vise holder Holding fixture Quantity 1 2

25

A ccesso r i es fo r Au t o m a te d M e a s u re me n t

Auto ma t i n g t h e Op era tio n


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.

Automatin g t h e 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.

ASC Connector

Operation b y 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-21, IRAffinity-1 and FTIR-8400S (IRsolution model) can be controlled from the IRsolution software.

26

A u t o mat ic D if f use R ef lect ance A t t achment D R S- 8010A SC ( P/ N 2 0 6 - 6 2 3 0 8 )


This attachment automates measurement of up to 24 samples. For details, refer to page 19.

N o t es
When this attachment is used on IRAffinity-1, the ASC cable (P/N 206-73433-91) is required. The BASIC software is required separately for the HYPER-IR model.

A u t o Samp ler f or Transmission M easurement A SC - 8000T ( P/N 2 0 6 - 6 3 9 0 0 )


This attachment accepts up to 18 samples for measurement in the transmission mode.

F eat u res
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 13 mm dia. pellet is provided. Use of the window-plate option enables measurement in the Nujol method.
DRS-8010ASC

N o t es
When this attachment is used on IRAffinity-1, the ASC cable (P/N 206-73433-91) is required. The BASIC software is required separately for the HYPER-IR model.

St an d ard C o n t ent
Description ASC-8000T main Pellet holder Fixing spring Tweezers P/N 206-63917 206-63951-01 Quantity 1 20 20 1 pair P/N 206-66699 206-81522

Op t io n s
Description KRS-Window set (with a set of window holder) Film holder (9 pcs. as a set)
ASC-8000T

F o r co n n ect io n wit h FTIR main body, a cab le is req u ired.


Description Cable for IRAffinity-1 P/N 206-73433-91 ( P/ N 2 0 6 - 6 3 6 6 3 - 9 2 )

Samp le Swit ch er 21

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.

F eat u res
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-1, IRPrestige-21).

A ccesso ries T h at C an B e U sed


Evacuable die for KBr pellets Sealed liquid cell Magnetic pellet holder Diamond cell 5 cm gas cell Sample holder for MHP-1 Mini Hand Press Fixed thickness cell Magnetic film holder 10 cm gas cell

Sample Switcher 21

A ccesso ries T h at C annot B e U sed N o t es


When this attachment is used on IRAffinity-1, the ASC cable (P/N 206-73433-91) is required. The BASIC software is required separately for the HYPER-IR model.

For connection with FTIR m ain body, a cable is requir ed.


Description Cable for IRAffinity-1 P/N 206-73433-91

27

Purg e Con t ro l K i t

Purge Cont rol Kit PCK-8000 (P/N 206- 62309) for FTIR-8100/8200/8600 Series PCK-8730 (P/N 206- 70170- 91) for FTIR-8300/8700 Series PCK-8940 (P/N 206- 71122- 91) for FTIR-8400/8400S/8900 Series PCK-8941 (P/N 206- 73512- 91) for IRAffinity-1, FTIR-8400/8400S/8900 Series PCK-21 (P /N 206-72352- 91) for IRPrestige-21
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 (10 m, 7 mm I.D., 10 mm O.D.) Exhaust parts
PCK-8730

Notes
The purge control kit cannot be used with the DBX-8000. Ventilate the site when purging with nitrogen gas.

Dry Air Su p p ly Unit


(P/N 2 00 -64 185-01 for 50 Hz l i ne, 100 VA C ) (P/N 2 00 -64 185-02 for 60 Hz l i ne, 100 VA C ) 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 soundproofing materials.

Note
Dimensions: 400W x 610D x 610H mm Dry air supply capacity: 10 to 20L / min. Dry air: -17C or lower in dew point.

28

Ext er nal D et ect or / O pt i onal D et ect or

Ext ern al D et ect or / Opt ional D et ect or


A DLATGS detector or LiTaO3 detector is mounted as standard on the IRPrestige-21, IRAffinity-1 and FTIR-8000 Series. Some applications require use of a high-sensitivity MCT detector or external installation of a special optical system.

Required Par ts
When Using the MCT Detector MCT Kit Second sample compartment When Using an External Optical System1 External Light Beam Switching Kit External Light Beam Switching Kit Second sample compartment External Light Flux Extraction Kit

IRPrestige-21 IRAffinity-1 FTIR-8000 Series 1)

1) Cannot be used on the FTIR-8100/8200/8500/8600.

Ext ern al L ig h t B eam Swit ch in g K it ( P/ N 2 0 6 - 7 0 1 2 5 - 9 2 )


This kit extracts infrared light from the right side of the IRPrestige-21, IRAffinity-1 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 m 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-1 and IRPrestige-21.

St an d ard C o n t ent
Description Switching mirror (with polystyrene film) External input signal connector Quantity 1 1set

Exterior and Content of External Light Beam Switching Kit

N o t es
Traceability is not provided for the polystyrene film. This kit cannot be used on the FTIR-8100/8100M/8100A/8200/8200D/8200A/8500/8600 and FTIR-8200PC/8600PC.

M C T K it

( P/N 2 0 6 - 7 2 0 1 7 - 9 1 )

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 the IRPrestige21 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.

Specif icat ions


Detector Liquid nitrogen cooled MCT detector With glass dewar (approx. 300 ml) With liquid nitrogen monitor 4,600 to 650 cm-1 8 hours (when liquid nitrogen is newly purchased)

Wavelength range Liquid nitrogen retention time

Not es
This kit cannot be mounted at the same time as the NIR set (P/N 206-72015-91). Liquid nitrogen is required when using the MCT detector.

29

Exter nal D et e c t o r / O p t i o na l De t e c t o r

Second Sample Compartment (with MCT detector) SSU-8000M CT ( P/ N 206- 62306- 01) (Not applicable to FTIR-8101)
If a gas cell, a flow cell, a thermovac evaporation type diffuse reflectance attachment, or another attachment that is to be installed externally is mounted to, and removed from, the standard sample compartment, high analytical productivity cannot be expected. The second sample compartment is used to accept such an attachment, so that measurement can be made by only switching the light beam. This method dramatically enhances analytical productivity. Also, the second sample compartment is designed to accept a customer-developed attachment.

305 Parallel beem, 40mm dia. 326

584

145

192

460 622

30

214 552

297

Features
The base plate of the FTIR main body is removed and the SSU8000MCT is installed in that place. The front panel and the top lid may be separately opened. The front panel may be removed by one-touch operation. A part (an acrylic resin plate) of the top lid may be removed. Equipped with piping for purge gas (dry air or nitrogen). For the type that accepts both the second compartment and the infrared microscope, please contact us or your local distributor. The MCT-8000 detector (supplied as standard) provides extremely high sensitivity and covers a wavenumber region of 4600 cm-1 to 750 cm-1. The glass dewar type MCT detector requires no reevacuation. The liquid nitrogen monitoring system protects the MCT elements.

247 mm Dimensions of FTIR-8000 Series and SSU-8000


2-6 x 8 hole depth 5 Window (removable) 6 dia. x 8 H hole depth 5 Chassis base plate (not removable) M6 depth 5 M4 depth 5

Second Sample Compartment SSU-8000 (P/N 206-62306)


A second sample compartment without MCT detector.

MCT Detector MCTD-8000 (P/N

206-62307)

(Window)

A set of a second sample compartment, an MCT detector, a preamplifier, and a condenser mirror.
(Window)

Focus position M5 depth 5

2-6 mm dia. pin length 3 Base fastening screw (3 places) Handle Front cover (removable)

Second Sample Compartment (SSU-8000) External Dimensions and Base Plate Dimensions

30

408

Tr ansm i ssi on M easur em ent

A ccesso ries f o r Transmission M easurement


Film samples can be measured easily if they are attached to the standard cassette or optional film holder.

C asset t e ( Samp le H older)

( P/ N 2 0 6 - 1 7 3 8 4 )

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 10 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-8100/8100M/8100A/ 8200/8200D/8200A/8500/8600 and FTIR-8200PC/8600PC.

F eat u res
Little clearance Rigid

St an d ard C o n t ent
Description Cassette ASSY Quantity 1

M ain t en an ce Part s
Description Cassette mounting screws P/N 037-02820-18

M ag n et ic- T yp e Film Sample H older


( P/N 2 0 0 - 6 6 7 5 4 - 1 1 ) Film samples are held between the stainless backplate (SUS 430) and rubber magnet for direct analysis.

St an d ard C o n t ent
Description Backplate (SUS430) Magnet sheet without hole Magnet sheet with 13 mm dia. hole Magnet sheet with 7 x 13 mm hole Magnet sheet with 7 x 19 mm hole Magnet sheet with 10 x 23 mm hole Quantity 1 1 1 1 1 1

Dimensions of Magnetic-Type Film

31

Tr ansm i s si o n M e a s u r e me n t

Universal Clip Holder

( P/ N 208- 97 207)
Pressure nut Silicone rubber o-ring

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.

Features
Applicable sample sizes range from 13 to 40 mm in diameter, and up to 13 mm thick. The pressure nut ensures easy measurement of mull samples. The rubber magnet and o-ring are used for positive holding of samples.
Slide stopper Clip

O rings for spare

Standard Con t ent


Description Universal clip holder Magnet base, 22 mm dia. Magnet base, 10 x 14 mm hole Spare O-ring Quantity 1 1 1 1

Two types of magnet base, 22mm and 10mm

EZ-Clip13

(P/N 208- 97208)

This one-touch sample holder uses a clip exclusive for 13 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 13 mm) also can be held. Diameter of light passage hole: 10 mm

Standard Con t ent


Description EZ-Clip13 Quantity 1
Universal Clip Holder

EZ-Clip25

(P/N 208- 97209)

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 13 mm) also can be held. Diameter of light passage hole: 10 mm

Standard Con t ent


Description EZ-Clip25 Quantity 1
EZ-Clip13 EZ-Clip25

32

Tr ansm i ssi on M easur em ent

Gas C ell
Gas cells are used when measuring gas samples. Select the optical pathlength to suit the concentration of the component.

Sh o rt Pat h len g t h Gas C ells 5 cm Gas C ell ( P/ N 2 0 2 - 3 2 0 0 6 10 cm Gas C ell ( P/ N 2 0 2 - 3 2 0 0 7 -

) )

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 10 cm gas cells are 42mL and 98mL, respectively. The last two digits of the catalog numbers show the material of the window plate, as listed below.

C ell W in d o w Plat es
Type of Window Plate Last two digits of P/N NaCl -10 KBr -20 KRS-5 -30

Spectrum of HCl Gas

L o n g Pat h len g t h Gas C ell


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

Sample inlet / outlet pipe Window Optics of Long Path Cell

33

Pel l et Me asu r e m e n t

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 13 mm dia. pellets, the evacuable die for KBr pellets, hydraulic press and vacuum pump are used.

Mini Hand Press MHP-1 (P/N 200-66747-91)


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 Co n t ent
1 2 3 4 5 6 Description Mini Hand Press Pellet holder Upper and lower cylinder Briquetting frame, 4 mm dia. Pellet remover Pellet remover base P/N 200-66747-01 202-35258 206-73717-91 200-66747-03 200-66747-04 Quantity 1 1 1 set 10 1 1

* Parts other than Mini Hand Press 1 are provided as maintenance parts. 2, 5 and 6 are shared for 4 and 3 mm dia. parts.

Options and M aintenance Parts


Description 4 mm dia. briquetting frame, 20 pieces 3 mm dia. briquetting frame, 10 pieces Upper/lower cylinder set 3 mm dia. briquetting frame, 20 pieces P/N 206-73718-91 200-66748 200-66749-01

Supplies
Description 10 briquetting frames, 3 mm dia., and upper and lower cylinders P/N 200-66748

Evacuable Die for KBr Pellets

(P/N 202-32010) Used to prepare KBr pellets, 13 mm dia. The amount of KBr crystal necessary for one pellet is about 200 mg and the sample 1 to 2 mg.

4 8 9 !0 !1 3 2

Standard Co n t ent
1 2 3 4 5 6 7 8 9 !0 !1 !2 Description Base Barrel Spring Plunger Mandrel Die frame Pellet holder Punching rod Punching base Plug Sieve Exhaust port P/N 202-35247 202-35251 202-35252 204-21049 202-35248* 202-35250* 202-35258* 202-35256 202-35255 202-35257 202-35261 202-35254 Quantity 1 1 1 1 2 4 4 1 1 1 1 1

7 6 5

* Packet of one when ordering by this P/N.

The following items are recommended for producing pellets of high transmittance: Quantity Description 1 SSP-10A Hydraulic Press 1 SA18-3M Vacuum Pump 100g KBr Crystal 1 each Agate Mortar and Pestle 1 Micro spatula

34

M icro D ie f o r 2 mm dia. K B r Pellet s


( P/ N 2 0 2 - 3 2 0 1 1 )

M icro D ie f o r 5 mm dia. K B r Pellet s


( P/ N 2 0 2 - 3 2 0 1 2 ) Used in combination with the KBr die (P/N 202-32010), which is for 13 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 1

St an d ard C o n t ent
Description 1 Mandrel for 2mm dia. pellets Mandrel for 5 mm dia. pellets 2 Die frame for 2 mm dia. pellets Die frame for 5 mm dia. pellets 3 Tool 4 Pellet holder P/N 202-35262 202-35264 202-35263 202-35265 202-35266 202-35258 Quantity 2 4 2 4 3 2

H yd rau lic Press SSP- 10A ( P/N 2 0 0 - 6 4 1 7 5 )


Used for producing KBr pellets. The maximum pressure is 10 tf/cm2. A high-precision pressure gauge is provided.

Vacu u m Pu mp SA 18- 3M ( P/N

261-79017)

This is a compact rotary vacuum pump, having a displacement capacity of 10 to 30 L/min., used for vacuum dehydration in production of KBr pellets. (100 VAC power is required.)

35

Pel l et Me asu r e m e n t

Magnetic-T yp e Pellet Holder


(P/N 2 00 -66 753-11) 13 mm diameter pellets are held between the stainless backplate (SUS430) and rubber magnet for direct analysis.

Agate Mortar and Pestle

(P/N 200-93508) Used to prepare KBr pellets or samples for diffuse reflectance method.

KBr Crystal (100 g)

(P/N 202-34141)

Used to prepare KBr pellets. Features a long storage life, thanks to its low hygroscopicity.

36

C el l s for Li qui d S am pl es

M easu r em en t U sin g D em o u n t able C ells


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: n= M 2n -sin2(1-2)
2

where 1 and 2 are the wavelengths of peaks or valleys, M is the degree of interference (number of the waves) between 1 and 2. When the refractive index (n) of the film is known and is uniform between the 1 and 2, 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 = 1 and = 0.

37

C el l s for L i q u i d S a m p l e s

Demountable Cell

( P/ N 202- 32000) 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.

P/N Type

202-32000-10 NaCl Demountable Cell A pair of NaCl plates (201-97942)

202-32000-20 KBr Demountable Cell A pair of KBr plates (201-97977)

202-32000-30 KRS-5 Demountable Cell A pair of KRS-5 plates (201-97943) 10 sheets 10 sheets

Contents

Metal holder (201-77662) 0.05 mm lead spacer (204-04900-14) ( P/ N 202- 32001)

1set 0.025 mm lead spacer (204-04900-13) 10sheets 0.1 mm lead spacer (204-04900-15)

Sealed Liq u id Cell

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.

P/N Type

202-32001-10 NaCI Sealed Liquid Cell A pair of NaCl plates, with and without hole (201-77160-10) Metal holder (201-77661) Gasket (202-35425) Lead cushion (202-35426) Rubber cushion (202-35427) Teflon stopper (201-75546) Syringe (200-34835) 1 2 2 2 2 1

202-32001-20 KBr Sealed Liquid Cell A pair of KBr plates, with and without hole (201-77160-20) set. pcs. pcs. pcs. pcs. pc.

202-32001-30 KRS-5 Sealed Liquid Cell A pair of KRS-5 plates, with and without hole (201-77160-30) 4 sheets 4 sheets 4 sheets 4 sheets

Contents

0.025 mm lead spacer (204-04901-13) 0.05 mm lead spacer (204-04901-14) (204-04901-34) for KRS-5 0.1 mm lead spacer (204-04901-15) (204-04901-35) for KRS-5 0.5 mm lead spacer (204-04901-18) (204-04901-38) for KRS-5

Fixed Thickn ess Cell

( P/ N 202- 32002) 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, 0.1 mm in thickness, KBr window plate, is 202-32002-25 NaCl -13 -14 -15 -16 -18 -19 -11 -12 KBr -23 -24 -25 -26 -28 -29 -21 -22 KRS-5 Not available -34 -35 -36 -38 -39 -31 -32

Cell Windo w an d Thickness


Thickness 0.025 mm 0.05 mm 0.1 mm 0.2 mm 0.5 mm 1.0 mm 2.0 mm 5.0 mm

38

Samp le C ell f o r Oil C ont ent D et erminat ion


This cell is used to quantitatively determine the concentration of oils extracted into carbon tetrachloride.

Type of cell 100 mm quartz cell (P/N 200-34473-02) 50 mm quartz cell (P/N 200-34473-01) 10 mm quartz cell (P/N 201-98716)

KRS-5 Oil content cell holder Type 1 (P/N 202-39897) Square cell holder (P/N 204-51216)

C ryst al Po lish ing K it

( P/ N 2 0 2 - 3 2 0 2 4 ) This kit is used for polishing an NaCl and KBr window plate. The kit contains a polishing plate, abrasive, chamois and rubber gloves.

39

Others

Far Infrared Kit

( P/ N 206- 72016- 91) In the far infrared region up to 240 cm-1, peaks of inorganic compounds and organometallic complexes are observed. The Far Infrared Kit is a Csl beam splitter mounted on the IRPrestige-21 for measuring spectra in the far infrared region. Using the Csl beam splitter enables spectra in the far infrared region up to 240 cm-1 to be measured. A standard light source and detector are used. Since the 400 cm-1 to 240 cm-1 region absorbs lots of moisture in air, purge the instrument with desiccated air, 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.
Far Infrared Spectrum of Bismuth Oxide

Feature
Measurement wavelength range 5000 cm-1 to 240 cm-1

Standard Co n t ent
Description Csl beam splitter Quantity 1

40

N I R M easur em ent

N IR M easu r em en t A ccesso r ies fo r t h e IR Pr est ig e- 21


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.

In t ro d u ct io n t o N ear- Inf rared ( N IR ) A nalysis


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-21, 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.

N ear- In f rared A pplicat ions


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.

A p p licat io n s an d A ccessories
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 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 (Macro Platform required). If the sample is a powder, use either diffuse reflection equipment UpIR A, near-infrared integrating sphere IntegratIR A, or a reflectiontype 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. of each component peak will depend on temperature. Therefore, measurement is conducted at a constant temperature using a heating transmission cell system. Here, the IRSolution PLS Quantitation Program will be required to create the calibration curves.

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.

D if f eren ce B et ween U pIR A and Int egrat IR 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 1. 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 1. Cost 2. Specialized for powdered sample analysis.

41

N I R M easu r em e n t

NIR Set

(P/N 206- 72015- 91) This option is attached to the IRPrestige-21, enabling near-infrared measurement. Experiments are conducted via software that switches between the mid-infrared and the near-infrared. (Cannot be used with the FTIR-8000 series.)

Specificat io n s
Measurement Range: Beam Splitter: Light Source: Detector: 12,500 cm-1 to 3,800 cm-1 Silicon-coated CaF2 Tungsten iodine lamp InGaAs detector

Standard Contents
Product Name Beam Splitter Storage Box CaF2 Beam Splitter Quantity 1 1

Upload Type Diffuse Reflectance Attachment UpIR A

(P/N 208-97271-91)

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.

Specificat io n s
Measurement range: 10,000 to 3,800 cm-1 Accessory recognition function: Included

Standard Accessories
P/N Product Name UpIR A Main Unit Gold-coated mirror for reference 208-97271-13 Test tube (pack of 6) 208-97271-17 Test tube holder Sample holder with sapphire window 208-97271-18 Quantity 1 1 1 1 1

Options
Product Name Test tube with screw cap (pack of 200) 25 x 2 mm sapphire window P/N 208-97271-20 208-97271-21

NIR Integrat ing Sphere IntegratIR A

(P/N 208-97272-91)

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 (P/N 206-72715-92 for IRPrestige-21 CE model, or P/N 206-72715-91 for other IRPresige-21 model) must be purchased separately.

Specificat io n s
Measurement range: 10,000 to 3,800 cm-1 Accessory recognition function: Included

Standard Accessories
Product Name IntegratIR A Main Unit Gold diffusion mirror with protective cap Test tube (pack of 6) Test tube holder P/N 208-97272-12 208-97271-17 Quantity 1 1 1 1

Options

Spectrum of a tablet (antipyretic)

Product Name Test tube (pack of 6)

P/N 208-97272-14

42

N I R M easur em ent

F ib er C o u p ler

( P/ N 2 0 6 - 7 2 7 5 1 - 9 1 )

The fiber coupler comes with two SMA connectors. Various fiber probes with SMA connectors can therefore be connected. The fiber coupler and fiber probe are separate items. Please purchase both of them. Contact Shimadzu when using fiber probes other than the recommended probe.

Sp ecif icat io n s
Measurement range: 10,000 to 3,800 cm-1 (However, this varies depending on the probe used.) Connector shape: 2 x SMA Accessory recognition function: Included

St an d ard A ccessories
Product Name Fiber Coupler Storage Box Quantity 1 1

Opt ions
Product Name Fiber cable for adjustment P/N 206-72758-91

R ef lect ive F ib er Probe

( P/ N 2 0 6 - 7 2 7 6 0 - 9 1 )

Near IR rays emitted from the probe head are directed to the sample, and the reflected light is collected for measurement. Pretreatment such as KBr dilution is unnecessary. Just insert the probe into the sample powders, or samples can be analyzed while they are contained in bags or glass bottles.

Sp ecif icat io n s
Measurement range: Connector shape: Probe shape: 10,000 to 3,800 cm-1 2 x SMA Probe head 6.4 mm dia. x 50 mm, SUS303 Handle 18 mm dia. x 100 mm, aluminum Operating temperature: Room temperature Permissible bending radius: 100 mm Length: 1 m from the probe head to connector

St an d ard A ccessories
Product Name Fiber Probe Mini Stand Reference Mirror Quantity 1 1 1

Op t io n s
Product Name Gold Diffusion Mirror Gold-coated Mirror Flexible Stand Mini Stand P/N 208-97272-12 208-97271-13 046-05514-01 046-05514-02
Black: L-Ala Blue: L-Arg Red: L-(Cys)2 Spectra of drugs contained in a glass bottle

43

N I R M easu r em e n t

Heating Tran smission 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 120C. The set comprises a transmission cell for measurement under heating and a temperature controller.

Specificat io n s
Measurement range: 12,500 to 3,800 cm-1 Accessory recognition function: Included Temperature range: Room temperature to 120C (heater temperature) Applicable test tube: 6 mm dia. x 50 mm Output: 5A Max. Power supply: 120/220 V selectable Results of measuring octanoic acid under heating (measured at Standard Accessories 10C intervals from 30 to 120C). P/N Quantity Product Name 1 Heating Transmission Cell Holder 208-97273-92 Increase in liberated 208-97274-92 1 Temperature Controller OH (6,920 cm-1) 1 6 x 50 mm test tube (pack of 500) caused by heating can be verified.

Options
Product Name 6 x 50 mm test tube (pack of 500) P/N 208-97273-11

Infrared M icroscope AIM-8800

( P / N 206- 7 2 5 0 0 - 9 2 / 9 6 / 3 4 / 3 5 )

NIR measurements of microscopic parts of the sample can be made. By fitting the AIM-8800 to an IRPrestige-21 unit with the NIR set installed and using the highsensitivity MCT detector, measurements can be conducted in the 10,000 to 3,800 cm-1 region. In order to use this accessory, the Light Beam Switching Kit (206-70125-92), AIM Connection Kit (206-72019-92) and Video Capture Board (088-50648-01) are required separately. The AIM-8800 will not work with notebook PCs.

Specificat io n s
Measurement range(Note) : 10,000 to 3,800 cm-1 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-21 unit with the NIR set installed.

Options
Product Name IRsolution Mapping Program P/N 206-72332-91

Reflection spectrum of an electronic part. The thickness of the coating film was calculated to be 2.28 m from the interference fringe. (refractive index 1.5)

50 %T 25 10000 9000 8000 7000 6000 5000 4000 1/cm

44

O pt i onal S of t w ar e

W id e Variet y o f Opt ional Programs


A variety of optional software is available for IRsolution, the Windows-based IRPrestige-21 control software that offers outstanding ease-ofoperation 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.

IR so lu t io n A g ent

( P/ N 2 0 6 - 2 1 6 0 0 - 9 2 )

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 21 CFR Part 11 (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.

M ap p in g Pro g ram

( P/ N 2 0 6 - 7 3 7 3 8 - 9 1 )

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)

45

Opti onal S o f t w a r e

Macro Plat f o rm

( P/ N 206- 72330- 91)

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 Pro gram

( P/ N 206- 73737- 91)

The 3D display program offers the following functionality. Changes the method of displaying dataData can be displayed in birds 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 Quant it at ion Software

( P/ N 206- 7233 1 - 9 1 )

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

Curvefittin g ( Peak split) Softwar e

(P/N 206-72333-91)

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 (3150-2750 cm-1) of ABS resin spectrum. Top : Target peak and specified peaks Bottom : Component peaks and a synthesized peak

46

M at er i al s for C el l Wi ndow P l at e

2. Materials for Cell Window Plate


Sample cells have a window made of various materials to meet the requirements of your analyses, such as wavenumber range and physical and chemical characteristics of the sample. The characteristics and features of the materials popularly used for the window of sample cells are described below. Some of the materials are used only rarely due to the difficulty of processing and high costs.

M at erials o f Sample C ell W indows


MateriaI Wavenumber range, cm-1 (m) 40,000~340 (0.25~29.4) NaCl 50,000~600 (0.2~16.6) KCl 40,000~500 (0.25~20.2) Csl 33,000~200 (0.3~50.0) KRS-5(TIBr+Tll) 16,600~250 (0.6~40.0) KRS-6(TIBr+TICI) 20,000~330 (0.5~30.0) AgCl 25,000~450 (0.4~22.2) AgBr 22,000~300 (0.45~33.3) ZnS(Irtran-2) 10,000~550 (1.0~13.3) ZnSe(Irtran-4) 10,000~550 (1.0~18.1) As 2 Se 3 10,000~600 (1.0~16.6) BaF 2 50,000~770 (0.2~12.9) CaF 2 (Irtran-3) 50,000~1,100 (0.2~9.9) CdTe(Irtran-6) 20,000~320 (0.5~31.2) Si 8,000~660 (1.25~15.1) Ge 5,500~660 (1.8~16.6) Diamond,type 40,000~12.5 (0.25~800) SiO 2 (Fused Silica) 50,000~2,500 (0.20~4.0) Refractive index (1000cm-1) 1.52 Water solubility at 20C (g/100 g H2O) 65 % transmission (thickness) 90% (5mm) 90% (5mm) 90% (10mm) 90% (5mm) 70% (2mm) 75% (1.5mm) 80% (5mm) 70% (1mm) 65% (1mm) 60% (0.63mm) 90% (1mm) 95% (3.6mm) 40% (5mm) 55% (2.5mm) 50% (2mm) 70% (1mm) 85% (1mm) Max.Temp. (Melting point) 300 (700) 400 (801) (776) 200 (621) 200 (414) (423) 29.9 40.2 9.3<100> 18.2<100> Knoop hardness

KBr

7.0<100>

1.49

36

1.46

34

1.74

44(0C)

2.37

0.05

2.17

0.32

1.98

1.5 x10-4

(457)

2.2

12 x10-6

200 300 (1180 Sublimate) 350 (1700) 180 (Softening poinit) 500 (1280) 900 (1402) 300 (1041) 300 (1420) 270 (936)

2.2

Insoluble

354

2.4

Insoluble

250

2.6

Insoluble

1.42 1.39 (2000cm-1) 2.69

0.004

82(500g)

Insoluble

158(500g) 43.5 Vickers hardness 1150

Insoluble

3.4

Insoluble

4.0

Insoluble

10

2.38 1.42 (3000cm-1)

Insoluble

(400) 1710 Softens

Mohs scale 500

Insoluble

%Transmission values given are typical ones, in the wavenumber range applicable to the respective materials, including the loss due to surface reflection.

47

Mater i als fo r C e l l Wi n d ow P la t e

Characterist ics of Cell Window Materials


Only the main characteristics of the cell window materials are described below. The "Clean-up" lists present only the representative solvents used to wash the cell windows. Even if a solvent is listed as "Clean-up", confirm that the solvent does not react with the samples. The "Harm" solvents can destroy the window plate through corrosion or dissolving. Some solvents not listed as "Harm" can be harmful to the material.

KRS-5
(Thallium bromide-iodide)

"Clean-up": chloroform, carbon tetrachloride, xylene.

Wide wavenumber range. High refractive index. Most widely used for ATR prisms. Almost insoluble in water. Toxic; must be processed at an authorized manufacturer's site.

"Harm": Lower alcohol. Ammonium salt solution, sulfuric acid, ammonia, EDTA, a solution of a compound that reacts with thallium to form a complex.

KBr
(Potassium bromide)

"Clean-up": chloroform, carbon tetrachloride.

KRS-6
(Thallium Bromide-Iodide) Similar characteristics as KRS-5. Not so popular as KRS-5.

"Clean-up": xylene, methanol.

Low cost and wide wavenumber "Harm": range. Aqueous solution. Lower alcohol. Easy to process with alcohol anhydride. Most popularly used. High mechanical strength. Store under humidity conditions lower than 50%. Some solvents not listed as "Harm" can be harmful to the material.

"Harm": A solution of a compound that reacts with thallium to form a complex.

AgCI
(Silver chloride) Almost insoluble in water. Darkens when hit by ultraviolet rays. Corrodes metals other than stainless steel. Fragile.

"Clean-up": acetone, CH2Cl2.

NaCl
(Sodium chloride)

"Clean-up": chloroform, carbon tetrachloride.

"Harm": Ammonia salt solution, EDTA, a solution of a compound that reacts with silver to form a complex.

Most inexpensive. Wide wavenumber range. Store under humidity conditions lower than 50%.

"Harm": Aqueous solution. Lower alcohol.

AgBr
(Silver bromide)

"Clean-up": with acetone, CH2Cl2.

KCI
(Potassium chloride) Similar characteristics as NaCl and KBr. Not popularly used.

Similar characteristics as AgCl.

"Harm": Ammonia salt solution, EDTA, a solution of a compound that reacts with silver to form a complex.

ZnS Csl
(Cesium iodide) Soft and hence liable to injure. "Harm": Applicable to analysis in Aqueous solution. Lower alcohol. far-infrared region. Highly deliquescent. Store under humidity conditions lower than 40%, and handle with care. "Clean-up": chloroform, carbon tetrachloride. (Zinc sulfide)

"Clean-up": acetone, alcohol.

Non-water soluble. "Harm": Acidic solution. Resistant against mechanical and thermal shocks. High refractive index. Effectively used for evaporation depositing. Pulverized and briquetted ZnS is called lrtran-2

48

Z n Se
(Zinc selenide)

"Clean-up": acetone, H2O.

Si
(Silicon)

"Clean-up": acetone, H2O.

Non-water soluble. "Harm": Resistant against weakly acidic Strongly acidic or alkaline solution. or alkaline solution. High refractive index. Used for ATR prisms. Pulverized and briquetted ZnSe is called lrtran-4. Applicable pH range: 6.5-9.5

Widely used as the material "Harm": for semiconductors. HF-NO3 mixture. Rarely used as cell window material. Ge can substitute Si as cell window material.

Ge A s 2 Se 3
(Arsenic tri-selenide) Insoluble in water. Brittle. (Germanium) "Clean-up": acetone, H2O.

"Clean-up": toluene, H2O.

Widely used as the material "Harm": for semiconductors. Hot sulfuric acid. Easily processed to be lenses. High refractive index, suitable as the material for ATR prism used in analysis of highly refractive samples. Non-watersoluble. "Clean-up": acetone, H2O.

B aF 2
(Barium fluoride) Soluble in acidic solution and ammonia. Usable up to 500C. Almost insoluble in water.

"Harm": Ammonium salt solution, acidic solution.

Diamond Type II
(Diamond)

"CIean-up": ethanol, acetone.

C aF 2
(Calcium fluoride)

"Clean-up": acetone, H2O.

Soluble in ammonium salt solution. "Harm": Resistant against acidic or Ammonium salt solution, acidic alkaline solution. solution. Hard, high mechanical strength. Suitable for high-pressure cell. CaF2 that occurs in nature is called fluorite. CaF2 which is pulverized and briquetted is called lrtran-3.

Harder than any other material. Applicable to wavelength range from ultraviolet to far infrared, though a gradual absorption is seen in the range from 3000cm-1 to 1500cm-1. Natural diamond is classified as Type I and Type II, and only the Type II is used as the material for cell window. Extremely expensive. Recommended for the window of high-pressure cell.

SiO 2
(Fused silica)

"CIean-up": ethanol, acetone.

CdTe
(Cadmium telluride)

"CIean-up": acetone, alcohol.

Effective for analysis in the ultraviolet and visible regions. Though useful up to 4 nm in the lR region, this material ensures high stability and is easy to process.

Material for mercury cadmium "Harm": telluride (MCT) detector. Acidic solution. Expensive. Used for cell window only in special cases. CdTe which is pulverized and briquetted is called Irtran-6.

49

Mater i als fo r C e l l Wi n d ow P la t e

Transmittan ce Characteristics of Representative Cell Window Materials

Transmittance (%)

Wavenumber (cm-1)

Transmittan ce of Alkali Halide Pellet (1mm thick)

Transmittance (%)

Wavenumber (cm-1)

50

U sab le W aven u mber R ange f or Various Solvent s

Carbon disulfide (0.1mm) Carbon tetrachloride (0.1mm) Chloroform (0.1mm) Dichloroethane (0.1mm) Ethylene tetrachloride (0.1mm)

Wavenumber (cm-1)

51

JQA-0376

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