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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
Semiconductors
Type of Sample
Oil content measurement Nonvolatile organic solvents Liquids Volatile organic solvents Aqueous solutions
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
3
Shi m adz u A c c e s s o r y L i n e - u p
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
27
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
30
31
Transmission Measurement
32
33
34
Pellet Measurement
SSP-10A SA18-3M
35
36
38
39 40 42
Others
UpIR A IntegratIR A
NIR Measurement
43 44 45
AIM-8800
Optional Software
46
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
( 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
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.
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
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
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.
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.
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.
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.
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
Infrared Light
DuraSamplIR2 Optics
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.
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
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.
DuraScope
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.
10
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. 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.
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.
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
12
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
Sample 20
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
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
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
Incident light
Applications
The diffuse reflectance spectroscopic method is applicable to any sample that can be pulverized. It also permits using, as the diluting substance, diamond powder or the like, which is not applicable to the KBr pellet method. This method is also applicable to detection of substances dissolved in a volatile solvent, such as fractions of liquid chromatography. LC effluent is made to drop on KBr powder, the mobile phase is removed by evaporation, and then the fraction is analyzed with the FTIR instrument equipped with a diffuse reflectance attachment.
HPLC fraction Remove mobile phase through evaporation Diffuse reflectance attachment
16
Interferometer
Detector
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
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
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.
Supplies
Description SiC emery paper (#320), 100 sheets SiC emery paper (#400), 100 sheets P/N 200-66751-01 200-66751-02
SiC Sampler
18
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.
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
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
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
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)
20
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
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
(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
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.
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
Spectrum of Single Fiber Red: Diamond cell used Black: Diamond cell not used
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
24
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
( 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
ASC Connector
26
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.
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
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).
Sample Switcher 21
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.
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
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
St an d ard C o n t ent
Description Switching mirror (with polystyrene film) External input signal connector Quantity 1 1set
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.
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.
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.
206-62307)
(Window)
A set of a second sample compartment, an MCT detector, a preamplifier, and a condenser mirror.
(Window)
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
( 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
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
31
Tr ansm i s si o n M e a s u r e me n t
( 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
EZ-Clip13
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
EZ-Clip25
This one-touch sample holder uses a clip exclusive for 25 mm dia. samples. An O-ring is located on the surface of the holder that contacts the sample to prevent damage to the sample.
Features
Thick samples (max. thickness 13 mm) also can be held. Diameter of light passage hole: 10 mm
32
Gas C ell
Gas cells are used when measuring gas samples. Select the optical pathlength to suit the concentration of the component.
) )
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
Pressure gauge
33
Pel l et Me asu r e m e n t
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.
Supplies
Description 10 briquetting frames, 3 mm dia., and upper and lower cylinders P/N 200-66748
(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
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
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
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
(P/N 200-93508) Used to prepare KBr pellets or samples for diffuse reflectance method.
(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
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
202-32000-30 KRS-5 Demountable Cell A pair of KRS-5 plates (201-97943) 10 sheets 10 sheets
Contents
1set 0.025 mm lead spacer (204-04900-13) 10sheets 0.1 mm lead spacer (204-04900-15)
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
( 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
38
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)
( 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
( 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
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.
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
(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
(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
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
( 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
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
( 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)
44
O pt i onal S of t w ar e
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.
45
Opti onal S o f t w a r e
Macro Plat f o rm
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.
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.
( 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.
(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
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
0.004
82(500g)
Insoluble
Insoluble
3.4
Insoluble
4.0
Insoluble
10
Insoluble
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
KRS-5
(Thallium bromide-iodide)
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)
KRS-6
(Thallium Bromide-Iodide) Similar characteristics as KRS-5. Not so popular as KRS-5.
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.
AgCI
(Silver chloride) Almost insoluble in water. Darkens when hit by ultraviolet rays. Corrodes metals other than stainless steel. Fragile.
NaCl
(Sodium chloride)
"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%.
AgBr
(Silver bromide)
KCI
(Potassium chloride) Similar characteristics as NaCl and KBr. Not popularly used.
"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)
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)
Si
(Silicon)
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.
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.
Diamond Type II
(Diamond)
C aF 2
(Calcium fluoride)
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)
CdTe
(Cadmium telluride)
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
Transmittance (%)
Wavenumber (cm-1)
Transmittance (%)
Wavenumber (cm-1)
50
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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