Quantitative measurement of active ingredient in a mixture of magnesiumstearate, lactose, EMCOMPRESS®, cellulose and CAB-O-SIL ®NIR IntegratIR with optional transmission tablet analyzerThe NIR IntegratIR comes complete with diffuse gold reference,sample holders and a removable general-purpose sample mountingplate. The NIR IntegratIR is configured for each specific FTIRspectrometer and includes a pre-aligned mount for your instrument.The NIR IntegratIR is a cost-effective, high-performancesampling option for laboratories with a standard FTIR spectrometerequipped with a near-infrared light source and beam splitter.The optional transmission tablet analysis stage for the NIRIntegratIR provides an automated tool for sampling 10 tablets ofa variety of sizes. With this option you can measure formulationreproducibility or verify pharmaceutical composition.P A R T N U M B E R048-60XXO R D E R I N G I N F O R M A T I O ND E S C R I P T I O NNIR IntegratIR Integrating Sphere AccessoryIncludes 2" diffuse gold-coated integrating sphere, InGaAsdetector, detector preamplifier, cable and baseplate for thespecific model spectrometer. The accessory also includes agold reference standard, vial holder, and 25 glass vials.Notes: Please see the FTIR instrument code sheet. Your spectrometer must becapable of interfacing with an external detector.Sampling Options for NIR IntegratIRP A R T N U M B E RD E S C R I P T I O N048-2999 Glass Sample Vials (Pack of 25), 19 x 65 mm048-3000 Diffuse Gold Reference048-3070 NIST Traceable NIR Reference Standard048-3071 NIST Traceable NIR Reference Standard – Recertification044-3010 Glass Vial Holder (for 19 mm vials)048-0150 Rotating Stage for Petri Dish (for heterogeneous samples)Includes 100 x 20 mm Petri Dish048-0151 Rotating Stage Adapter for 500 mL beaker048-0060 Automated Transmission Tablet Analysis Stage forNIR IntegratIRIncludes 3 tablet plates for 7.5, 8.5 and 10 mm tabletsNote: Please contact us for other options. Stage rotates counterclockwise.I N T E G R A T I N G S P H E R E S – R E F L E C T A N C E F R O M A L L P E R S P E C T I V E S61
P I K E T E C H N O L O G I E S W W W . P I K E T E C H . C O M 6 0 8 - 2 7 4 - 2 7 2 1Integrating Spheres – Introduction and TheoryMeasuring Sample ReflectanceReflectance sampling accessories rely upon a light beam comingfrom the spectrometer to be focused upon the sample. In orderto achieve the best signal-to-noise ratio (SNR), the smaller thefocus is, the easier it is to refocus the illuminated sample spotback onto the detector. In order to measure light reflected at alarger angle, optical designs will allow only a small area of thesample to be projected onto the detector. This arrangementserves well if the sample is microscopically homogeneous, butwill result in a larger sample position error. When the sample ismoved, the focused beam will see a different portion of the sampleresulting in measurement-to-measurement differences. This iscalled insertion error because the spectrum will be slightlydifferent each time the sample is inserted.Some industrial or natural samples are inhomogeneouseither because they are mixtures of different substances orbecause they have a particle size comparable to the probingbeam diameter. Clearly, if the probing beam could be larger andthe reflected light could all be collected, a more representativespectrum could be measured.Some other samples develop a directional scattering. Forexample, fibers wound on a mandrel are highly oriented, not justmacroscopically as parallel, unidirectional filaments, but also inmany cases the molecules of the drawn fibers are oriented withinthe fiber itself. Such a sample, when placed in a reflectanceaccessory will generate different results depending on the anglefrom which the detector is “viewing” the sample. When the overallreflectance needs to be measured reproducibly, for example tomeasure the concentration of a minor ingredient in the sample,only isotropic optical systems, insensitive to such directionalitiescould be utilized.Furthermore, in some cases, not just the reflectance in asmall solid angle but the reflectance in all angles is sought. Mostreflectance accessories measure at fixed or variable angles, narroweror wider collection angles, but there is a need for a devicethat uniformly collects all reflected light from a sample. In otherwords it measures the total reflectance of the sample.Therefore the main reasons for using integrating spheres forthe measurement of sample reflectance are the following:• Efficient measurement of combined diffuse and specularreflectance• Uniform detection of reflectance even when sample isinhomogeneous• Isotropic detection of reflectance even on samples that reflectin preferred directions• Reduction of polarization effects from the illuminating beamand the sample• Measurement of absolute reflectance (with specialintegrating spheres)All of the above concerns are addressed with integratingsphere based reflectometers.Integrating Sphere OpticsIntegrating spheres are highly reflective enclosures that areplaced in close proximity to the sample, such that the reflectedlight enters the sphere, bounces around the highly reflectivediffuse surface of the sphere wall and finally impinges upon thedetector – usually part of the integrating sphere assembly. Thename, integrating sphere, refers to one of the main functions ofthe device, namely that it spatially integrates the light flux, in ourapplication the light reflected from a sample. In spite of the longhistory of engineering and development of the sphere, the applicationsand further developments continue to this day. Advancesin the theory, detector and electronics development and most ofall, new applications, drive the progress.As the name implies, the main part of the device is a spherewith a very highly reflecting inner surface. The surface shouldapproach the ideal Lambertian scatterer, which means that thelight falling on the surface is evenly scattered in all directions andthe scattered light intensity is proportional to the cosine of theangle of observation.EntrancePort (A e )ρ wSampleArea ofSurface (A s )Optical geometry of an integrating sphereSamplePort (A s )F.O.V.BaffleDetectorPort (A d )In an upward sample positioning sphere the infrared beamfrom the interferometer is directed through an entrance portonto the sample placed behind the sample port (shown above).Samples can be directly touching the sphere or separated fromthe sphere by a thin, infrared transparent window. The detectoris placed close to the sphere, so that it can view the integratingsphere with a large solid angle. In order to improve the isotropy(non-directionality) of the detection, the detector is not directly inthe line of sight of the sample. A small, also highly reflective andscattering baffle is placed in the sphere such that it blocks thefirst reflection of the sample from reaching the detector.62
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FTIR INSTRUMENT CODEXXABB BomemFTLA