Related Manuals for Thermo Electron Thermo Spectra-Tech Collector II
Summary of Contents for Thermo Electron Thermo Spectra-Tech Collector II
- Page 1 COLLECTOR™ II User's Manual P/N 0030-0XX P/N 700-0042 Version 3.9 A Thermo Electron business...
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Page 3: Table Of Contents
Table of Contents General Information The Manual ......................3 Packing and Unpacking...................3 Technical Support Center..................3 Copyrights & Trademarks..................3 Contact Thermo Spectra-Tech ................3 Introduction to Diffuse Reflectance Spectroscopy...........4 COLLECTOR II Product Description ...............4 BLOCKER Description ....................6 Diffuse Reflectance Sampling Technique ...............7 Installation & Alignment Sample Compartment Baseplate Removal .............9 COLLECTOR II Installation ...................10 Purge Cover/Purge Insert Removal ..............13... -
Page 5: General Information
General Information The Manual This manual is designed as a tutorial to guide you through the installation of Collector II and through a typicalanalysis. If you have any questions, please contact a Thermo Spectra-Tech Technical Representative. Packing & Unpacking The Collector II is shipped in a protective foam filled cardboard box. Upon arrival please check the box to ensure that all pieces have been received and that no pieces are damaged. -
Page 6: Introduction To Diffuse Reflectance Spectroscopy
Banner Introduction to Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) Diffuse reflectance spectroscopy is a powerful technique for infrared analysis of fine particles and powders in concentrations that range from undiluted to parts per thousand (0.1%). Analyses are fast and easy because little or no sample preparation is required. Powder samples can be measured “as is”... -
Page 7: Collector Ii Product Description
Banner COLLECTOR II Product Description The Spectra-Tech Diffuse Reflectance (DRIFT) Accessory, “The COLLECTOR II” is designed for use in FT-IR spectrometers. The design employs 4 flat and 2 aspherical reflectors, plus an alignment mirror. The aspherics are off-axis ellipsoids which focus and collect infrared energy with a 6X condensation of the beam. -
Page 8: Blocker Description
General Information BLOCKER Description For certain samples, it might be desirable to eliminate the component of the reflected energy which is not diffused by scattering - commonly called the specular component (reflectance from a mirror is pure specular). While specular reflectance occurs over all angles, the COLLECTOR II has a provision for lowering it’s contribution to the spectrum - the BLOCKER. -
Page 9: Diffuse Reflectance Sampling Technique
General Information Diffuse Reflectance Sampling Technique Specular Reflection When the infrared beam is focused on the surface of the particulate sample, it can interact with the sample two ways. First, it may simply reflect off the sample surface in the same way visible light reflects off a mirror. - Page 10 General Information Diffuse Reflectance Sampling Technique Diffuse Reflectance Spectrum The goal of diffuse reflectance spectroscopy is to maximize the diffused component, because it contains information about the absorption characteristics of the sample, and to minimize the specular component, which causes distortions in the data. Since it is difficult to determine the absorption characteristics and the refractive index of a powdered sample just by looking at it, the recommended approach is to try running the pure powder using a KBr background.
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Page 11: Installation & Alignment
Installation & Alignment Sample Compartment Baseplate Removal All Collector II’s are pre-aligned and tested in a FT-IR spectrometer prior to shipment. Additionally, most versions of the Collector II are shipped with the Baseplate pre-attached to the accessory for rapid and reproducible installations (as illustrated below). This baseplate attaches to the floor of your spectrometer sample compartment and provides properly positioned mounting holes for the Collector II. -
Page 12: Collector Ii Installation
Installation & Alignment COLLECTOR II Installation Record the open beam energy Record the open beam energy of your spectrometer by monitoring either the throughput energy number or the height of the centerburst of the interferogram. Note this value for later use. Attach foam purge rings Attach purge rings to both ends of the Collector II. - Page 13 Installation & Alignment COLLECTOR II Installation Attach hosing Attach the open end of the plastic hosing (provided) to the purge nipple on the back of the Collector II. For Nicolet systems with purge capabilities: Attach the other end of the tubing to the socket in the sample compartment.
- Page 14 Installation & Alignment COLLECTOR II Installation Adjust Sample Height/Focus While monitoring maximum throughput energy value or the height of the centerburst of the interferogram, use a 3/32 balldriver to adjust the screw that positions the alignment mirror for maximum throughput signal. Energy Throughput Validation When the Collector II is installed, observe the “throughput count”...
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Page 15: Purge Cover/Purge Insert Removal
Installation & Alignment Purge Cover/Purge Insert Removal Detach Purge Cover/Purge Insert The Collector II with its attached baseplate must be removed from the sample compartment to access the screws that hold the Purge Cover/Purge Insert. Remove the four buttonhead screws that hold the Purge Cover/Purge Insert in place using a 1/16 balldriver. -
Page 16: Mirror Alignment
Installation & Alignment Mirror Alignment Adjustment Introduction The COLLECTOR II is configured at the factory for your spectrometer. The COLLECTOR II is also pre-aligned so that only minor adjustments (tilt and/rotation) of the mirrors may be necessary. There are four mirrors to adjust M1, M2, M6, M7 and the sample position. - Page 17 Installation & Alignment Mirror Alignment Check Beam on Alignment Mirror Leave the OUTPUT ellipsoid mirror open. Close the INPUT ellipsoid mirror. Note: The output is the left ellipsoid for a right to left beam and the right ellipsoid for a left to right beam.
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Page 18: Mirror Fine Adjustment
Installation & Alignment Mirror Fine Adjustment Fine-Tune Mirror Rotation Mirror Put the spectrometer in align Mount Either mode (throughput, tune End of Tool etc.). can be used Peak the throughput energy to all the mirrors by rotating each mirror in the following Mirror order M7, M6, M2 and M1. - Page 19 Installation & Alignment Mirror Fine Adjustment Fine-Tune Tilt Adjustment Test the tilt of the mirror by lightly pressing the mirror mount in each direction noting the energy count. The tilt of the mirrors is adjusted through the two screws located at the base of the mirrors.
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Page 20: Purge Cover/Purge Insert Reinstallation
Installation & Alignment Purge Cover/Purge Insert Reinstallation Attach Purge Cover/Purge Insert After the Collector II is aligned for optimal energy throughput, remove the accessory from the compartment and attach the Purge Cover/Purge Insert. Reattach Purge Hose Reattach Purge Hose (see instructions on page 9 &... -
Page 21: Operation
Operation Using the COLLECTOR II Select an Appropriate Background A suitable background must be chosen. The background must match the sample matrix. Potassium Bromide (KBr) makes a good diffuse reflectance dilution matrix since it has no absorption peaks in the infrared. KBr is also a good background for many undiluted or neat samples. - Page 22 Operation Using the COLLECTOR II Collect Background Spectrum Pull the push/pull tube out. Place the cup containing the background powder into the cup holder. Push the push/pull tube firmly into the sampling position. Note: The ellipsoids should remain closed. Collect the Background spectrum. Collect Background Spectrum - Alternate Method Slide the ellipsoids open.
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Page 23: Sample Preparation Powders
Operation Sample Preparation Powders The diffuse reflectance technique is ideal for measuring pure samples or mixtures that are available in powdered form, such as pharmaceuticals and other high molecular weight organic materials. Some samples may need to be ground for the analysis. Powders are easier to run by diffuse reflectance than by infrared transmission because less preparation is required. - Page 24 Operation Sample Preparation Powders The following is a general rule to follow when preparing samples and matrices for Diffuse Reflectance analysis: Organic Samples: 10% Sample (by weight) 90% Matrix (by weight) Inorganic Samples: 2-5% Sample (by weight) 95-98% Matrix (by weight) Sample Cups Volume By Weight: Micro Cup: 0.10 grams KBr Macro Cup: 0.25 grams KBr...
- Page 25 Operation Sample Preparation Powders 5.When the sample cup is filled, place it on a flat surface and level the sample surface with a spatula. This reduces reflections off the sample Spatula surface and helps ensure reproducible results. Sample Collector II...
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Page 26: Sample Preparation Intractable Samples
Operation Sample Preparation Intractable Samples Diffuse Reflectance is not limited to powders and small solid samples. A Si-Carb™ Sampling Kit can be used in conjunction with the COLLECTOR™ II to analyze many types of intractable samples without time consuming sample preparation. A small disk of silicon-carbide paper is used to abrade the surface to be analyzed. -
Page 27: Factors That Affect Diffuse Reflectance Spectra
Operation Factors that Affect Diffuse Reflectance Spectra The spectral information you get from a diffuse reflectance accessory is affected by a number of factors. Refractive Index of Sample The higher the refractive index of the sample, the more true specular (mirror) reflection will occur at the sample surface. - Page 28 Operation Factors that Affect Diffuse Reflectance Spectra Homogeneity of the Sample The more uniform the sample, the more linear the relationship between band intensity and sample concentration in the resulting spectrum. You can obtain the best results when the sample material is thoroughly ground and well mixed with the matrix material, if one is used.
- Page 29 Operation Factors that Affect Diffuse Reflectance Spectra Common Problems with Diffuse Reflectance Spectra As with any analytical technique, you will have more confidence in the data you produce if you recognize problems when they occur. This section identifies some common problems with diffuse reflectance analysis, illustrates their effects on the spectral data and explains how to solve them.
- Page 30 Operation Factors that Affect Diffuse Reflectance Spectra Sample Bands are too Big Bands with values below 1% R (above 49 Kubelka-Munk units) are considered totally absorbing and normally have a flattened or “squared off” end. Several totally absorbing bands are present in this spectrum. When the % reflectance value of a spectral band approaches 1% R (49 Kubelka-Munk units), the intensity is so close to totally absorbing that it...
- Page 31 Operation Factors that Affect Diffuse Reflectance Spectra To minimize specular reflection due to particle size or concentration, thoroughly grind the sample material and mix it well with the matrix material, if one is used. The particles should be small and the mixture should be homogeneous in particle size and composition.
- Page 32 Operation Factors that Affect Diffuse Reflectance Spectra To minimize or eliminate this effect, the sample can be further diluted with a diffusely scattering matrix such as KBr and the matrix crystals can be crushed to a smaller and more consistent size. Potassium permanganate -1% in KBr.
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Page 33: Mounting Methods
Appendix A Mounting Methods Spectrometer Mating Plate Standoffs Analect FX6200 None Beckman 1000, 2000 .576” Bomem DA3 1-3/4” Bomem Michelson 1-1/2” Bomem MB 1” IBM 32,85,98,38 None 1-1/2” Digilab , FTS-14/15/20/80 3/4” Digilab Qualimatic, FTS-50, FTS-60 None Digilab FTS-10, 11 1”... - Page 34 Appendix A Mounting Methods Nicolet 5-X, MX-S Digilab Qualimatic 10-X, 3600, MX-1 FTS-50, FTS-60 and old 20's with 3600 optical bench. (2) 8-32 screws thru clearance holes in Bottom view of baseplate. baseplate. Two hold-down screws to mating baseplate. Mounts on two pins into sample compartment.
- Page 36 Empowering your FT-IR A Thermo Electron Company Thermo Spectra-Tech Phone: 203-926-8998 230 Long Hill Cross Rd. 800-THE-FTIR PO Box 869 FAX: 203-926-8909 www.thermospectra-tech.com Shelton, CT 06484-0869 info@thermospectra-tech.com...
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