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Thermo Scientific Nicolet NIR User Manual
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Thermo Scientific Nicolet NIR User Manual

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Nicolet NIR
with OMNIC Paradigm software
User Guide
269-362000
Revision A
March 2023

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Summary of Contents for Thermo Scientific Nicolet NIR

  • Page 1 Nicolet NIR with OMNIC Paradigm software User Guide 269-362000 Revision A March 2023...
  • Page 2 © 2023 Thermo Fisher Scientific Inc. All rights reserved. For technical support, please contact: www.thermofisher.com Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the product operation. This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.
  • Page 3 The optional Thermo Scientific NIR Module offers convenient, reproducible diffuse reflection sampling with the Nicolet™ iS™50 spectrometer using the Integrating Sphere or a fiber optic accessory. Figure 1-1: NIR Module Thermo Scientific NIR Module (mounts on the left side of the spectrometer) Thermo Scientific NIR Module User Guide 3...
  • Page 4 Standards wheel (contains 2%, 10%, 20%, 40%, and 80% glass filters and a polystyrene sample) The optional fiber optic sampling area can be used with the Thermo Scientific SabIR diffuse reflection probe, or with probes from other manufactures if they have SMA connectors. For information about additional sampling modules for the Nicolet iS50 spectrometer, contact our sales representative in your area.

  • Page 5: Conventions Used In This Manual

    Avoid hazard. Indicates a hazardous situation which, if not avoided, could result in serious injury or death. CAUTION Avoid hazard. Indicates a hazardous situation which, if not avoided, could result in minor or moderate injury. Thermo Scientific NIR Module User Guide...
  • Page 6 NIR Module NOTICE Follow instructions with this label to avoid damaging the system hardware or losing data. Note Contains helpful supplementary information. Tip Provides helpful information that can make a task easier. NIR Module User Guide Thermo Scientific...

  • Page 7: Operating Precautions

    Avoid scraping the sampling window with samples or sample containers. Protect the electrical port on the surface of the Integrating Sphere. If the connector is clogged or jammed, contact a Thermo Scientific service representative. Precautions for fiber optic cables: Do not drop the cables or knock them against a hard surface.
  • Page 8 Make sure the probe is clean before you insert it into the holster. Do not use the probe by itself to measure liquids. When sampling liquids, use the transflectance adapter available for the probe. NIR Module User Guide Thermo Scientific...

  • Page 9: Specifications

    SMA type Detector InGaAs Probe (optional) Thermo Scientific SabIR diffuse reflection probe SabIR Probe internal reference Spectralon® The NIR Module spectral range is dependent upon the spectrometer configuration. The table below shows the available configurations and their corresponding spectral ranges.
  • Page 10 11,000 - 3,800 cm-1 Note The NIR Module requires a CaF2 window installed in the external beam port on the left side of the spectrometer. Calcium Fluoride Indium Gallium Arsenide Extended range Potassium Bromide NIR Module User Guide Thermo Scientific...

  • Page 11: Compatible Software

    For more information, refer to the help system in your TQ Analyst software. Running Integrating Sphere or SabIR quantitative methods that have been transferred to any Thermo Scientific Antaris™ near-infrared analyzer that uses RESULT version 3.0 or higher. For information about adding...
  • Page 12 [This page intentionally left blank]...
  • Page 13 The Integrating Sphere is a fast and easy-to-use tool for diffuse reflection sampling of solids and powders. Integrating Sphere features The major features of the NIR Module Integrating Sphere are highlighted below. Figure 5-1: NIR Integrating Sphere sampling area features Touch Point Sample accessory holder Thermo Scientific NIR Module User Guide 13...
  • Page 14 Integrating Sphere beam path is selected. Sample accessory holder. Mounts over the sampling window and holds Thermo Scientific sample cups and tablet holder accessories. Internal gold reference. Can be used to collect background spectra. When enabled, the reference automatically moves into the beam path during background data collection and out of the beam path during sample collection.
  • Page 15 May be placed directly on the Integrating Sphere window or in one of the tablet holder accessories. May be measured in clear glass, flat-bottom vials, clear plastic bags, or in Thermo Scientific sample cups. Fill the sample cup to a depth of at least 5 mm. To improve reproducibility, fill the cup with the powder until it is overflowing and then level it with a spatula.
  • Page 16 Avoid hazard to the eye. Do not stare at the beam that exits the Integrating Sphere sampling window when the spectrometer is powered on and the Integrating Sphere beam path is selected. Before you begin NIR Module User Guide Thermo Scientific...
  • Page 17 To measure a tablet with the Integrating Sphere ❖ 1. If you have not already done so, go to Configure> Sample Location > NIR Integrating Sphere (or press the Integrating Sphere Touch Point) to configure the instrument for Integrated Sphere sampling. Thermo Scientific NIR Module User Guide...
  • Page 18 You can collect backgrounds using an internal or external reference (or using no reference). The most recent background spectrum remains in memory and is compared against sample data until a new background spectrum is collected. NIR Module User Guide Thermo Scientific...
  • Page 19 Sampling accessories for the Integrating Sphere Optional Thermo Scientific accessories for the Integrating Sphere are described in the table below, followed by additional information. To order an accessory, contact our local sales or service representative or see our contact information at the beginning of this document or help system.
  • Page 20 Table 5-2: Optional Thermo Scientific accessories for the Integrating Sphere This accessory… Does this… Sample accessory holder Holds Thermo Scientific sample cups and tablet holder accessories. The sample accessory holder attaches to the top of the NIR Module. The kit...
  • Page 21 The VLS allows you to run transflection experiments with viscous liquids. The VLS fits in the sample accessory holder. For detailed information about the VLS, please refer to the document or topic with that title. Thermo Scientific NIR Module User Guide...
  • Page 22 Sample Spinner, please refer to the document or topic with that title. USING THE SAMPLE ACCESSORY HOLDER To install the sample accessory holder ❖ 1. Insert the tab into the slot. Slot NIR Module User Guide Thermo Scientific...
  • Page 23 When performing multiple data collections on a sample, you can use these indicators, along with the indentations in the sample cups, to rotate the sample to repeatable positions. Figure 5-5: Repeatable positioning using sample cups and rings Thermo Scientific NIR Module User Guide...
  • Page 24 Powder Sample cup USING THE UNIVERSAL TABLET HOLDER The universal tablet holder can be used along with the sample accessory holder to position round tablets of many sizes and thicknesses on the Integrating Sphere. NIR Module User Guide Thermo Scientific...
  • Page 25 1. Align the notch with the pin. Notch Universal tablet pin holder Sample accessory To adjust the iris ❖ 1. Use your finger to gently turn the black ring to open the iris. Iris adjustment Iris Thermo Scientific NIR Module User Guide...
  • Page 26 Tablet Iris adjustment Height adjustment 5. Gently turn the black ring to close the iris around the tablet. NOTICE Do not overtighten the iris or you may damage it. Iris Tablet Iris adjustment ring NIR Module User Guide Thermo Scientific...
  • Page 27 The ports are compatible with fiber optic sampling accessories that use various sampling techniques and have standard SMA connectors, including the optional Thermo Scientific SabIR diffuse reflection probe. Thermo Scientific...
  • Page 28 Figure 5-1: NIR fiber optic sampling area features Fiber optic Touch Point Fiber optic ports SabIR Probe (optional) The fiber optic sampling area includes these features: NIR Module User Guide Thermo Scientific...
  • Page 29 The Touch Point LED shows the status of the NIR Module. Using the optional SabIR Probe The fiber optic sampling area is optimized for use with the Thermo Scientific SabIR diffuse reflection probe to provide easy, remote sampling of solids and powders.
  • Page 30 Electrical connector. Attaches to the electrical port on the NIR Module and is the power source to the probe. LED indicators. Three LEDs on the probe handle tell you the probe status. The LED states are described below. NIR Module User Guide Thermo Scientific...
  • Page 31 To attach the strain relief mechanism to the NIR Module ❖ 1. Align the two pegs and the center thumbscrew on the end of the strain relief mechanism with the holes below the fiber optic connectors. Thermo Scientific NIR Module User Guide...
  • Page 32 Do not use the probe in an explosive environment. Save all protective caps so they can be put back on the probe shaft and cable connectors and the fiber optic ports when they are not being used. NIR Module User Guide Thermo Scientific...
  • Page 33 3. Remove the cable cover from the strain relief mechanism by loosening the two thumbscrews. Cable cover Thumbscrews (2) 4. Remove the sheath from the SabIR Probe tip and insert the probe into the holster. The probe is in position when you hear it “click” into place. Thermo Scientific NIR Module User Guide...
  • Page 34 Hand-tighten the connectors until you feel a small amount of resistance, i.e., until they are finger- tight. Attach the cables to the correct ports to achieve consistent, repeatable results. Do not discard the protective caps; replace them when the ports are not in use. NIR Module User Guide Thermo Scientific...
  • Page 35 8. Gently maneuver the cables so the silver ring fits in the groove in the strain relief mechanism (see the previous image). 9. Replace the strain relief cover and secure it with the thumbscrews. Make sure the silver ring is completely hidden by the cover. Thermo Scientific NIR Module User Guide...
  • Page 36 Do not allow hard materials (i.e., glass, metal, ceramic, etc.) to contact the sapphire sampling window. Do not use the probe by itself to measure liquids. When sampling liquids, use the transflectance adapter. Refer to the "Sampling accessories for the SabIR Probe" section for more information. NIR Module User Guide Thermo Scientific...
  • Page 37 May be measured directly in small or large bins, or indirectly through clear packaging such as glass or plastic. May be measured directly or indirectly through a clear glass or plastic container. Thermo Scientific NIR Module User Guide...
  • Page 38 When sampling powders directly, make sure the sample is thick enough so the probe window is fully covered by the sample material but that enough of the sample material remains underneath the probe window to obtain an accurate reading. Figure 5-4: Sampling a powder with a diffuse reflection probe NIR Module User Guide Thermo Scientific...
  • Page 39 Your first experiment with the NIR SabIR Probe This section explains how to configure your Thermo Scientific optic SabIR Probe and demonstrates how to use it to analyze a sample. You can press the Touch Point to start the process and respond to prompts in the software while it is running, or simply use commands in the software to achieve the same result.
  • Page 40 (we use polymer beads for this demonstration) To measure a sample with the Thermo Scientific SabIR Probe ❖ 1. If you have not already done so, go to Configure > Sample Location > Fiber Optic SabIR Probe (or press the Fiber Optic Touch Point) to configure the instrument for fiber optic sampling.
  • Page 41 Point) to collect the sample data. Do not move the probe until the yellow light on the probe handle has turned off. Wait for the process to complete in the software and the spectrum will be collected. Thermo Scientific NIR Module User Guide...
  • Page 42 Figure 5-8: Report showing a diffuse reflection spectrum of polymer taken with the iS50 NIR Module and Thermo Scientific SabIR Probe 5. Clean the probe tip. Pour a small amount of cleaning solution (one part isopropyl alcohol with nine parts water) onto a soft cloth and gently rub the cloth on the probe shaft.
  • Page 43 Do not move the probe until the yellow light turns off. Sampling accessories for the SabIR Probe Optional Thermo Scientific accessories for the SabIR Probe are described briefly below. To order an accessory, contact our local sales or service representative or see our contact information at the beginning of this document.
  • Page 44 Table 5-3: Optional Thermo Scientific accessories for the SabIR Probe This accessory… Does this… SabIR Transflectance Adapter Slides on the SabIR Probe shaft SabIR Probe and transflectance adapter used to measure a liquid and allows you to sample analyze liquids...
  • Page 45 NOTICE Power off the instrument before you disconnect the SabIR Probe to avoid damaging the instrument’s electronics. Thermo Scientific NIR Module User Guide...
  • Page 46 To disconnect the Thermo Scientific SabIR Probe ❖ 1. Power off the instrument. NOTICE To avoid contaminating the internal reference, make sure the probe shaft and tip are clean before you insert the probe into the holster. 2. Insert the SabIR Probe into the holster to avoid causing strain on the fiber optic cables from the weight of the probe.
  • Page 47 NIR Module when they are not being used. Using fiber optic accessories from other manufacturers This section covers usage of your fiber optic accessories from other manufacturers besides Thermo Fisher. Thermo Scientific NIR Module User Guide...
  • Page 48 Tip It is important to consistently attach the fiber optic cables to the same ports when connecting sampling accessories. If there are differences between the fiber optic cables, and they are not always attached to the same ports, your data may be affected. NIR Module User Guide Thermo Scientific...
  • Page 49 "Your first experiment with the NIR SabIR Probe" section using the fiber optic Touch Point or the software to continue to the next step. Do not move the sampling accessory until the instrument has completed collecting data. Thermo Scientific NIR Module User Guide...
  • Page 50 [This page intentionally left blank]...
  • Page 51 Use a damp (not wet), soft cloth and a mild soap to clean the Integrating Sphere cover and other metal parts, including the sample accessory holder. Dry them with a clean cloth. Figure 6-1: Sample accessory holder Thermo Scientific NIR Module User Guide 51...
  • Page 52 Chemical wipes are usually not recommended for cleaning the Integrating Sphere sampling window as embedded clays can make these slightly abrasive. Use of soaps or other surfactants for cleaning the sampling window is discouraged as these can leave a residue bound to the window surface. NIR Module User Guide Thermo Scientific...
  • Page 53 Dry them with a clean cloth or allow it to air dry. Notice Do not use harsh solvents to clean the sample rings or you may damage them. Thermo Scientific NIR Module User Guide...
  • Page 54 Avoid eye hazard. Do not stare at the beam that exits the SabIR sampling window when the SabIR Probe is connected to the NIR Module and the spectrometer is powered on and the Fiber Optic beam path is selected. NIR Module User Guide Thermo Scientific...
  • Page 55 To clean the Thermo Scientific SabIR Probe ❖ 1. Remove the SabIR Probe from the holster. 2. Pour a small amount of the cleaning solution onto a soft cloth and use it to gently clean the probe shaft. Allow the shaft to air dry.
  • Page 56 If the background quality does not improve after thoroughly cleaning the Spectralon reference, the reference may need to be replaced. Contact our sales or service representative in your area for more information. NIR Module User Guide Thermo Scientific...