Thermo Scientific Nicolet NIR User manual

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

© 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.
The contents of this document are subject to change without notice. All technical information
in this document is for reference purposes only. System configurations and specifications in
this document supersede all previous information received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this document is complete,
accurate or error-free and assumes no responsibility and will not be liable for any errors,
omissions, damage, or loss that might result from any use of this document, even if the
information in the document is followed properly.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a
purchaser. This document shall in no way govern or modify any Terms and Conditions of
Sale, which Terms and Conditions of Sale shall govern all conflicting information between the
two documents.
For Research Use Only. This instrument or accessory is not a medical device and is not
intended to be used for the prevention, diagnosis, treatment, or cure of disease.
WARNING
Avoid an explosion or fire hazard.
This instrument or accessory is not designed for use in an explosive
atmosphere.

NIR Module
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
AThermo Scientific NIR Module (mounts on the left side of the spectrometer)
Thermo Scientific NIR Module User Guide 3
Chapter 1

NIR Module
BFiber optic sampling area (optional)
CIntegrating Sphere sampling area
DThermo Scientific SabIR Probe
The NIR Module provides these enhanced features:
lIntegrated design
lPush button configuration
lTwo sampling options: local (Integrating Sphere) and remote (fiber optic, optional)
lUp to two dedicated detectors
lAutomated internal reference
lStandards 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.
NOTICE
Be sure that all persons operating this system read the site and safety manual
first.
Table of contents
NIR Module 3
Table of contents 4
4 NIR Module User Guide Thermo Scientific

Conventions used in this manual 5
Operating precautions 7
Specifications 9
Compatible software 11
Integrating Sphere sampling 13
Fiber optic sampling 27
Using the optional SabIR Probe 29
Using fiber optic accessories from other manufacturers 47
Conventions used in this manual
DANGER
Avoid hazard. Indicates a hazardous situation which, if not avoided, will
result in serious injury or death.
WARNING
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 5
NIR Module

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.
6 NIR Module User Guide Thermo Scientific

Operating precautions
Read these operating precautions before using the NIR Module to avoid damaging your equipment.
Precautions for the Integrating Sphere:
lDo not pour liquids directly onto the Integrating Sphere.
lDo not use harsh detergents, chemicals, or abrasives to clean the surface of the Integrating
Sphere; these can damage the finish.
lMake sure your sample materials will not react with the sapphire crystal sampling window.
lUse solvents that do not react with sapphire crystals when cleaning the sampling window.
lAvoid scraping the sampling window with samples or sample containers.
lProtect 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:
lDo not drop the cables or knock them against a hard surface.
lDo not bend the cables or tightly coil them. The radius of the coils for the SabIR Probe should be
at least 30 cm. For other fiber optic accessories, refer to their user guides.
lAvoid twisting the cables when attaching the connectors to the ports.
lDo not over-tighten or use tools to tighten the connectors when attaching the cables to the ports.
lDo not touch the end of a fiber optic cable connector or use solvents to clean it.
lKeep a protective cap on each end of the cable when it is not in use.
Precautions for the SabIR Probe:
lDo not drop the probe or knock it against a hard surface.
lDo not subject the probe to rapid or excessive changes in temperature.
Thermo Scientific NIR Module User Guide 7
Chapter 2

lWipe off spilled chemicals immediately.
lMake sure your sample material will not react with the sapphire sampling window.
lDo not allow hard materials (glass, metal, ceramic, etc.) to contact the sampling window.
lUse solvents that do not react with sapphire crystals when cleaning the sampling window.
lPower off the instrument before connecting the SabIR Probe.
lMake sure the probe is clean before you insert it into the holster.
lDo not use the probe by itself to measure liquids. When sampling liquids, use the transflectance
adapter available for the probe.
8 NIR Module User Guide Thermo Scientific

Specifications
Feature Specification
Crystal material Sapphire
Internal reference Diffuse gold
Detector Dedicated Indium Gallium Arsenide (InGaAs)
Table 3-1: Specifications for the Integrating Sphere sampling area
Feature Specification
Fiber optic connectors SMA type
Detector InGaAs
Probe (optional) Thermo Scientific SabIR diffuse reflection probe
SabIR Probe internal reference Spectralon®
Table 3-2: Specifications for the optional fiber optic sampling area
The NIR Module spectral range is dependent upon the spectrometer configuration. The table below
shows the available configurations and their corresponding spectral ranges.
Thermo Scientific NIR Module User Guide 9
Chapter 3

Source Beamsplitter Detector Spectral range
White light CaF21InGaAs212,000 - 3,800 cm-1
White light XT-KBr3InGaAsb 11,000 - 3,800 cm-1
Table 3-3: NIR Module available spectral ranges
Note The NIR Module requires a CaF2 window installed in the external beam port on the left side
of the spectrometer.
1Calcium Fluoride
2Indium Gallium Arsenide
3Extended range Potassium Bromide
10 NIR Module User Guide Thermo Scientific

Compatible software
Software Use for...
OMNIC
Paradigm Collecting and analyzing NIR spectra.
TQ Analyst™
Creating quantitative and classification methods for use with OMNIC
Paradigm software or RESULT™ software. TQ Analyst software provides an
extensive suite of chemometrics features that you can use to identify raw
materials, perform quantitative analysis, and take spectral measurements.
For more information, refer to the help system in your TQ Analyst software.
RESULT
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
TQ Analyst methods to a RESULT workflow, please refer to your RESULT
Integration Software User Guide.
Note: Only methods created in TQ Analyst software version 8.4 or higher
can be transferred from OMNIC Paradigm to RESULT software.
Table 4-1: Software compatible with the NIR Module
Thermo Scientific NIR Module User Guide 11
Chapter 4

[This page intentionally left blank]

Integrating Sphere sampling
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
ATouch Point
BSample accessory holder
Thermo Scientific NIR Module User Guide 13
Chapter 5

CSampling window
DGold reference
lSampling window. Light from the spectrometer passes through this transparent sapphire window
to the sample.
CAUTION
Avoid eye hazard. 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.
lSample accessory holder. Mounts over the sampling window and holds Thermo Scientific
sample cups and tablet holder accessories.
lInternal 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.
lTouch Point. Automatically configures the spectrometer for Integrating Sphere sampling.
Samples compatible with the Integrating Sphere
The Integrating Sphere can be used to measure a wide variety of samples. Some examples are
provided below. Samples may be measured directly or in clear glass or plastic containers.
14 NIR Module User Guide Thermo Scientific

Types Characteristics Examples
Solids1Must have a rough or
diffuse surface
Coated textiles, paper, wood, polymers, and
plastics (especially plastics that have a
milky, opaque appearance)
Tablets2Must have a reflective
surface
White or colored doses of aspirin,
acetaminophen, or other drugs
Powders,
granules,
pellets3
Particles can be any size,
from fine to rough ground
up to large pellets
Polyethylene, excipients, flour
Liquids, gels4Must be a suspension or
opaque, or use a dip probe Milk, colloidal suspensions, dispersed solids
Table 5-1: Samples compatible with the Integrating Sphere
NOTICE
lDo not pour liquids directly onto the sampling area of the Integrating Sphere, especially the
area around the electrical connector for the Sample Spinner accessory.
lMake sure your sample materials and cleaning solvents will not react with the sapphire
sampling window. Refer to the "Cleaning the Integrating Sphere sampling window" section for
more information.
lAvoid scraping the sampling window with samples or sample containers.
1Use enough sample to completely cover the Integrating Sphere window. Place abrasive solids in a
clear glass or plastic container.
2May be placed directly on the Integrating Sphere window or in one of the tablet holder accessories.
3May 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. If possible, use a closed sample cup and
cover.
4Must be measured in clear glass, flat-bottom vials or clear plastic bags. Do not use Thermo
Scientific sample cups for liquids. If the liquid is clear, you can analyze it using the SabIR Probe with
a transflectance adapter. See "Using the optional SabIR Probe" and "Sampling accessories for the
SabIR Probe" for more information.
Thermo Scientific NIR Module User Guide 15

A variety of accessories are available for fast, reproducible sampling of tablets, pellets, powders, and
gels. For more information, please refer to the "Sampling accessories for the Integrating Sphere"
section.
Sample thickness, or the amount of sample, should be taken into consideration when using the
Integrating Sphere. If a solid sample is too thin or if there is not enough of a powder sample, you may
encounter problems with the spectra.
Your first experiment with the NIR Integrating Sphere
This section explains how to configure your NIR Integrating Sphere and demonstrates how to use the
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 software commands to achieve the same result.
SETTING UP THE INTEGRATING SPHERE
1. Start OMNIC Paradigm software. The software automatically loads the default, commonly used
settings, but you can create your own settings for your specific analysis needs.
If you need to create new settings, select New, then enter a name for the new collection settings.
Modify the settings as needed, then select Save. The new collection settings will be available for
selection in the Settings dropdown menu.
NOTICE
Make sure that Sampling accessory shows as NIR Integrating Sphere. If it does not, a different
instrument or accessory has been selected or the instrument is not installed properly.
2. Ensure that the Integrating Sphere is properly recognized. If not, go to Configure and select
Sample Location > NIR Integrating Sphere.
MEASURING A SAMPLE WITH THE INTEGRATING SPHERE
CAUTION
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
16 NIR Module User Guide Thermo Scientific

lIf the spectrometer has been powered off for more than 20 minutes, power it on and allow it to
stabilize for at least an hour.
lMake sure the sampling window is clean. Please refer to the "Cleaning the Integrating Sphere
sampling window" section for instructions and recommended solvents.
lHave your sample material on hand. For your first analysis, we recommend that you use a 325g
aspirin tablet.
NOTICE
lDo not pour liquids directly onto the sampling area of the Integrating Sphere, especially not the
area around the electrical connector for the sample spinner.
lMake sure your sample materials and cleaning solvents will not react with the sapphire window.
Refer to the "Cleaning the Integrating Sphere sampling window" section for more information.
lAvoid scraping the sampling window with samples or sample containers.
Figure 5-2: Solid sample ready for measurement with the Integrating Sphere
❖ 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 17

Figure 5-3: Integrating Sphere Touch Point
2. In the Dashboard, select Preview and Measure Background. This will create a new spectra tab
and open a background preview. Select Start Background Measurement to continue, then wait
for the process to complete. For more information, see "Collecting backgrounds with the
Integrating Sphere"
3. When the background measurement is done, place the sample in the center of the Integrating
Sphere sampling window. See "Samples compatible with the Integrating Sphere" for more
information.
4. After loading the sample, you can preview the sample and start the measurement. Select Start
Sample Measurement and wait for the process to complete.
Note If you do not enter a name for your measurement (when prompted or in the Dashboard
settings), the measurement name will automatically default to the current time and date. If
desired, you can rename the measurement later.
5. Remove the sample and clean the Integrating Sphere window.
Moisten a clean white paper napkin with isopropyl alcohol and use it to wipe the window. Dry the
window with a clean napkin.
Collecting backgrounds with the Integrating Sphere
A background is a reference spectrum that accounts for the unique optics of the sampling module and
the instrument. Each sample spectrum is ratioed against a background so that the final spectrum is
free of these features.
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.
18 NIR Module User Guide Thermo Scientific

When the internal reference is used, a gold mirror located underneath the Integrating Sphere window
closes during background collection, causing all of the light beam to be reflected back into the
Integrating Sphere. A typical background spectrum using the internal reference should resemble the
following.
Figure 5-4: Typical gold reference background spectrum taken with the Integrating Sphere
Tip Once a material is selected for a background reference, make sure to use the same material
each time you run your experiment.
Center the reference over the Integrating Sphere window and then respond to the prompt by
choosing OK or pressing the Integrating Sphere Touch Point. Do not move the reference until the
instrument has finished collecting the data.
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.
Thermo Scientific NIR Module User Guide 19

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
includes two sample cup rings: a
concentric (centering) ring and an
eccentric (offset) ring. The concentric
ring can be used to achieve consistent
positioning with the sample cups and the
sample accessory holder. The eccentric
ring works with the sample accessory
holder and the 5 cm sample cups to allow
sampling over a wider area. Refer to the
"Using the Sample Cups and Rings"
section for more information.
5 cm open sample cups
These come in packages of three sample
cups. Each cup has a 4.78 mm low OH
quartz window and can be used with the
sample accessory holder and sample
rings to measure powders. The open
sample cups are not recommended for
liquids and gels.
Table 5-2: Optional Thermo Scientific accessories for the Integrating Sphere
20 NIR Module User Guide Thermo Scientific