Theory and Utility of FT-NIR

Spectroscopy
An Introduction to
Nicolet Antaris FT-NIR Analyzers
2
The study of the interaction of
electromagnetic waves and matter
(Includes UV, visible, NIR, IR, Raman etc.)
MOLECULAR SPECTROSCOPY
MOLECULAR SPECTROSCOPY
3
Transitions Guide to the EM Spectrum
4
Radiowave NMR
Microwave Rotation of molecules, ESR
IR Fundamental molecular
vibrations
NIR Overtones and combinations of
Mid-IR
UV / Visible Electronic transitions, energy of
electrons raised to an excited
state
X-Ray Core electronic transitions in
atom
SPECTRAL ABSORPTIONS
SPECTRAL ABSORPTIONS
5
Vibrational Spectroscopic Regions
Mid-IR Spectral Region
4,000 - 400 cm
-1
(wavenumber)
2,500 - 25,000 nm (wavelength of light)
NIR Spectral Region
12,820 - 4,000 cm
-1
(wavenumber)
780 - 2,500 nm (wavelength of light)
To convert between nm and wavenumbers, simply take the inverse of the
number in nm and multiply by 10
7
. For example, to convert 1000 nm into
wavenumbers, take 1000, invert it and multiply by 10
7
. This gives 10,000 cm
-1
.
6
What Information Comes From the NIR ?
Mid-IR spectroscopy makes use of fundamental vibrations
Near-IR spectroscopy uses Overtones and Combination
Bands
Overtones and Combination Bands are types of vibrations
related to the fundamental vibrations seen in the Mid-IR
3000 cm
-1
6000 cm
-1
9000 cm
-1
12000 cm
-1
3
rd
Overtone
2
nd
Overtone
1
st
Overtone
Fundamental
Vibration
7
Nature of Overtones
Musical instruments like guitars and pianos make use of
fundamentals and overtones just like in spectroscopy
Overtones occur at about 2 and 3 times the frequency of
the fundamental vibration. Absorption intensity decreases
with increasing overtones
Band overlap increases with increasing overtones
8
Fundamental and Overtones A Quantum View Fundamental and Overtones A Quantum View
-500
1500
3500
5500
7500
9500
11500
13500
15500
17500
-0.75 -0.25 0.25 0.75
Di spl acement from Equi l i bri um Bond Length (Angstroms)
E
n
e
r
g
y

(
c
m
-
1
)
2
nd
Overtone v = 0 3
1
st
Overtone v = 0 2
Fundamental v = 0 1
=3
=2
=1
=0
9
Occur Close to
Integer Multiples Of Fundamental Bands.
For example: C-H Overtones Will Occur Near:
First Overtone
2960cm-1 (C-H Stretch) * 2 = 5920 cm
-1
3378 nm (C-H Stretch) * 1/2 = 1689 nm
Second Overtone
2960cm-1 (C-H Stretch) * 3 = 8880 cm
-1
3378 nm (C-H Stretch)* 1/3 = 1126 nm
Overtones
Overtones
10
Combination Bands
There are vibrations in the Near-IR other than overtones of
fundamentals. These are called Combination Bands.
COMBINATION Bands are the sum of several fundamentals
from different vibrations. One photon of light excites two
vibrations.
Combination Bands are typically found at lower energies than
overtones.
11
COMBINATION Bands Appear Near The Sum Of Two Or
Three FUNDAMENTAL Bands
For Example: A C-H Combination Will Occur Near
2960cm
-1
(C-H Stretch) + 1460cm
-1
(C-H Bend)
= 4420cm
-1
= 2262nm
Combination Bands
Combination Bands
12
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
1.1
1.2
A
b
s
o
r
b
a
n
c
e
4000 5000 6000 7000 8000 9000 10000 11000
Wavenumbers (cm
-1
)
Example NIR Spectrum
3
rd
Overtone
2
nd
Overtone
1
st
Overtone
Combination
13
NIR Characteristics
R-H groups have the strongest overtones due to hydrogens
degree of anharmonicity.
O-H, N-H, C-H, S-H bonds etc. strong NIR absorbers
H
2
and O
2
has no change in dipole moment, hence no NIR
absorption
R-H stretch or R-H stretch/bend form most NIR bands
14
Typical Absorptions
Frequency (cm
-1
)
14,300 11,111 9090 7692 6666 5882 5263 4761 4347 4000
700 900 1100 1300 1500 1700 1900 2100 2300 2500
Wavelength (nm)
15
Typical FT-NIR Measurements
Qualitative and quantitative analysis
Identification
Qualification and quantitation
Determination of change
Process monitoring and control
Can measure all sample types
Solids Softgels Films
Liquids Grains Suspensions
Tablets Pastes Syrups
Powders
16
Uses for NIR Spectroscopy
NIR spectroscopy finds widespread use as an excellent
QA/QC analysis tool in industrial applications:
Pharmaceutical
Chemical
Petrochemical
Food and Beverage
Polymer
Agriculture
NIR is a proven and popular technique because it is
rapid, accurate, non-destructive and can go through
glass and plastic to analyze the material inside
17
The FT-NIR Analysis Advantage
Large pathlength
Analyze more sample
Sampling in situ - through
glass, packaging materials
No sample preparation
required
Accurate and precise
Fast - Results in seconds
No Hazardous reagents
Non-destructive
Remote sampling capabilities
18
ASTM NIR Method E 1944
USP Chapter <1119>
European Pharmacopeia
(Ph.Eur.) 2.2.40 1997
(European Directorate for the Quality of Medicines)
Regulatory Acceptance for Near IR
19
Types of Near IR Instrumentation
Filter Wavelength filters used to select specific
wavelengths for analysis
Dispersive Gratings or prisms in combination with slits
Fourier Transform (Nicolet Antaris) Interferometer and
internal HeNe laser
20
A complete analyzer for the pharmaceutical, food &
beverage, chemical, and polymer industries
Nicolet Antaris
TM
FT-NIR Analyzer
21
FT-NIR Spectrometer
Detector
IR Source
Fixed mirror
x 0 -x
Beamsplitter
Laser diode
He-Ne laser
Sample
Moving mirror
22
Based on the same interferometer technology used for
mid-infrared and FT-Raman
Utilizes all the advantages of FT based instruments
Internal calibration is derived from He-Ne laser
(precision = 0.01 cm
-1
)
High resolution (4 cm
-1
)
All wavelengths are measured simultaneously
Higher energy throughput (larger apertures)
Excellent stability and reproducibility
Dynamic alignment
FT Technology for Near Infrared
23
Limitation of Old Dispersive Technology
Mechanically complicated
Grating filter and chopper
Poor resolution
16 cm
-1
or worse
Loss of spectral information
Wavelength inaccuracy
Due to prism or grating
Stray light effects
Difficult to transfer methods
due to wavelength inaccuracy
24
Traditional NIR Problems
Poor Wavelength Accuracy and Precision
FT-NIR advantage: data repeatability and method
reliability due to superior wavelength accuracy and
precision
Internal frequency reference with HeNe laser
7299.02500
Water Vapor Peak Bench S/N AFA00
7299.02100
Water Vapor Peak Bench S/N AFA0
1300
1350
1400
1450
1500
1550
1600
1650
S
i
n
g
l
e

B
e
a
m
7300
Wavenumbers (cm-1)
25
Traditional NIR Problems
Low Resolution
Information can be hidden at lower resolution
Need resolution to distinguish two closely related materials
FT-NIR advantage simpler models with fewer calibration
spectra possible with greater specificity
32 cm
-1
2 cm
-1
26
Traditional NIR Problems
Poor System Stability and Artifacts
Stability consistency
in measurement
results
Artifacts peaks or
other anomalies in the
spectrum not due to
the sample
Problems eliminated
with Nicolet Antaris
design
Sampling with an FT-NIR Analyzer
28
Measurement Techniques
Transmission
Liquid analysis
Quantitative
Qualitative
Films
Tablets
Semi-solids
Diffuse reflectance
Powders
Solids
Tablets
Fibers
Pastes
Suspensions with high
solids contents
Opaque semi-solids
29
Nicolet Antaris FT-NIR Analyzer - Overview
Fiber Optic
Integrating Sphere
Transmission
Method Development Sampling System (MDS) shown above
Dedicated configurations also available for specific analyses
30
MDS System
All techniques on one
system
Other Dedicated Systems
RTS System
Liquid Analyzer
Solid Sampling System
Tablet Analyzer
Fiber Optic System
Fiber Optic Multiplexer
Tablet Analyzer
Fiber Optic
Integrating Sphere
Transmission
Nicolet Antaris FT-NIR Analyzers
31
Nicolet Antaris Optical Bench
Rugged industrial platform
Dynamic Alignment
User-replaceable and pre-
aligned consumables
Modular design flexibility with
stability of fixed beampaths
Integrated validation (Built to
meet or exceed USP
monograph)
32
Near IR Quartz Halogen Source
External replacement with only 3
screws
No wires
Source change in seconds
Pinned-in-place aluminum
housing for lock-and-key fit
High throughput
33
Internal Referencing For All Collection Types
Protected internal reference material
simplifies background collection
Spectralon
Diffuse Gold Flag
Eliminates errors due damaged
reference materials
Collect backgrounds with sample
already loaded
Easy to use and automated
34
Reflection Sampling Integrating Sphere
Ideal collection
environment for diffusely
reflected light
High efficiency collection
Internal gold background
material
Sample simply needs to be
placed on the instrument
for data collection
35
Liquid Sampling - Transmission Compartment
Collect data on liquid, film or
paper
Accommodates vials, tubes,
cuvettes and card holders
Temperature control
Automatic internal background
position in transmission cell
Reproducible positioning
36
Fiber Optic Sampling SabIR and 3
rd
Party Probes
Transflectance or reflection
sampling
Fiber optic port uses standard
SMA connectors
Remote sampling capability for
At-line, near-line, on-line
Ideal for incoming raw material
identification and in-process
analysis
37
Solid Transmission Sampling Tablet Analyzer
Thick, opaque tablets give
quantitative results for
Content uniformity
API or excipient concentrations
Physical properties like hardness
Integrating sphere reflection data
gives tablet coating information
Collect reflection and transmission
data without removing the tablet
Dedicated softgel detector
Transmission
Diffuse Reflection
38
Antaris II
Method Development System - All sampling types for NIR
Transmission, tablets, softgels, diffuse reflection, fiber optics
Automatic sampling of solid dosage forms - 40 tablets at once
Simultaneous reflection and transmission measurement of tablets
Configurable base system with selection of sampling modules
39
Remote Sampling Fiber Optics Antaris MX
AntarisMX
Simultaneous multi-channel
measurement
Simultaneous internal backgrounds
No mechanical multiplexing
Dual trigger probe capability
Programmable analog/digital I/O
options with RESULT Interface
Spectral corrections adjust for fiber
optic differences
40
Analyzer performance verification
Traditionally done with probe
pulled off process
Internal reference channel can
qualify operation while probe is
inline
Traceable reference standards
for spectroscopic performance
checks according to USP
<1119>
41
Fiber optic probes
High quality probes with
proprietary window mounts in
custom configurations
Specialty probes
Fermentation dual mode
reflection and transmission
Retractable dryer probe with self
cleaning tip and wash chamber
42
High Throughput Sampling Autosampler RS
and Multipro Autosampler
Multiple samples with no operator
interaction
Eliminates sample-to-sample
operator error
Useful for analyzing tablets,
softgels, solids or powders in vials
Transfer already existing methods
for seamless scale-up
43
Heterogeneous Sampling Sample Spinners
Obtain spectra of heterogeneous
samples like
Polymer pellets Grains
Coarse powders Silage
Granular solids Corn
Crystalline materials
Eliminate the need to collect multiple
spectra on the same sample
44
Antaris EX: A complete process analyzer
Hazardous environments
Integrated computing
Integrated process
communications
Same sampling technology
and advantages as MX
Simultaneous measurements
with internal referencing and
qualification
Not a box that you have to put
inside of another box!
Complete new lineup of
probes
45
Hazardous environments
Three EX models:
EX-Z1 for Class I Division 1/Zone 1
Environments
EX-Z2 for Class I Division 2/Zone 2
Environments
EX-IP65 for
Enclosures are:
Hose washable, Stainless steel,
corrosion proof
Individually certified
Vortex cooling provides operating
temperature range of -20 to 40 C
Purge systems (different for each
environment) linked to power of
system
46
On Blender Analysis
47
Blending in Development Multiple sizes
Instrumentation must work with a wide range of blender sizes
Issues of scale with equipment size and weight
48
Monitoring the Blend with NIR
By scanning the sample (pharmaceutical powder blend)
through a window in the modified lid, the progression of mixing
and concentration of components can be measured
Data is triggered when bin is upside down (powder in contact
with sampling window)
Powered by rechargeable battery pack
Diffuse reflection sampling
Wireless communications to remote PC with RESULT
software for control/DAQ
Standard deviation measurement can be used to determine
when mix is fully achieved
49
The Spectroscopy Technology
Optical Bench Optical Bench
Optical Module Sub-Assembly Optical Module Sub-Assembly
Spectrometer Assembly Spectrometer Assembly
Source Semiconductor based NIR tunable laser
Not a light bulb/globar does not go out or fade
Rated for a 25 year lifetime (Telcordia Spec.)
Wavelength selection - High resolution (2 nm / 8cm-1)
Fabry-Perot tunable filter
Tuning range of hundreds of nm
Scans full range in tens of milliseconds
Insensitive to vibration
Internal Wavelength and Amplitude Reference
Ensures optimum wavelength calibration over
time
50
Instrumentation and Sampling Interface
Detector: Single element InGaAs photodiode
Optimized detector element sized to collect highest solid angle for
maximum efficiency
Baseline s/n of 0.0002
Wavelength ranges available
1350-1550 nm, 1550-1800 nm and
1800 1970 nm
Fast Scanning (~80 ms / scan)
Sample sensing area of 40 mm
(coincides with ~600 mg sample size)
Smaller spot size available (~10 mm) for
intra-dosage uniformity investigation
Wireless communication (~15 meters)
Battery operation (2 3 hours)
Fiber Optic Input
From Spectrometer
Collimating Lens
Assembly
Sapphire
Window
Assembly
Detector Lens
Assembly
Extended Range High
Performance Single
Element InGaAs Detector
Diffuse Gold Reference
Validation Sample Position
Fiber Optic Input
From Spectrometer
Collimating Lens
Assembly
Sapphire
Window
Assembly
Detector Lens
Assembly
Extended Range High
Performance Single
Element InGaAs Detector
Fiber Optic Input
From Spectrometer
Collimating Lens
Assembly
Sapphire
Window
Assembly
Detector Lens
Assembly
Extended Range High
Performance Single
Element InGaAs Detector
Diffuse Gold Reference
Validation Sample Position
Diffusely reflected energy
51
Summary
On Blender Real-time analysis provides a rapid and calibration
free method of getting blend information and performing
experiments
With the correct type of optical interface the instrumentation
can be quickly moved between blender sizes and types for
scale-up development
Instrumentation is process friendly
Small
Lightweight
Easy to set up
Long battery life
Robust
RESULT Software Suite for the
Nicolet Antaris Analyzer
53
RESULT Software Suite for Near IR
RESULT is the software package made for collecting
Near IR data with the Nicolet Antaris Analyzer
Provides
Real time data acquisition
Sample prediction using developed models
Chemometrics tools for method development
Full suite of compliance tools
54
RESULT Provides Tools for all Users
RESULT Operation allows users with no science training
to run routine analyses
Minimal training time and one-click use
RESULT Integration provides the tools to develop
workflows with integrated SOPs for workroom deployment
Design simple workflows like Raw Material ID
Create sophisticated experiments with logical gates, delays and
repeats
55
RESULT Provides Tools for all Users
TQ Analyst is a powerful chemometrics package
Easy to use
Fully integrated with spectral collection software
No secondary programs needed
Administrator Mode
Creates new users
Maintains system integrity
Sets workflow access privileges for all users
56
ValPro Instrument Qualification Platform
Design qualification (DQ)
documentation provided
Detailed Installation Qualification (IQ)
procedure
USP-based Operational Qualification
(OQ) tests provided
Traceable & serialized internal validation
wheel
Tools for Performance Qualification
(PQ)
57
21 CFR Part 11 Compliance with RESULT
Full Suite of Part 11 Tools
Full operation auditing
SOP enforcement and
automation
Digital signatures
Security, access control, and
privilege and workflow
assignment
58
Software Validation
TQ Analyst Algorithms
Fully Documented
Externally reproduced for verification in Excel
Demonstrates internal validation
59
Process Analytical Technology (PAT)
PAT is a systemfor designing, analyzing, and
controlling manufacturing through timely
measurements (i.e., during processing) of critical
quality and performance attributes of raw and in-
process materials and processes with the goal of
ensuring final product quality
Seamless migration of FT-NIR technology from the
laboratory to the manufacturing floor
60
Time for a Paradigm Shift - PAT
In-process testing that currently exists in
pharmaceutical manufacturing consists of
Physical measurements
Results from samples sent to the lab while processes
were halted or continued blindly
Current testing is not real-time, nor whole batch
Non-optimal conditions can still occur (over-
blending for example)
Testing and waiting for results is costly
61
Typical FT-NIR PAT Applications
Blending and mixing
Reaction monitoring
Fermentation
Drying
Post tableting tests
62
Traditionally, optimal mixing time
was determined during process
development and scale-up
Avoids problems of incomplete or
over-blending (de-blending)
Improves efficiency of production
processes and equipment usage
Assures product uniformity
Goals
Establish adequacy of mixing
Eliminate thieving/process
interference
Eliminate error and recipe
approach
Accurate endpoint determination
NIR in the Manufacturing Process
63
Integration with manufacturing systems
RESULT OPC (OLE for
Process Control) Server
facilitates powerful
communication with
manufacturing systems
Send and receive
commands
automatically
Trigger runs, endpoints,
valves, etc.
64
Communication is Essential to Process Control
Communication system must be able to bridge
Disparate technologies from various manufacturers
Compatibility with both high and low level interfaces
Opposing computer platforms
Geographic separation from target
Interface with business software to expand the process
control loop
Data communication architecture must be inclusive,
not exclusive
Existing and modern facilities
65
OPC in Process: Dryer Monitor
Analyzer Data
Processing
OPC Server
Output
SCADA or DCS
OPC Input
Dryer Data
Collection
66
Typical FT-NIR Pharmaceutical Applications
Raw Material ID
Moisture Content
Content Uniformity
Tablet API
Coating Thickness
Process Analytical Technology (PAT)
67
Pharmaceutical Application: Raw material ID
Apply NIR to inspect incoming
raw materials quickly at the
loading dock
Equip the receiving area with
an NIR to be used by
technicians who are not
trained as scientists
Confirm the identity of each
container of material that is
received, without lab wet
chemistry techniques that are
time-consuming and
expensive
68
Library Raw Material Samples
One lot each of the following substances was provided
for the construction of the raw material library
d-Glucose
d-Fructose
Sucrose
d-Mannitol
d-Sorbitol
-d-Lactose Monohydrate
Acetylsalicylic Acid
Acetaminophen
L-Ascorbic Acid
Citric Acid
69
Validation Samples
d-Glucose - Second lot from a different manufacturer
d-Fructose - Second lot from a different manufacturer
Acetaminophen - Second lot from a different manufacturer
Salicylic Acid - Degradation product of Acetylsalicylic Acid
2-acetamidophenol - Constitutional isomer of acetaminophen
-d-Lactose anhydrous - Dehydrated form of library material
Black items are positive challenge samples (Should Pass)
Red items are negative challenge samples (Should Fail)
70
External Challenge Validation Results
Compound Score Result
Glucose (Lot #2) 99.9 Pass
Fructose (Lot #2) 98.0 Pass
Acetaminophen (Lot #2) 100.0 Pass
Salicylic Acid 55.2 Fail
2-Acetamidophenol 19.3 Fail
Lactose Anhydrous 68.9 Fail
71
FT-NIR Success stories
Customer had a plant with diverse array of incoming raw
materials that needed to be classified accurately.
Implemented NIR testing for over 200 materials
Based upon technician time savings alone, paid back the
investment in about 7 months
Needed to identify a small number of materials at very
high volume composing the bulk of their test load
Implemented 100 % inspection for ID and qualification
Dropped their testing time on each incoming shipment of
raw material by 68 %
72
Lyophilized Material Analysis
Lyophilized materials are an excellent application for
analysis by NIR
Packaging cannot be opened without corrupting the
product inside
Can apply to food,
pharmaceutical, fine
chemical or biotech
industries
73
Current Testing for Lyophilized Products
Current testing methods like Karl Fisher titration, LOD
or GC
cumbersome, time consuming and costly
destructive
NIR does not need solvents or carrier gases
NIR calibrations for lyophilized materials have been
shown to be as accurate as the reference method
Other components can also be measured using the
same NIR spectrum (Buffer, API, Cryoprotectant)
74
Case Study For Lyophilized Sample Analysis
Primary component of interest in any lyophilized materials is
moisture (0.5% - 2.0% typically)
Sample is Thrombin, a topical coagulant used in the medical
and dental fields
Thrombin loses its efficacy if exposed to high heat or wet
conditions. Current application will look at moisture and
potency in Thrombin
75
Moisture First Overtone Region
76
Close-up of First Moisture Overtone Region
77
Calibration Curve for Moisture
78
Calibration for Potency
Quantification of Active
Pharmaceutical Ingredient (API)
in Tablets
80
Show Concentration Differences in Tablets
Distinguish different clinical tablet formulations by amount
of active ingredient
Finished product is a tablet and manufacturing protocols
need independent verification of amount of active
ingredient
Understand the differences between transmission and
reflection analysis of tablets
81
Reflectance Spectra for Clinical Tablets
0.25
0.35
0.45
0.55
0.65
0.75
L
o
g
(
1
/
R
)
5000 6000 7000 8000 9000
-2.2
-1.8
-1.4
-1.0
-0.6
-0.2
0.2
0.6
1.0
1.4
L
o
g
(
1
/
R
)
5400 5500 5600 5700 5800 5900 6000
Wavenumbers (cm
-1
)
Expanded
Second
Derivative
82
Tablet Reflection Results
0
10
20
30
0 10 20 30
Label Claim (Rel. Units)
N
I
R

C
a
l
c
u
l
a
t
e
d

(
R
e
l
.

U
n
i
t
s
)
Calibration
Validation
R = 0.99742
RMSEC = 0.606
83
Tablet Transmission Results
0
10
20
30
0 10 20 30
Label Claim (Rel. Units)
N
I
R

C
a
l
c
u
l
a
t
e
d

(
R
e
l
.

U
n
i
t
s
)
Calibration
Validation
R = 0.99965
RMSEC = 0.0561
84
API Quantification Can Also Be Done Using
Qualitative Methodology - Discriminant Analysis
PC1
P
C
3
0
1
2
4
12
16
24
Principal component scores plot reveals quantitative method
may not be necessary
The required information is obtained with excellent results
using qualitative analysis (Discriminant)
85
NIR in Pharmaceuticals - Summary
NIR has proven useful in the following applications:
Raw Material ID
Raw Materials - Particle Size
Analysis of Parenteral Drugs - Lyophilized Materials
Quantification of API in Tablets
Blend Homogeneity
Lactose Polymorph Screening
SoftGel Analysis
Enzyme Activity
86
Near IR in the Chemical Industry
Near IR analysis has proven worth across the chemical
industry
Fine chemicals
Polymers
Petrochemicals
Paints, coatings and adhesives
Soaps and cleaners
Synthetic materials
At-line, near-line and on-line
Polymerization Monitoring:
Acid Value and Hydroxide
88
HoVal Analysis in NIR - Purpose
HoVal is short for Hydroxyl Value, an important metric in
polymerization reactions
Measures both starting materials (Acid and OH)
simultaneously from the same spectra
Condensation polymers (Polyesters) show decrease in
acid and alcohol concentration with time
Use NIR to monitor this decrease will show when
polymerization is finished
89
Experimental
Samples were placed into 6 mm disposable vials
Analysis using Nicolet Antaris Transmission module
90
Spectral Data for HoVal Analysis
0.4
0.8
1.2
1.6
2.0
2.4
2.8
5000 6000 7000 8000 9000 10000
Wavenumbers (cm
-1
)
91
Hydroxyl Value Correlation
Acid Number Correlation
NIR Replaces Two Wet Chemical Methods
Plasticizer Content in PVC
93
Plasticizer Content in PVC
Plasticizers are common additives to polymers.
The quantity of plasticizer determines the properties of
the polymer.
The plasticizer contents of polymers differ depending
on the application.
Primary methods often involve tedious and time-
consuming extractions.
94
Samples
Samples of polyvinyl chloride (PVC) with varying
amounts of dioctylphthalate (DOP) as plasticizer
Three types of samples:
Opaque PVC plates with 5 - 50% DOP
Transparent PVC plates with 5 - 50% DOP
PVC Films with 9 - 40% DOP
95
FT-NIR Measurements
As is measurements (no sample
preparation or modification).
Data collected from 4,000 cm
-1
to
10,000 cm
-1
4 cm
-1
resolution.
90 scans
One (1) minute collection time.
All measurements done on
Integrating Sphere
96
Non-Transparent Plates
97
Calibration Parameters
MSC
4125-3946
4296-4263
Norris 5,5
2
nd
Derivative
3 Films
MSC
4772-4520
5935-5322
Norris 5,5
2
nd
Derivative
4 Transparent
MSC 8982-3920 Norris 9,0
2
nd
Derivative
4 Opaque
Pathlength
Region
(cm
-1
)
Smoothing
Data
Format
Factors
98
Non-Transparent Plates
99
Calibration Results
0.407 0.999 0.174 0.999 Films
1.45 0.996 0.591 0.999
Transparent
Plates
1.49 0.995 0.375 0.999 Opaque
RMSECV Corr. Coeff. RMSEC Corr. Coeff.
Cross Validation Calibration
100
Conclusions on NIR of Plasticizer Content
Additives such as plasticizers can be measured in
various forms of plastic materials
These materials can be finished or unfinished
Measurements can be in-process or QC
measurements
The analyses can be done easily, rapidly and non-
destructively
Current methodology for extraction of matrix
elements in polymers is extremely time consuming
101
Near IR and Food
Near IR analysis of food and food products has found
extensive use in all segments of the industry
Processed foods
Beverages
Grain
Fruit
Meat
Common components like protein, moisture, ash, starch
and fat are measured simultaneously without destroying
the sample
102
FT-NIR As A Process Analytic in Food
Develop methods for any type of food product
High resolution advantage of FT technology keeps
number of standards low
Many different sampling accessories for food products
Sample spinner
SabIR Fiber Optic Probe
Cheese and Viscous Liquid Samplers
Softgel detector (Gum)
OPC Output for analyzer incorporation into Process
Control Systems
103
NIR Analysis in the Food Industry
Moisture and Protein in Barley
Viscous Liquid Analysis
Oil in Rice Powder
Amylose Levels in Corn
Multi-component Analysis of Wine
Fat and Dry Matter in Cheese
Discrimination of J ellybeans
Choline Chloride Levels in Silage
104
FT-NIR Nicolet Antaris Spectrometer Platform
RESULT Analyzer Software Platform
TQ Analyst Chemometric Software Platform
ValPro Validation/Qualification Platform
Support Pyramid of Supportproducts and services
Sales
Applications
Service
Customer
Nicolet Antaris Product Line Complete Solution
105
The FT-NIR Advantage
The Bottom Line:
Save Time and Money.
Use FT-NIR to its maximum capability.