of 64
8/10/2019 NIR Applications Phk [Compatibility Mode]
1/64
FT-NIR Spectroscopy for Food and
Subtitle
8/10/2019 NIR Applications Phk [Compatibility Mode]
2/64
If youre going to need a year to train a horseto locate contriband pick a musical one
We all know that exceptionally well-
designed, manufactured, delivered and
(necessarily) make great Analytical
Methods
8/10/2019 NIR Applications Phk [Compatibility Mode]
3/64
If youre going to need a year to train a horseto locate contriband pick a musical one
We all know that exceptionally well-
designed, manufactured, delivered and
(necessarily) make great Analytical
Methods
Clever p e o p l e make great AnalyticalMethods
A clever person can make sound and
successful methods with the simplest of
tools or lar el incom lete tools for the
job, by learning to apply them to the
greatest advantage
8/10/2019 NIR Applications Phk [Compatibility Mode]
4/64
If youre going to need a year to train a dogto locate contriband pick a musical one
However, given the chance, clever
p e o p l e will pick exceptionally well, ,
installed i n st r u m e n t s because it will
make their job a whole lot easier!
Clever people together with greatinstruments can make exceptional
na y ca e o s
8/10/2019 NIR Applications Phk [Compatibility Mode]
5/64
If youre going to need a year to train a dogto locate contriband pick one with a greatgreat nose
8/10/2019 NIR Applications Phk [Compatibility Mode]
6/64
If youre going to need a year to train a dogto locate contriband pick one with a greatgreat nose - an an inc ination to use it!
8/10/2019 NIR Applications Phk [Compatibility Mode]
7/64
The MPA Multi-Purpose Analyzer
multiple measurement accessories for
different sampling techniques: er p c ro es
Integrating Sphere
automated Sample Wheel
Sam le Rotator
software controlled measurement
accessories selection full line of sampling accessories and
options
8/10/2019 NIR Applications Phk [Compatibility Mode]
8/64
Unique Features of Bruker MPA
Custom-made Instrument:
Each customer buys exactly the instrument that matches his application.There is no need to purchase anything that is not wanted or needed.
MPA fully equippedMPA basic configuration
8/10/2019 NIR Applications Phk [Compatibility Mode]
9/64
Maximum Flexibility:
Fi er OpticProbes
Samp eCompartment
IntegratingExternalp ereransm ss on
8/10/2019 NIR Applications Phk [Compatibility Mode]
10/64
The MATRIX-F
compact Process Spectrometer
with RocksolidTM
Interferometer mo u ar es gn
robust, rugged and waterproof
high long-run Stability
high measuring Accuracy
unrestricted Method Transfer possible
all Components in 19 Geometry
8/10/2019 NIR Applications Phk [Compatibility Mode]
11/64
The MATRIX-I
based on the optical module of MATRIX-F
robust, rugged and waterproof fixed, gold-coated Integration Sphere
vibration and temperature insensitive
at-line and in-line Installation
used for heterogeneous and coarse-
gra ne ma er a s
much better light efficiency than probes
8/10/2019 NIR Applications Phk [Compatibility Mode]
12/64
Calibration Transfer:
e except ona per ormance o t e nstrument ensures a smootcalibration transfer not only to other MPA instruments but also to the
MATRIXprocess spectrometers.
8/10/2019 NIR Applications Phk [Compatibility Mode]
13/64
Calibration Transfer:
e except ona per ormance o t e nstrument ensures a smootcalibration transfer not only to other MPA instruments but also to the
MATRIXprocess spectrometers.
One Calibration
8/10/2019 NIR Applications Phk [Compatibility Mode]
14/64
Spectrometer Calibration at H20 Vapor Bands
. 025
a
resolution = 25 cm -1.
020
eams
pectr
resolution = 2 cm -1. 015S
ing
le
. 010
target: 7.306,74 cm-1
7800 7600 7400 7200 7000 6800 6600Wavenumber / cm-1
8/10/2019 NIR Applications Phk [Compatibility Mode]
15/64
OPUS spectroscopy software:
ex e so tware, opt m ze orthe special demands of the FT-
NIR technology.
Various software acka es enable a ualitative as well as a uantitativeanalysis of the samples.
Modular design, additional software packages can seamlessly beintegrated in the existing OPUS suite.
The customer is able to use all software functions without any restriction.
8/10/2019 NIR Applications Phk [Compatibility Mode]
16/64
OPUS/IDENT:
Identification software with factor
analysis as well as with the Euclidian
distance calculations
Hierarchical libraries offer the
identification of samples in multiple
lar e libraries ossible >2 000
samples)
g egree o separa on, even
with very similar products!
8/10/2019 NIR Applications Phk [Compatibility Mode]
17/64
OPUS/QUANT:
Quantification software with
automated calibration function:
user defined optimization regions
functions
even inex erienced users to
generate calibrations at a push of a
button
the process of time consuming
method generation and optimization
8/10/2019 NIR Applications Phk [Compatibility Mode]
18/64
OPUS/LAB:
Easy-to-use interface for the
even inex erienced users can
use OPUS/LAB
pre-defined order of events
no mistakes
freely configurable to the needs
of your users
8/10/2019 NIR Applications Phk [Compatibility Mode]
19/64
Full GMP and 21 CFR part 11 compliance:
OPUS in combination with the MPAcomplies with regulations issued
by ISO, ASTM, FDA and USP.
full GMP capabilities like multiplesecurity levels, non-editable data files
.
electronic records and signatures.
Bruker Optics is a certified supplier and
companies.
8/10/2019 NIR Applications Phk [Compatibility Mode]
20/64
Training:
free training after the installationof the instrument
erman ra n ng courses w ce a year
English training course once a year
personal in-house training at thecustomers facility on demand
every instrument is supported by anexpert who is available for you when
8/10/2019 NIR Applications Phk [Compatibility Mode]
21/64
Areas of Application
ChemistryPetro & Polymer
Food & FeedPharma
Cosmetics
8/10/2019 NIR Applications Phk [Compatibility Mode]
22/64
Sample Forms
Powders Tablets Seeds Paper Liquids
Granulates Phials Foils
Coatings
Emulsions
Pastes Resins
8/10/2019 NIR Applications Phk [Compatibility Mode]
23/64
Limits of NIR Technology
Detection of C-H-, N-H-, O-H- and C=O-vibrations
(mainly examination of organic compounds).
The NIR-technique is currently not suitable for trace analysis
Usually in the percentage range, sometimes down to 0.1%
Examination of complex mixtures (> 5-7 components)usually demands a higher calibration effort.
NIR is often not suitable for the identification of unknown samples.
8/10/2019 NIR Applications Phk [Compatibility Mode]
24/64
-
How does a quantitative analysis work?
Analysis
rr
r
rrr
rr
r
r
rr
Factors
1
2
Spectra
0.6
0.
7
0.8
0.9
Units
Reference
rrrr
rr
r
r
r
r3
4
5500060007000800090001000011000Wavenumber cm-1
0.2
0.3
0.4
0.5
Absorbance
Building up acalibration curve
Calculation of thespectral parameters
Measurement of spectra
with known concentration
- uantif in unknown Sam les
1.5 % Comp. A
34 % Comp. B
62% Comp. C
e erm na on oconcentration(s)
na ys s ounknown spectrum
Measurement ofunknown samples
8/10/2019 NIR Applications Phk [Compatibility Mode]
25/64
Pharmaceutical A lications
Subtitle
8/10/2019 NIR Applications Phk [Compatibility Mode]
26/64
NIR Applications of Pharmaceuticals
Substance Identification in the Receipt of Goods
Quantification of active Materials (APIs)
auxiliary Materials
Fi ers
in Powders, Capsules, Tablets or Vials
Drying Processes
Blending Solvent Recovery
...
8/10/2019 NIR Applications Phk [Compatibility Mode]
27/64
Calibration of active Ingredients
Calibration of
Ibuprofene Paracetamol
in Tablets
measued with
External Transmission Unit
8/10/2019 NIR Applications Phk [Compatibility Mode]
28/64
Ibuprofen in Tablets
73
69
e/%
65
67
NIRva
lu
61
63
59
59 61 63 65 67 69 71 73
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
29/64
Paracetamol in Tablets
94
90
e/%
86
88
NIRva
lu
82
84
80
80 82 84 86 88 90 92 94
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
30/64
Calibration of active Ingredients
Results:
R2
Range RMSECV
Ibuprofene 99.41 60 - 74% 0.3%
Paracetamol 99.46 81 - 94% 0.3%
8/10/2019 NIR Applications Phk [Compatibility Mode]
31/64
Ingredients of Vitamin Solutions
Calibration of
Methanol Water
Sugar
in Vitamin B2 Solution
measured with
1 mm Transmission Probe
8/10/2019 NIR Applications Phk [Compatibility Mode]
32/64
Methanol in Vitamin B2 Solution
59
53
55
e/%
49
51
NIRvalu
45
47
43
43 45 47 49 51 53 55 57 59
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
33/64
Water in Vitamin B2 Solution
50
45
e/%
40
NIRvalu
35
30
30 35 40 45 50
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
34/64
Sugar in Vitamin B2 Solution
10
8e/%
7
NIRvalu
6
5
5 6 7 8 9 10
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
35/64
Calibration of Ingredients
Results:
R2
Range RMSEP
Methanol 99.87 44 - 59% 0.18%
Water 99.92 31 - 49% 0.15%
Sugar 99.33 5.5 - 9.6% 0.11%
8/10/2019 NIR Applications Phk [Compatibility Mode]
36/64
Cosmetics A lications
Subtitle
8/10/2019 NIR Applications Phk [Compatibility Mode]
37/64
Calibration of Shampoo
Calibration of
Wash Active Substancesin Shampoo
measured at 30
oC
in the Sample Compartment
8/10/2019 NIR Applications Phk [Compatibility Mode]
38/64
Wash Active Substances in Shampoo
265
kg
225
245
/mmol
185
205
IRvalu
145
165
145 165 185 205 225 245 265 285
reference value / mmol/kg
8/10/2019 NIR Applications Phk [Compatibility Mode]
39/64
Calibration of Shampoo
Results:
R
2
Range RMSECV
WAS 99.43 150-282 2.5 [mmol/kg]
8/10/2019 NIR Applications Phk [Compatibility Mode]
40/64
Surfactant in aqueous Solution
80
lue/%
20NIR
v
0
0 20 40 60 80
reference value / %
8/10/2019 NIR Applications Phk [Compatibility Mode]
41/64
Food & Feed A lications
Subtitle
8/10/2019 NIR Applications Phk [Compatibility Mode]
42/64
M P A with Integrating Sphere and Sample Compartment
8/10/2019 NIR Applications Phk [Compatibility Mode]
43/64
M P A Int.Sphere/Sample Comp./Transmission Unit
8/10/2019 NIR Applications Phk [Compatibility Mode]
44/64
MPA with Petri Dish Rotator
8/10/2019 NIR Applications Phk [Compatibility Mode]
45/64
MPA with Rotator and Transmission Unit
8/10/2019 NIR Applications Phk [Compatibility Mode]
46/64
Starter Calibrationsfor Food Aapplications
8/10/2019 NIR Applications Phk [Compatibility Mode]
47/64
Food Starter Calibrations for turn-keysolutions
Multiple Packages
- -
B-MEA-M Meat
- -
Single Package
PriceList
B-DAI-S Dairy
B-MEA-S Meat
B-OIL-S Edible Oils
8/10/2019 NIR Applications Phk [Compatibility Mode]
48/64
NIR Starter Calibration Packages: Dairy
Liquid Milk and Milk Products in Transmission (1mm flow cell)
aw an w o e m
Whey
Whey protein concentrate
Lactose Concentrate
Brine (Mozzarella)
Cleaning and disinfection solvents
8/10/2019 NIR Applications Phk [Compatibility Mode]
49/64
Starter Calibration for Milk Powder
Calibration of
Protein
Ash
Lactose
in Milk Powder
Measured on the sphere with IN311/C
+ IN311-S
8/10/2019 NIR Applications Phk [Compatibility Mode]
50/64
Measurements of melamine in milk powder
.8
0.9
1.2
1.4
Pure milk powder (red)
0.7
nits
0.6
0.8
1.0
0.5
0.6
Absorb
ance
400050006000700080009000100001100012000
0.2
0.4
0
.3
0.4
Pure melamine (blue)
400050006000700080009000100001100012000
Wavenumber cm-1
50
8/10/2019 NIR Applications Phk [Compatibility Mode]
51/64
Measurements of melamine in milk powder
1.4
0
. .
.0
1.2
s
0.3
5
0.
-1
0.8
1.
Absorbance
Unit
0.3
0
0.4
0.6 60006200640066006800700072000.2
5
400050006000700080009000100001100012000
Wavenumber cm-1
0.2
51
8/10/2019 NIR Applications Phk [Compatibility Mode]
52/64
Measurements of melamine in milk powder
NIR-Calibration melamine in milk powder3.2
2.2
2.7
ion/%
= .
RMSECV= 0.057
1.2
1.7
R-Predict
0.7
NI
.
0.2 0.7 1.2 1.7 2.2 2.7 3.2
True Value / %
52
8/10/2019 NIR Applications Phk [Compatibility Mode]
53/64
Measurements of melamine in liquid milk
0
3.5
Liquid milk of 1.5% and 3.5% of fat with admixture of melamine from 0.05% - 0.3%
.0
2.5
3.
1.0
1.5
2
Absorbanc
e
Units
0.0
0.5
400050006000700080009000100001100012000
Wavenumber cm-1
-0.5
53
8/10/2019 NIR Applications Phk [Compatibility Mode]
54/64
Measurements of melamine in liquid milk
NIR-Calibration melamine in liquid milk
0.31
0.26
ion/%
= .
RMSECV= 0.0042
0.16
.
R-Predict
0.11NI
.
0.06 0.11 0.16 0.21 0.26 0.31
True Value / %
54
8/10/2019 NIR Applications Phk [Compatibility Mode]
55/64
Measurement: Oils in Sample Compartment
Instrumentation:
- u urpose na yzer
- MPA-C: Sample Compartment
-
- IN601C08: Insert for Vials
-
Resolution: 8 cm-1
No. of Scans: 32 Scans Temperature: 50
oC
8/10/2019 NIR Applications Phk [Compatibility Mode]
56/64
External Heating Block
8/10/2019 NIR Applications Phk [Compatibility Mode]
57/64
Universal Calibrations
Property Data Set Performance
Name Unit n Min Max Rank R2
SEPIodine Value IV 607 0.1 133 9 99.9 0.56
Trans Fatty Acids % 532 0.0 60.4 13 99.9 0.61
TFA low range % 243 0.0 2.6 11 93.2 0.17
These calibrations should normally work without further adaptation
with common customer samples.
8/10/2019 NIR Applications Phk [Compatibility Mode]
58/64
8/10/2019 NIR Applications Phk [Compatibility Mode]
59/64
Measurement: Trans content in Fats/Oils
trans content wasexpressed as %FA
Universal trans contentcalibration covers transcontent from 0 to 56 FA
8/10/2019 NIR Applications Phk [Compatibility Mode]
60/64
Starter Calibrations
Property Data Set Performance
Name Unit n Min Max Rank R2
SEPAnisidine Value AnV 270 0 195 14 95.2 8.64
Free Fatty Acids % 790 0.1 6.0 9 99.8 0.09
C16:0 (Palmitic Acid) % 608 4 16 10 95.2 0.50
C18:0 (Stearic Acid) % 660 1.8 92 15 98.2 1.41
C18:0 (Stearic Acid) % 482 1.6 6 14 94.3 0.25
C18:1 (Oleic Acid) % 800 0 85 17 99.9 0.65
C18:2 (Linoleic Acid) % 597 2.5 67 12 99.9 0.20
C18:3 (Linolenic Acid) % 412 0 9.5 10 99.3 0.20
Customer samples should be added for optimum performance.
8/10/2019 NIR Applications Phk [Compatibility Mode]
61/64
8/10/2019 NIR Applications Phk [Compatibility Mode]
62/64
Mix of ingredients for animal feed
Energy Source
wheat, barley, corn, oats, fat, molassesetc.
Vegetable Proteinsoya, rapesee s, sun ower see s etc.
Crude Fibers , , .
Minerals
, , ,etc.
8/10/2019 NIR Applications Phk [Compatibility Mode]
63/64
Task of a Nutritionist: the best feed inconstant quality for the lowest price
For the optimization of the mixed feed the Nutritionist needs to know
the property values of the raw materials for:protein, moisture (dry matter), fiber, oil (fat) and ash.
For this task classical wet chemistry is slow and expensive!
This is a NIR task!
8/10/2019 NIR Applications Phk [Compatibility Mode]
64/64
www.brukeroptics.com