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������������� ������������������������������ ���
NIR Seminar – Campden – October 14th 2009
Giovanni Campolongo
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I Italian Near Infrared Symphosium
2004 Lodi
• Limo •Fiber Optic on the Ham•Baby Food Plasmon (Heinz Group)
12th International Conference on Near-infrared Spectroscopy
2005 Auckland
• On-line Maillard reaction monitoring for food additives production (caramel)
NIR Seminar – Campden – October 14th 2009
VII CISETA2005 Cernobbio
• Ice cream mixtures
II Italian Near Infrared Symphosium2006
Ferrara
• Inorganic Integrators• Pectin• SO2• Proteolysis index in P.D.O. Cheeses
13th International Conference on Near-infrared Spectroscopy
2007 Umeå
• Cous cous• Vanilline• Wheat flour rheological paramethers
III Italian Near Infrared Symphosium
2008 Lazise
• On-line polymerization process• Licopen content in Tomatoes• Barilla FT-NIR Network for Flour monitoring
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Lab & R&D
• University• State agencies for control• Private Labs
NIR Seminar – Campden – October 14th 2009
INDUSTRY
NEEDS • Raw material control • Monitoring production processes• Fianl products quality control
TECHNOLOGY PRODUCERS
• Analytical systems
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NIR Seminar – Campden – October 14th 2009
# �������
BARILLA
DIFFERENT PRODUCTS
DIFFERENT RAW MATERIALS
Wheat Flours
Industrialbread
Quality 1
Quality 2
NIR Seminar – Campden – October 14th 2009
BARILLA BAKERY
bread
Snacks
Quality 2
Quality 3
Quality 4
Quality 5
Quality up to 12
Cakes
( ) � ���� ����* ������ � �" % ����������� ��'
TARGET: Assess Quality of incoming Wheat Flour batches
• Identify Parameters to check• Identify an Analytical System able to perform quickly such
checking• Define sampling methods• Collect samples and verify
12 different Wheat Flour Qualities considered
NIR Seminar – Campden – October 14th 2009
12 different Wheat Flour Qualities considered 8 – 100 – 106 – 108 – 110 – 114 – 120 – 141 – 144 – 158 – 164 –
175…
• Samples collected starting from March 2007
• Samples collected from different suppliers all over Italy
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CHEMICAL PARAMETERS REFERENCE METHODS
Farinographic
RHEOLOGICAL PARAMETERS
MoistureProtein ContentFalling Number
UNI reference Methods
Brabender Farinograph
NIR Seminar – Campden – October 14th 2009
Farinographic Baking Absorption
Alveographic WP/L
Chopin Alveograph
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• 3 Sub-samples for each incoming Flour Batch (3 spectra measurment for each batch)• Each spectra as average of 64 scans having a rotating petri dish system• Samples Temperature: 20 � 5�C
Spectra acquisition by diffuse reflectance using an FT-NIR SpectrometerWavelenght range 4000 – 10000 cm-1
NIR Seminar – Campden – October 14th 2009
Data management• NIRCal Chemometeric software to develop quantitative calibration models with Evaluation Set Tecnique
Chemometric software NIRCal 5.0
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PEDRIGNANO BARILLA HEADQUARTER
MASTER UNIT Spectra Libraries Main Database
Sample’s spectraMeasurements
reports
CalibrationsSupport
NIR Seminar – Campden – October 14th 2009
Spectra Libraries Main DatabaseDevelopement of Quantitative Calibrations
ClientPicenengo
(Local database)
ClientNovara(Local database) ClientCastiglione
(Local database)ClientRubbiano
(Local database)
ClientAscoli(Local database)
ClientMelfi(Local database)
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Checking incoming raw materials chemical composition Why NIR?
NIR Seminar – Campden – October 14th 2009
Checking chemical composition of finished formulations
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Raw materials are paid according to chemical
composition
Example: Soy Flour according to protein content
Check every batch supplied means to pay the correct price
NIR Seminar – Campden – October 14th 2009
To produce according to the declared composition by having
an instant monitoringFinished products
PlusTo obtain the same chemical
composition they could be used different and new raw materials,
maybe cheaper
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NIR Seminar – Campden – October 14th 2009
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WHEAT GLUTEN AND MELAMINE
NIR Seminar – Campden – October 14th 2009
� ����� ��������� �� ���� ��.�� �������.���������� ���� �� ����������� ������* � �������� �
Original SpectraAll Spectra
Wavelengths
Re
fle
cta
nc
e
40005000600070008000900010000
0.2
0.4
0.6
0.8
NIR
Ca
l : C
usc
us
_S
em
ola
to_
Fa
rin
a_
Um
idita
23
11
06
26
/04
/20
07
10
.34
.43
Ad
min
istr
ato
r
Calibration SpectraValidation Spectra
����
NIR Seminar – Campden – October 14th 2009
Samples Method Range R C-set/V-set SEP SEC
Umidità 210 PLS 10.00 - 16.09 0.99 / 0.99 0.12 0.12
Proteine 144 PLS 11.02 - 14.03 0.97 / 0.97 0.16 0.15
Ceneri 210 PLS 0.69 - 1.35 0.94 / 0.93 0.20 0.22
Wavelengths40005000600070008000900010000
NIR
Ca
l : C
usc
us
_S
em
ola
to_
Fa
rin
a_
Um
idita
23
11
06
26
/04
/20
07
10
.34
.43
Ad
min
istr
ato
r
����
/ �������� ��������� �� �� ��'
Original Property / Predicted PropertyAll Spectra
True Property lactose
Pre
dic
ted
Pro
per
ty la
cto
se
3.0 3.5 4.0 4.5 5.0 5.53.5
4.0
4.5
5.0
5.5
NIR
Cal
: L
atti
ero
case
ario
onl
ine-
aggi
orna
to2.
nir
Lact
ose
- im
plem
ente
d2
23/0
5/20
05 9
.25.
39 c
amg
V a l i d a t i o n S p e c tra f (x )= 0 .6 5 2 3 x + 1 . 7 1 3 7 r= 0 .7 7 7 8 3 8C a l i b ra t i o n S p e c t ra f (x )= 0 . 6 5 5 3 x + 1 .6 9 9 3 r= 0 . 8 0 9 5 2 3
P ro p e rty Ou t l i e r S p e c t raV a l i d a t i o n S p e c traC a l i b ra t i o n S p e c t ra
����
Original Property / Predicted PropertyAll Spectra
True Property fat A
Pre
dict
ed
Pro
pert
y fa
t A
0 2 4 6
0
2
4
6
NIR
Cal
: L
atti
ero
case
ario
onl
ine-
aggi
orna
to2.
nir
Fat
A -
im
plem
ente
d2
23/0
5/20
05 8
.49.
25 c
amg
V a l i d a t i o n S p e c t ra f (x )= 0 . 9 8 8 9 x + 0 . 0 2 4 3 r= 0 .9 9 3 5 8 8Ca l i b ra t i o n S p e c t ra f (x )= 0 . 9 8 8 2 x + 0 .0 3 6 3 r= 0 . 9 9 4 1 0 7V a l i d a t i o n S p e c t raCa l i b ra t i o n S p e c t ra
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NIR Seminar – Campden – October 14th 2009
Property(%)
C-Set SEE (SEC)
V-Set SEE (SEP)
C-Set Regression Coefficient
V-Set Regression Coefficient
Fat 0.17 0.17 0.99 0.99
Protein 0.17 0.16 0.85 0.86
Dry matter 0.31 0.31 0.98 0.98
Lactose 0.16 0.17 0.81 0.78
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Olive grinding Olive paste
Gramolatura
EstrazioneHusk WaterExtractionExtraction
Solvent
NIR Seminar – Campden – October 14th 2009
EstrazioneHusk
Separation
Filtration
Extraction
Extra-virgin Olive oil
Husk Oil
Water
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Spectrometer FT-NIR NIRFlex N500
• 2 acquisition each sample• Every acquisition is tha average of 64 scan with rotating petri dish (total time< 1min)• Temperature 20°C
NIR Seminar – Campden – October 14th 2009
PARAMETR Standard errorSEP [%] Range samples
Moisture 0.8 34.8 – 71.7 240
Fat 0.9 15.8 – 31.1 200
Samples from different geograpical regions 2007
Predicted Property vs. Original PropertyAll Spectra
Original Property Moisture
Pre
dic
ted
Pro
pe
rty
Mo
istu
re
40 50 60 7030
40
50
60
70
NIR
Ca
l :
co
py
of
Mo
istu
re,
0.8
05
0,
1-6
./6
, 4
60
0-1
00
00
. 2
4/0
4/2
00
8 1
4.3
0.4
9 A
dm
inis
tra
tor
Calibration Spectra f(x)=0.9873x+0.7300 r=0.9937 r2=0.9873 Sdev(x-y)=0.8254 BIAS(x-y)= 0 range(x)=34.8 .. 71.73 n=342Validation Spectra f(x)=1.0032x-0.1181 r=0.9920 r2=0.9840 Sdev(x-y)=0.8178 BIAS(x-y)=-0.0647 range(x)=41.8 .. 70.97 n=133Calibration SpectraValidation Spectra
����
Predicted Property vs. Original PropertyAll Spectra
Original Property Moisture
Pre
dic
ted
Pro
pe
rty
Mo
istu
re
40 50 60 7030
40
50
60
70
NIR
Ca
l :
co
py
of
Mo
istu
re,
0.8
05
0,
1-6
./6
, 4
60
0-1
00
00
. 2
4/0
4/2
00
8 1
4.3
0.4
9 A
dm
inis
tra
tor
Calibration Spectra f(x)=0.9873x+0.7300 r=0.9937 r2=0.9873 Sdev(x-y)=0.8254 BIAS(x-y)= 0 range(x)=34.8 .. 71.73 n=342Validation Spectra f(x)=1.0032x-0.1181 r=0.9920 r2=0.9840 Sdev(x-y)=0.8178 BIAS(x-y)=-0.0647 range(x)=41.8 .. 70.97 n=133Calibration SpectraValidation Spectra
����
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Diffuse reflectance
NIR Seminar – Campden – October 14th 2009
PARAMETR Standard error SEP [%] Range Samples
Moisture 1.8 24.7 – 70.7 170
Fat 0.3 1.0 – 12.1 180
Samples from different geograpical regions
Predicted Property vs. Original PropertyAll Spectra
Original Property Fat
Pre
dic
ted
Pro
pe
rty
Fa
t
0 2 4 6 8 10 120
2
4
6
8
10
12
NIR
Ca
l :
SV
_G
ras
si_
23
04
08
23
/04
/20
08
12
.17
.37
Ad
min
istr
ato
rCalibration Spectra f(x)=0.9621x+0.1741 r=0.9809 r2=0.9621 Sdev(x-y)=0.3836 BIAS(x-y)= 0 range(x)= 1 .. 12.1 n=296Validation Spectra f(x)=0.9366x+0.3830 r=0.9729 r2=0.9466 Sdev(x-y)=0.3878 BIAS(x-y)=-0.09397 range(x)= 2 .. 8.7 n=84Calibration SpectraValidation Spectra
����
Predicted Property vs. Original PropertyAll Spectra
Original Property Fat
Pre
dic
ted
Pro
pe
rty
Fa
t
0 2 4 6 8 10 120
2
4
6
8
10
12
NIR
Ca
l :
SV
_G
ras
si_
23
04
08
23
/04
/20
08
12
.17
.37
Ad
min
istr
ato
rCalibration Spectra f(x)=0.9621x+0.1741 r=0.9809 r2=0.9621 Sdev(x-y)=0.3836 BIAS(x-y)= 0 range(x)= 1 .. 12.1 n=296Validation Spectra f(x)=0.9366x+0.3830 r=0.9729 r2=0.9466 Sdev(x-y)=0.3878 BIAS(x-y)=-0.09397 range(x)= 2 .. 8.7 n=84Calibration SpectraValidation Spectra
����
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Olive Grinding Olive paste
Gramolatura
Fat content= 23.4%
NIR Seminar – Campden – October 14th 2009
EstrazioneHusk WaterExtractionFat content= 6.6%
Constant monitoring of plant yield
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Customization according to the needs of a specific industry
General calibrations developed thanks to refernce lab
NIR Seminar – Campden – October 14th 2009
PARAMETRO Standard error SEP [%] Range samples
Moisture 1.3 41.8 – 67.7 120
Fat 0.18 2.00 – 8.00 120
Predicted Property vs. Original PropertyAll Spectra
Original Property Grassi
Pre
dict
ed P
rope
rty
Gra
ssi
2 4 6 8
2
4
6
8
NIR
Cal
: Sa
nse
verg
ini g
rass
i <8%
121
207
13/0
5/20
08 1
3.56
.38
Adm
inis
trato
r
Calibration Spectra f(x)=0.9709x+0.1267 r=0.9854 r2=0.9709 Sdev(x-y)=0.2279 BIAS(x-y)= 0 range(x)= 2 .. 8 n=181Validation Spectra f(x)=0.9876x+0.0605 r=0.9915 r2=0.9831 Sdev(x-y)=0.1812 BIAS(x-y)=-0.006503 range(x)=2.49 .. 7.4 n=58
User SpectraCalibration SpectraValidation Spectra
����
Predicted Property vs. Original PropertyAll Spectra
Original Property Grassi
Pre
dict
ed P
rope
rty
Gra
ssi
2 4 6 8
2
4
6
8
NIR
Cal
: Sa
nse
verg
ini g
rass
i <8%
121
207
13/0
5/20
08 1
3.56
.38
Adm
inis
trato
r
Calibration Spectra f(x)=0.9709x+0.1267 r=0.9854 r2=0.9709 Sdev(x-y)=0.2279 BIAS(x-y)= 0 range(x)= 2 .. 8 n=181Validation Spectra f(x)=0.9876x+0.0605 r=0.9915 r2=0.9831 Sdev(x-y)=0.1812 BIAS(x-y)=-0.006503 range(x)=2.49 .. 7.4 n=58
User SpectraCalibration SpectraValidation Spectra
����
Higher measurement accuracy
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Transflettanza
� ������� * ��
NIR Seminar – Campden – October 14th 2009
Spettrometro FT-NIR NIRLab N200
PARAMETER Standard error SEP [%] Range Samples
Solvents 0.06 0.02 – 1.03 105
Impurities 0.07 0.02 – 0.99 105
Original Property / Predicted PropertyAll Spectra
True Property Impurezze
Pre
dict
ed P
rope
rty
Impu
rezz
e
0.00 0.25 0.50 0.75 1.00 1.25
0.00
0.25
0.50
0.75
1.00
NIR
Cal
: ad
riaol
i - b
asse
con
cent
razi
on im
pure
zze.
nir i
mpu
rezz
e ba
sse
conc
netra
zion
i 030
7 13
/05/
2008
14.
25.5
6 ca
mg
Validation Spectra f(x)=0.9227x+0.0132 r=0.975797Calibration Spectra f(x)=0.9487x+0.0229 r=0.974025
Property Outlier SpectraValidation SpectraCalibration SpectraUser Spectra
����
Original Property / Predicted PropertyAll Spectra
True Property Impurezze
Pre
dict
ed P
rope
rty
Impu
rezz
e
0.00 0.25 0.50 0.75 1.00 1.25
0.00
0.25
0.50
0.75
1.00
NIR
Cal
: ad
riaol
i - b
asse
con
cent
razi
on im
pure
zze.
nir i
mpu
rezz
e ba
sse
conc
netra
zion
i 030
7 13
/05/
2008
14.
25.5
6 ca
mg
Validation Spectra f(x)=0.9227x+0.0132 r=0.975797Calibration Spectra f(x)=0.9487x+0.0229 r=0.974025
Property Outlier SpectraValidation SpectraCalibration SpectraUser Spectra
����
�2� 2/ 2�( ) ����$ ��� �������$�����
Istituto ZooprofilatticoSperimentale della Lombardia
e dell'Emilia Romagna
Spettrometro FT-NIR NIRFlex N-500 with
liquids cell
NIR Seminar – Campden – October 14th 2009
Parameters for olive oil quality evaluation
Acidity
Perox.
K232 K270�K
Tocoferol
Polifenol
Predicted Property vs. Original PropertyAll Spectra
Original Property Olio Acidità
Pre
dict
ed P
rope
rty
Olio
Aci
dità
-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
NIR
Cal
: O
lio o
liva
acid
ità 1
4/05
/200
8 9.
25.4
3 Ad
min
istra
tor
Calibration Spectra f(x)=0.9959x+0.0021 r=0.9979 r2=0.9959 Sdev(x-y)=0.0400 BIAS(x-y)= 0 range(x)=0.01 .. 2.97 n=150Validation Spectra f(x)=0.9887x+0.0130 r=0.9918 r2=0.9837 Sdev(x-y)=0.0452 BIAS(x-y)=-0.008318 range(x)=0.04 .. 1.795 n=75Calibration SpectraValidation Spectra
����
Predicted Property vs. Original PropertyAll Spectra
Original Property Olio Acidità
Pre
dict
ed P
rope
rty
Olio
Aci
dità
-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
NIR
Cal
: O
lio o
liva
acid
ità 1
4/05
/200
8 9.
25.4
3 Ad
min
istra
tor
Calibration Spectra f(x)=0.9959x+0.0021 r=0.9979 r2=0.9959 Sdev(x-y)=0.0400 BIAS(x-y)= 0 range(x)=0.01 .. 2.97 n=150Validation Spectra f(x)=0.9887x+0.0130 r=0.9918 r2=0.9837 Sdev(x-y)=0.0452 BIAS(x-y)=-0.008318 range(x)=0.04 .. 1.795 n=75Calibration SpectraValidation Spectra
����
Standard
�2� 2/ 2�( ) ����$ ��� �������$�����
Istituto ZooprofilatticoSperimentale della Lombardia
e dell'Emilia Romagna
NIR Seminar – Campden – October 14th 2009
Scores vs. ScoresAll Spectra
PC 1
PC
2
-0.2 -0.1 -0.0 0.1 0.2 0.3
-0.2
-0.1
-0.0
0.1
0.2
NIR
Cal
: O
lio o
liva
acid
ità 1
4/05
/200
8 9.
26.5
7 A
dmin
istra
tor
����
Scores vs. ScoresAll Spectra
PC 1
PC
2
-0.2 -0.1 -0.0 0.1 0.2 0.3
-0.2
-0.1
-0.0
0.1
0.2
NIR
Cal
: O
lio o
liva
acid
ità 1
4/05
/200
8 9.
26.5
7 A
dmin
istra
tor
����
PARAMETErStandard
error SEP
Coeff.Reg. R Range N. Spt.
(cp. X 3)
Acidity 0.04 0.99 0.01 – 2.97 228
Peroxidenum.
1.8 0.97 3.2 – 43.4 237
K232 0.12 0.98 1.99 – 5.27 237
k270 0.06 0.97 0.08 – 1.49 237
�K 0.0002 0.95 0.0001 –0.0555 237
Polifenol 30 0.70 139 - 300 93
Tocoferol 21 0.95 7 - 282 129
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Dipartimento di Chimica e tecnologie Farmaceutiche e Alimentari - Univ. Genova
Application of differenet multi-variate analysis techiniques to identify the
geograpichal origin of olive oil
NIR Seminar – Campden – October 14th 2009
200 samples of olive oil
“Near infrared spectroscopy and classmodelling techniques for thegeographical authentication of Ligurianextra virgin olive oil”Journal of Near Infrared Spectroscopy,November 2007
���� ���! �! �� ����3, ���& �4 ��� � 5�� �! ��������
Dry matterProteinFatParameter
NIR Seminar – Campden – October 14th 2009
15.40 –19.906.80 – 8.401.40 – 5.30Range
0.290.210.16SEP
0.330.210.16SEC
0.950.790.98R V-SET
0.960.860.99R C-Set
ncl, logdg1, nleds2Pretreatments
PLSPLSPLSMethod
968897Samples
matterProteinFatParameter
Pretreated spectra for “fat content”
���� ���! �! � ������� ��� � �! ������������� ��� ��� ���
Predicted Property vs. Original PropertyAll Spectra
Pre
dict
ed P
rope
rty
Fat
0 2 4 60
2
4
6
NIR
Cal
: cop
y of
Om
ogen
izza
to g
rass
i 0409
06 0
7/0
9/20
06
17.2
3.0
4 bu
chi
Calibration Spectra f(x)=0.9887x+0.0421 r=0.994357 range(x)=1.32-6.32 Sdev(x-y)=0.1134 BIAS(x-y)=1.35324e-014 n=108Validation Spectra f(x)=0.9756x+0.0837 r=0.994598 range(x)=1.49-6.03 Sdev(x-y)=0.1096 BIAS(x-y)=0.00778034 n=52Calibration SpectraValidation Spectra
NIR Seminar – Campden – October 14th 2009
Original Property Fat0 2 4 6
NIR
Cal
: cop
y of
Om
ogen
izza
to g
rass
i 0409
06 0
7/0
9/20
06
17.2
3.0
4 bu
chi
����
Measurement time = 15 sec.
ParameterFat[%]
Samples 80
Regres. C-set 0.99
Regres. V-set 0.99
SEE C-set 0.11
SEP V-set 0.11
Range 1.32 - 6.32
6 ��' ��������� ��� ����� �+ ����� ����� � � � ������7������ � ���
NIR Seminar – Campden – October 14th 2009
PARAMETHERSProteinTotal fat
Saturated Fatty AcidUnsaturated Fatty Acid
Lactose
���������� ��������� �����) �� ��������������� �� �* ����� ���� � �����2� 2/ 2���������� �����8
NIR Seminar – Campden – October 14th 2009
Predicted Property vs. Original PropertyUser Spectra
Original Property proteolisi TCA 12%
Pre
dic
ted
Pro
per
ty p
rote
olis
i TC
A 1
2%
0 5 10 15 20 25
0
5
10
15
20
NIR
Cal
: R
agu
san
o p
rote
olis
i TC
A 1
2% 2
5060
6 1
3/05
/200
7 2
3.5
8.49
Adm
inis
trat
orCalibration Spectra f(x)=0.9300x+0.5710 r=0.964346 range(x)=0.43-22.04 Sdev(x-y)=1.1547 BIAS(x-y)=8.82512e-015 n=1207Validation Spectra f(x)=0.9472x+0.4541 r=0.963864 range(x)=0.63-20.02 Sdev(x-y)=1.1610 BIAS(x-y)=-0.0124169 n=597
User SpectraCalibration SpectraValidation SpectraProperty Outlier Spectra
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Predicted Property vs. Original PropertyUser Spectra
Original Property proteolisi TCA 12%
Pre
dic
ted
Pro
per
ty p
rote
olis
i TC
A 1
2%
0 5 10 15 20 25
0
5
10
15
20
NIR
Cal
: R
agu
san
o p
rote
olis
i TC
A 1
2% 2
5060
6 1
3/05
/200
7 2
3.5
8.49
Adm
inis
trat
orCalibration Spectra f(x)=0.9300x+0.5710 r=0.964346 range(x)=0.43-22.04 Sdev(x-y)=1.1547 BIAS(x-y)=8.82512e-015 n=1207Validation Spectra f(x)=0.9472x+0.4541 r=0.963864 range(x)=0.63-20.02 Sdev(x-y)=1.1610 BIAS(x-y)=-0.0124169 n=597
User SpectraCalibration SpectraValidation SpectraProperty Outlier Spectra
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Parameter Samples Samples Range [%] R SEC/SEP [%]
Soluble nitrogen TCA 12%
C-set 408 0.11 – 6.84 0.96 0.31
V-Set 197 0.12 – 15.67 0.96 0.30
Proteolysis index TCA
12%
C-set 408 0.43 – 22.04 0.96 1.15
V-Set 197 0.63 – 20.02 0.96 1.16
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NIR Seminar – Campden – October 14th 2009
Only one calibration for each parameter
Fat SEP = 0.4%
Protein SEP = 0.10%
Dry matterSEP = 0.41%
DIFFERENT MIXTURES OF ICE-CREAMS
MilkVanillaCremeYogurt
Chcocolate
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Spectrometer FT-NIR Buchi Nirflex N-419
Original Property / Predicted PropertyAll Spectra
Pre
dic
ted
Pro
per
ty A
sso
rbim
ento
a 6
10
0.50
NIR
Cal
: B
S11
1.n
ir A
SB
610
- n
ew 0
.92*
11/
03/2
005
14.4
8.06
ferg
Validation Spectra f(x)=0.9389x+0.0292 r=0.968015Calibration Spectra f(x)=0.9497x+0.0220 r=0.974547Validation SpectraCalibration Spectra
Original Property / Predicted PropertyAll Spectra
Pre
dic
ted
Pro
per
ty A
sso
rbim
ento
a 6
10
0.50
NIR
Cal
: B
S11
1.n
ir A
SB
610
- n
ew 0
.92*
11/
03/2
005
14.4
8.06
ferg
Validation Spectra f(x)=0.9389x+0.0292 r=0.968015Calibration Spectra f(x)=0.9497x+0.0220 r=0.974547Validation SpectraCalibration Spectra
NIR Seminar – Campden – October 14th 2009
True Property Assorbimento a 610
Pre
dic
ted
Pro
per
ty A
sso
rbim
ento
a 6
10
0.30 0.35 0.40 0.45 0.500.25
0.30
0.35
0.40
0.45
NIR
Cal
: B
S11
1.n
ir A
SB
610
- n
ew 0
.92*
11/
03/2
005
14.4
8.06
ferg
���� True Property Assorbimento a 610
Pre
dic
ted
Pro
per
ty A
sso
rbim
ento
a 6
10
0.30 0.35 0.40 0.45 0.500.25
0.30
0.35
0.40
0.45
NIR
Cal
: B
S11
1.n
ir A
SB
610
- n
ew 0
.92*
11/
03/2
005
14.4
8.06
ferg
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Original SpectraAll Spectra
1/cm
Tra
nsm
itta
nce
5000 6000 7000 8000 9000
0.0
0.2
0.4
0.6
0.8
NIR
Cal
: B
S11
1.ni
r A
SB
610
- n
ew
0.9
2*
11
/03
/200
5 1
4.5
1.44
ferg
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Original SpectraAll Spectra
1/cm
Tra
nsm
itta
nce
5000 6000 7000 8000 9000
0.0
0.2
0.4
0.6
0.8
NIR
Cal
: B
S11
1.ni
r A
SB
610
- n
ew
0.9
2*
11
/03
/200
5 1
4.5
1.44
ferg
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Reading at a 610nm0.009/0.0100.97/0.960.275-0.52765610nm
0.04/0.040.98/0.970.325-1.133125550mn
SEC/ SEPR C-Set/ V-SetRangeSamplesParameter
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Parameter NaHCO3 CaHPO4 CaCO3 MgO
Camp. 107 107 64 64
R C-Set 0.99 0.99 0.99 0.99
R V-Set 0.99 0.98 0.99 0.99
SEC 1.1 1.7 2.0 1.8
SEP 1.0 1.8 2.0 1.8
San Marco Plant
State University of Parma
Büchi
+
+
NIR Seminar – Campden – October 14th 2009
NaHCo3 CaHPO4
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PARAMETERS
Moisture
CONSTANT MONITORING OF PRODUCTION
PROCESS
Analisi dei campioni tal
NIR Seminar – Campden – October 14th 2009
MoistureEsterification ratioGalacturonic Acid content
OPTIMIZATION OF PRODUCTION
PROCESS
PRODUCT WITH HIGHER QUALITY
Analisi dei campioni tal quali in uscita dalla produzione
Una sola scansione tutti i parametri contemporanemante
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NIR Seminar – Campden – October 14th 2009
PARAMETER SEC SEP C-set r V-set r C-slope V-slope
Moisture 1.09 1.08 0.88 0.78 0.77 0.78
NaCl 0.29 0.50 0.92 0.62 0.85 0.71
Protein 0.99 0.97 0.82 0.80 0.68 0.66
N(TCA) 0.70 0.70 0.83 0.78 0.68 0.67
Proteolysisindex
1.88 1.82 0.79 0.72 0.63 0.62
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NIR Seminar – Campden – October 14th 2009
Regressione con set di validazione.
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NIR Seminar – Campden – October 14th 2009
P r e d ic te d P r o p e r ty v s . O r ig in a l P r o p e r tyAl l S p e c tra
O r ig in a l P ro pe r ty V a n illina
Pred
icte
d Pr
oper
ty V
anill
ina
1 2 3
1
2
3
NIRC
al :
Vani
llina
quan
titativ
a 14
0507
14/
05/2
007
22.4
6.48 A
dmin
istra
tor
C a l i b ra t i o n S p e c t ra f (x )= 0 .9 5 5 6 x+ 0 .0 7 6 5 r= 0 .9 7 7 5 3 5 ra n g e (x)= 0 .6 4 2 -3 .4 9 9 S d e v(x-y)= 0 .1 1 7 7 B IA S (x-y)= -1 .6 3 5 7 3 e -0 1 5 n = 6 0V a l i d a t i o n S p e c t ra f (x )= 0 .9 5 2 7 x+ 0 .0 9 3 1 r= 0 .9 5 8 9 9 1 ra n g e (x)= 0 .7 7 6 -2 .3 4 5 S d e v(x-y)= 0 .1 2 1 1 B IA S (x-y)= -0 .0 1 3 4 0 9 5 n = 2 8C a l i b ra t i o n S p e c t raV a l i d a t i o n S p e c t ra
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P r e d ic te d P r o p e r ty v s . O r ig in a l P r o p e r tyAl l S p e c tra
O r ig in a l P ro pe r ty V a n illina
Pred
icte
d Pr
oper
ty V
anill
ina
1 2 3
1
2
3
NIRC
al :
Vani
llina
quan
titativ
a 14
0507
14/
05/2
007
22.4
6.48 A
dmin
istra
tor
C a l i b ra t i o n S p e c t ra f (x )= 0 .9 5 5 6 x+ 0 .0 7 6 5 r= 0 .9 7 7 5 3 5 ra n g e (x)= 0 .6 4 2 -3 .4 9 9 S d e v(x-y)= 0 .1 1 7 7 B IA S (x-y)= -1 .6 3 5 7 3 e -0 1 5 n = 6 0V a l i d a t i o n S p e c t ra f (x )= 0 .9 5 2 7 x+ 0 .0 9 3 1 r= 0 .9 5 8 9 9 1 ra n g e (x)= 0 .7 7 6 -2 .3 4 5 S d e v(x-y)= 0 .1 2 1 1 B IA S (x-y)= -0 .0 1 3 4 0 9 5 n = 2 8C a l i b ra t i o n S p e c t raV a l i d a t i o n S p e c t ra
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0.120.970.64 – 3.5060C-setVanillin
0.120.960.77 – 2.3428V-Set
SEC/SEP [%]R
Range[%]SpectraSetParameter
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Transflectance analysis of samples of honey as it is
NIR Seminar – Campden – October 14th 2009
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Batch Product No. of samples Target (% alcohol)
1 Whiskey 1 12 40
2 Whiskey 2 14 40
3 Whiskey 2 15 40
4 Whiskey 2 4 40
5 Whiskey 1 15 43
NIR Seminar – Campden – October 14th 2009
Full Calibration Range(40% and 43% alcohol)
True Property Density OnlineP
redi
cted
Pro
pert
y D
ensi
ty O
nlin
e40 41 42 43
40
41
42
43Validation Spectra f(x)=1.0016x-0.0694 r=0.999919Calibration Spectra f(x)=0.9998x+0.0080 r=0.999903Validation SpectraCalibration Spectra
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NIR Seminar – Campden – October 14th 2009
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