wp 11 - high-throughput activities at iict - isa · 2016. 6. 28. · dn - policromyx phazir 1stder...

T4F - WP 11: High throughput activities at IICT/ISA – Brussells, April 2016

WP 11 - High-throughput activities at IICT - ISA

Ulisboa/ISA/CEF

José Rodrigues

Ana Alves, Sara Santos, Rita Simões

Py/GC-FID or MS

Auto sampler Frontier Lab


TNA Access Andrea Hevia/Juan Majada CETEMAS

Pinus pinaster Solid wood spectra acquisition – 1.4 mm slit

Spectra every 2 mm on the transversal section Spectra every 1 mm on the transversal section

Itrax


TNA Access Isabel Quilón/ Ricardo Alia INIA-CIFOR

Pinus halepensis

R² = 0.965

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

11.0

12.0

3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0

Tota

l ext

ractive

s N

IR p

redic

ted [

%]

Total extractives Soxhlet [%]

R² = 0.989

24

25

26

27

28

29

30

31

32

33

24 25 26 27 28 29 30 31 32 33

Kla

son

NIR

pre

dic

ted

dat

a (%

)

Klason laboratory data (%)

y = 0.9038x + 0.0058

R² = 0.9002

0.044

0.049

0.054

0.059

0.064

0.069

0.074

0.079

0.084

0.044 0.049 0.054 0.059 0.064 0.069 0.074 0.079 0.084

H/G

NIR

pre

dic

ted

da

ta

H/G Py-GC/FID


Bench instrument - Bruker MPA

Handheld instrument - PHAZIR

Portable unit - ASD LabSpec5000

JDSU MicroNIR 1700


• OPUS interface the most userfrindly

• Delivered wit chemometric package

• Optional accessories

• ASD interface user-friendly

• Requires external chemometric software,

•Optional accessories

• Portable 5.6 kg

• PHAZIR interface not so user-friendly

•Handheld but not for long ~1.25 kg

•Writing the sample names cumbersome.

• Requires external chemometric software

•JSD MicroNIR

• Requires external chemometric software

•Handheld 60g

•Powdered by USB


InstrumentResolution (distance between

data points)

No. of

scans

Scan

time [s]

Measurement

diameter [mm]

Range

Nm (cm-1)

MPA 8cm-1 (4 cm-1) 100 60 24800 – 2667

(12500-3750)

MPA 20cm-1 (10 cm-1) 5 1.3 24800 – 2667

(12500-3750)

MPA 32cm-1 (16 cm-1) 5 1 24

PHAZIR 8 nm (32 cm-1) 5 3 141604 - 2396

(6234 - 4174)

350 – 1000

(28500 – 10000)

1000 – 2500

(1000 – 4000)

JDSU 67- 23 cm-1 20 0.5 ~ 22 960

Lab Spec1.4nm - 350/1000nm

2nm - 1000 /2500nm

34ms

*????? 17.5

ASD_Blag1004UC_Av.

MPA_20_5\ Blag1004UC.0

MPA_32_5_Blag1004UC.0

Phazir_Blag1004UC.0


5000 6000 7000 8000 9000 10000

Wavenumber cm-1

0.0

5

0.1

0

0.1

5

0.2

0

0.2

5

0.3

0

0.3

5

0.4

0

0.4

5

Logarith

mic

Reflecta

nce

Page1/1

ASD_Blag1004UC_Av.

MPA_20_5\ Blag1004UC.0


Phazir_Blag1004UC.0


5000 5200 5400 5600 5800 6000 -0.0

00015

-0

.000010

-0.0

00005

0.0

00000

0.0

00005

0.0

00010

Logarith

mic

Reflecta

nce

Detector change


Data set (no.

of samples) PrePro r2 RMSECV RPD Rk Out Range

Phazir

Klason

lignin 75 VN 0.96 0.388 5.02 3 0

6267-5848; 6639-5429;

5010-4591; 4382-4173

H/G 75 MSC 0.89 0.0052 3.05 6 2

2396-1996; 1915-1755;

1675-1595

MPA

Klason

lignin 75 MSC 0.96 0.385 5.05 2 0 6109-4597

H/G 75 MSC 0.91 0.0047 3.35 3 2 6102-5446; 4601-4246

LabSpec5000

Klason

lignin 75 MSC 0.97 0.355 5.51 5 2

2351-2050; 1901-1451;

1302-1002

H/G 75 MSC 0.93 0.045 3.72 5 1 2351-2200; 1751-1601


Solid wood-transversal surfaces Model for basic density

Solid wood spectra aquisition – each 2mm


Solid wood-transversal surfaces Models for chemical composition

Ethanol extractives (%) Water extractives (%)



Solid wood-transversal surfaces Models for chemical composition

Klason lignin (%) S/G ratio

Solid wood spectra at each 2mm


Parameter R2 RMSECV RPD Rank R2 RMSECV RPD Rank

S/G 84.16 0.0488 2.51 1 82.60 0.0514 2.40 1

Klasson lignin* 89.93 0.923 3.15 2

Ethanol 92.90 0.304 3.75 2 87.26 0.407 2.80 4

Total extractives 95.51 0.279 4.72 2 83.51 0.533 2.46 4

Density 97.27 0.0261 6.06 5

Solid woodMilled wood extractive free

Milled wood Solid wood

* Solid wood (estimated data from milled wood)

Models summary


Sampling

MOE, MOR 20 x 20 x 360 mm

Janka hardness

20 x 20 x 150 mm

Normal density 12% de RH

20 x 20 x 20 mm

NIR spectra

20 x 20 x 150 mm


Variable Data

preprocesing Wavelenght (cm-1) CV/TS RK R

2 RMSE RPD

CV 1 0.90 33.8 3.1

TS 1 0.90 35.2 3.2

CV 1 0.93 22.3 3.73

TS 1 0.91 22.9 3.3

CV 1 0.74 10.3 1.96

TS 1 0.85 9.05 2.58

CV 3 0.82 976 2.33

TS 3 0.76 1140 2.05

CV 1 0.78 6.15 2.11

TS 1 0.74 8.51 1.95

CV 1 0.87 5.43 2.73

TS 1 0.87 5.68 2.79

DN

(kg/m3)

DB

(kg/m3)

MOR

(MPa)

MOE

(MPa)

DjankaTg

(MPa)

DjankaR

(MPa) 2ndDer

2ndDer

1stDer+SLS

NoPrePro

2ndDer

NoPrePro 11500-3825

11500-5440

7500-5400 4600-3800

6804-6094

8800-6090

11500-6080

DN - Normal density; DB - Basic density; MOR - Modulus of rupture; MOE - Modulus of elasticity

PLS-R models for solid wood – Eucalytus grandis


• MPA accessory test: • Integration sphere vs fiber-probe

• Spectra acquisition: • Transversal vs radial

• Surface preparation: • Sanded vs not sanded • Equipment: • MPA • PHAZIR • JDSU MicroNIR 1700

R2 R2

0.87 0.90

0.86 0.87

0.92 0.90

0.88

0.79

0.80


JDSU MicroNIR 1700 vs Bruker MPA Solid wood- transversal spectra

rk = 2 R² = 80

RMSE = 32 RPD = 2.24

400

450

500

550

600

650

700

400 450 500 550 600 650 700 750

PR

EDIC

TIO

N

TRUE

DB - JDSU MicroNIR 1700

1stDer+SLS 11120-7770 7000-5920 cm-1 1stDer 6100-5450 4600-3800 cm-1

rk = 4 R² = 88

RMSE = 28 RPD = 2.92

400

450

500

550

600

650

700

750

350 450 550 650 750

PR

EDIC

TIO

N

TRUE

DB - Bruker MPA


Policromyx Phazir vs Bruker MPA Solid wood- radial spectra

rk = 6 R² = 79

RMSE = 48.5 RPD = 2.2

400

500

600

700

800

900

1000

350 450 550 650 750 850 950

PR

EDIC

TIO

N

TRUE

DN - Policromyx Phazir

1stDer 6250-4250 cm-1 NoPrePro 11500-3825 cm-1

rk = 5 R² = 934

RMSE = 28 RPD = 3.9

400

500

600

700

800

900

1000

350 450 550 650 750 850 950

PR

EDIC

TIO

N

TRUE

DN - Bruker MPA


Pyroliser: micro-furnace, Frontier Labs, model EGA/PY-3030S Auto-sampler: AS-1020E GC: Agilent HP 6890

Gas Chromatograph (GC)

Oven

Column

Detector:

MSD

FID (Flame Ionization Detector)

CDS Pyroliser

Controler Resistively heated probe Interface


Sampling for Analytical pyrolysis

ANKON filter bags for extraction, 1g or smaller quantities

Sampling for analytical pyrolysis: ♦ Earlywood ♦ Latewood ♦ and in between


Bruker MPA – equipped with Fibre Probe


Eucalyptus globulus Spectra acquired at each 2mm on the transversal surface with a 2mm rectangular slit using a fiber probe.

wp 11 - high-throughput activities at iict - isa · 2016. 6. 28. · dn - policromyx phazir 1stder...

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