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NIR&Wood – Sounds Good! #2 San Michele all’Adige, May 30, 2016 Probe technology for in-situ NIR applications 5/30/2016 Innovation with Integrity

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Page 1: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

NIR&Wood – Sounds Good! #2

San Michele all’Adige, May 30, 2016

Probe technology for in-situ NIR applications

5/30/2016 Innovation with Integrity

Page 2: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Sampling technology: definitions/1

Sample

DTC Source

Mirror

Transflectance

Sample

DTC Source

Diffuse reflectance

Sample

DTC

Source

Trasmission

30.05.2016 2

Page 3: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Sampling technology: definitions/1

30.05.2016 3

DTC Source

ATR

Sample

Sample

DTC Laser

Raman Scattering

Page 4: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

FO Cables, connectors

30 maggio 2016 4

• FO cables use standard male SMA 905 connectors

• Adaptors for connecting 2 fibres

Page 5: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Overview

30.05.2016 5

• Fiberoptic technology

• Reflectance Probes

• Sensor Heads

• Transmission Probes

• Flow Cells

• Transflectance Probes

Page 6: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Overview

30.05.2016 6

• Fiberoptic technology

• Reflectance Probes

• Sensor Heads

• Transmission Probes

• Flow Cells

• Transflectance Probes

Page 7: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Light Fiber Optics (“FO Cables”)

30.05.2016 7

• NIR low OH content quartz fiber

• Core diameter Ø 600 µm or 1000 µm

• Cladding and coating defines the optical and mechanical properties

• 7+7 fibers for reflection probes

• 6+1 fibers for reflection or transflection

• 1+1 fibers for transmission

Pure fused silica core (low OH)

Fluorine doped

fused silica cladding

Acrylate coating

Metal sheathed

Tefzel jacket

Page 8: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Monofiber Vs. Fiber bundle

30.05.2016 8

Page 9: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Sampling technology: spectral range

30.05.2016 9

MIR NIR Raman

Transmission + +++ n/a

Transflectance - ++ n/a

Diffuse reflectance + +++ +++

ATR +++ - n/a

Page 10: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

• Attenuation profile

Achievable Distances

30.05.2016 10

• length 1m

170m

290m

Page 11: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Cutoff frequencies

30.05.2016 11

Distance (m)

cu

toff

(cm

-1)

Page 12: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Fiber Optic Process Probes Reflection Probes for Solids

30.05.2016 12

• Functional Principle of Reflection Probes: Diffuse Reflectance

• Types of Solid Immersion Probes:

• IN264 – TURBIDO: Monofiber Reflection Probe

• IN268 – REFLECTOR (7+7): Multifiber Reflection Probe

• IN269 – ALBEDO (7+7): Multifiber Reflection Probe with Separate Flange

• IN270 – Hellma 668.008 (7+7): Multifiber Reflection Probe

Page 13: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Illumination

Specular reflection

Principle of diffuse reflectance

30/05/2016 13

Kubelka P., and Munk,F., Z.tech.Phys.12,593 (1931)

Page 14: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Functional Principle of Reflection Probes

30.05.2016 14

Sample

Detector

Source

Page 15: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probes: Principle of Diffuse Reflectance

30.05.2016 15

Page 16: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probes: Setup for In-Line-Measurements

30.05.2016 16

NIR Spectrum

Analysis

Result

Source

Fiber-Optic Cable

Probe

Sample

Detector

15g/kg

Fiber-Optic Cable

Page 17: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN263

30.05.2016 17

• Immersion depth: 325 mm

• Temperature range: -40ºC to 200ºC

• Diameter of probe: 10mm

• Connection: Fiber Bundle, BQC Adapter

Page 18: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN263: Installation in a Mixer

30.05.2016 18

Page 19: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN264 Turbido: Monofiber Reflection Probe

30.05.2016 19

Page 20: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN264 Turbido: Monofiber Reflection Probe

30.05.2016 20

• Materials: Stainless Steel 1.4435 (316L) or on request: Hastelloy, stainless steel 1.4571 (316Ti), Titanium, PTFE

• Sapphire window, sealing by epoxy glue

• Optical fiber: 600 µm, 3 m, 2 x SMA connector

• Illuminated spot: Ø 1 mm

• Probe diameter: 12 mm

• Immersion depth 300 mm

• Temperature: max. 130 °C (continuous use)

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Reflection Probe IN268 Reflector: Multifiber Reflection Probe

30.05.2016 21

Page 22: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN268 Reflector: Multifiber Reflection Probe

30.05.2016 22

• Materials: Stainless Steel 1.4435 (316L) or on request: Hastelloy, stainless steel 1.4571 (316Ti), Titanium, PTFE

• Sapphire window, sealing by epoxy glue

• Optical fiber: 7+7 600 µm, 2 m

• Illuminated spot: Ø 3 mm

• Probe diameter: 12 mm

• Immersion depth 300 mm

• Temperature: max. 130°C (continuous use)

• Pressure range: 0-16 bar, vacuum-resistant

Page 23: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN268 Reflector: Variation Reflector FLUSH

30.05.2016 23

Reflector Flush

Reflector Flush Plane

Cleaning Nozzle

Page 24: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN269 Albedo: Multifiber Reflection Probe with Flange

30.05.2016 24

Page 25: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN269 Albedo: Multifiber Reflection Probe with Flange

30.05.2016 25

• Materials: Stainless Steel 1.4435 (316L) or on request: Hastelloy, stainless steel 1.4571 (316Ti), Titanium, PTFE

• Sapphire window, O-Ring sealing (Kalrez®)

• Optical fiber: 7+7 600 µm, 2 m,

• Illuminated spot: Ø 5 mm

• Probe diameter: 50 mm

• Immersion depth 100 mm

• Temperature: max. 130oC (continuous use)

• Pressure range: 0-16 bar

Page 26: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN270: Hellma 668.008 Multifiber Reflection Probe

30.05.2016 26

Page 27: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Reflection Probe IN270: Hellma 668.008 Multifiber Reflection Probe

30.05.2016 27

• Materials: Stainless Steel 1.4435 (316L), other materials on request

• Sapphire window, EPDM, Kalrez® or brazed sealing

• Optical fiber: 7+7 600 µm

• Illuminated spot: Ø 2-4 mm @2.5 mm distance

• 30°illumination reflection

• Probe diameter: 30 mm

• Immersion depth 250 mm

• Temperature: 5 to 140 °C (continuous use)

• Maximum pressure: 10 bar

• Hygienic design, FDA conforming seals

Page 28: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Non contact system

30.05.2016 28

100÷400 mm

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Non contact system

30.05.2016 29

Page 30: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Non contact system

30.05.2016 30

• SS 1.4301, quartz window

• 2 NIR sources 5 W (or 4x20W)

• Working distance: 10 ÷40 cm

• Sample spot: 10 mm approx.

• Internal BKG

• Max distance to spectrometer:

100m

Page 31: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Non contact system

30.05.2016 31

• Air blade

• Vortex cooler (T > 40°C)

Page 32: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Installation on Cement Kilns Moisture and Calorific power

30.05.2016 32

Page 33: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Fiber Optic Process Probes Liquid Probes & Flow Cells

30.05.2016 33

• Types of Probes and Flow Cells:

• IN237 Series – Transmission Probe with or without flange

• Total Quartz Flange Immersion Probe

Page 34: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Fiber Optic Process Probes Liquid Probes & Flow Cells

30.05.2016 34

Optical Path Length d

Beers Law: AB ·c·d

Page 35: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Transmission Probes: Setup for In-Line-Measurements

30.05.2016 35

Medium

Optical Slit

NIR Spectrum

Analysis

Result

Source

Fibre-Optic Cable

Probe

Detector

15g/l

Fibre-Optic Cable

Page 36: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Transmission Probe IN237 Series: Hellma 661.790 – 793

30.05.2016 36

Page 37: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Transmission Flow Cells by PLS: ProTec TM50 and ProTec TM80 Series

30.05.2016 37

Page 38: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Transmission Flow Cells by PLS: ProTec TM50 and ProTec TM80 Series

30.05.2016 38

• Materials: Stainless Steel 1.4571 (316Ti) or on request: Hastelloy, stainless steel 1.4435 (316L), Tantalum, PTFE or PVDF

• Sapphire windows and Isolast® O-ring seals, other sealing materials on request

• Optical path length: 1 to 100 mm

• Optical fiber: 600 µm, 2 x SMA-905

• Temperature range: -20 to 230°C (depending on sealing material)

• Pressure range up to 250 bar (depending on flange)

• Connection: DIN or ANSI flanges, others on request

Page 39: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

• Principle of transflection combines transmission and reflection components.

• Types of Transflection Probes:

• IN271X-02 (6+1): Multifiber Transflection Probe

Fiber Optic Process Probes Transflection Probes for Emulsions etc.

30.05.2016 39

Page 40: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Fiber Optic Process Probes Transflection Probes for Emulsions etc.

30.05.2016 40

Rear-coated mirror for reflection

Light beam

Light path

Window

© by Hellma

• The light passes the medium, is reflected by a rear-coated mirror and passes through the solution a second time. Additionally, diffuse reflectance takes place in emulsions, dispersion etc., e.g. during crystallization.

Page 41: Probe technology for in-situ NIR applicationscostfp1407.iam.upr.si/en/resources/files/publications/...Fiber Optic Process Probes Reflection Probes for Solids 30.05.2016 12 • Functional

Probe IN271X-02: Multifiber Transflection Probe

30.05.2016 41

Illumination

Reception

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Innovation with Integrity

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