Combination of laser-optical methods for inline dough rheology monitoring

Similar documents
How DLS Works: Interference of Light

RHEOLASER LAB MICRORHEOLOGY & END USE PROPERTIES ANALYSIS. MICRORHEOLOGY

In-depth analysis of viscoelastic properties thanks to Microrheology: non-contact rheology

Non contact measurement of viscoelastic properties of biopolymers

Soft matters end use properties analysis thanks to Microrheology

Particles, drops, and bubbles. Lecture 3

Diffusing-wave spectroscopy: From particle sizing to micro-rheology. Prof. Yacine Hemar Food Group School of Chemical Sciences

Dynamic Mechanical Analysis of Solid Polymers and Polymer Melts

Part 8. Special Topic: Light Scattering

Fluorescence Spectroscopy

CHAPTER TWO: EXPERIMENTAL AND INSTRUMENTATION TECHNIQUES

PHYSICAL SCIENCES PART A

Kolligative Eigenschaften der Makromolekülen

Modeling of the Bread Baking Process Using Moving Boundary and Arbitrary-Lagrangian-Eulerian (ALE) C. Anandharamakrishnan, N. Chhanwal, P.

Measuring structure of low viscosity fluids in oscillation using rheometers with and without a separate torque transducer

Microstructure changes during baking

CM4655 Polymer Rheology Lab. Torsional Shear Flow: Parallel-plate and Cone-and-plate

Micro-rheology of cells and soft matter with the NanoTracker

Supplementary Information. SI Text 1: Derivation and assumptions of the effective temperature model

EXPERIMENTALLY DETERMINING THE VISCOELASTIC BEHAVIOR OF A CURING THERMOSET EPOXY R. Thorpe 1, A. Poursartip 1*

Micro-Rheology Measurements with the NanoTracker

INFLUENCE OF α-amylase ON RHEOLOGICAL PROPERTIES OF DOUGH. Abstract

Rheological Properties and Fatigue Resistance of Crumb Rubber Modified Bitumen

Polymer Dynamics and Rheology

CONSISTENCY OF RHEOLOGICAL EXPERIMENTS FOR PSA CHARACTERIZATION

Byong Yong Yu, and Seung-Yeop Kwak *

Nature Protocols: doi: /nprot Supplementary Figure 1

Rheological Properties of Fresh Building Materials

Mechanical properties of polymers: an overview. Suryasarathi Bose Dept. of Materials Engineering, IISc, Bangalore

Simulation of light scattering from Brownian particles

Chem728 Spr. 12 page 1 2/29/12. Assignment 2 Estimates of Hydrodynamic Radii from Dynamic Light Scattering Data. ANSWERS

Visualize and Measure Nanoparticle Size and Concentration

Knowledge of basic math concepts is expected (conversions, units, trigonometry, vectors, etc.)

University Graz / Austria Institut für Chemie Volker Ribitsch

Chapter 1 Fluid Characteristics

Static and dynamic light scattering. Cy Jeffries EMBL Hamburg

Les Houches School of Foam: Rheology of Complex Fluids

Possibility of using acoustic techniques for dough processing evaluation

Gold-poly(N-isopropylacrylamide) core-shell colloids with homogeneous density profiles: A small angle scattering study

Supplementary material to On the rheology of pendular gels and morphological developments in paste- like ternary systems based on capillary attraction

Aging in laponite water suspensions. P. K. Bhattacharyya Institute for Soldier Nanotechnologies Massachusetts Institute of Technology

A Technique for Characterizing Complex Polymer Solutions in Extensional Flows. Gavin Braithwaite Stephen Spiegelberg

Morphology and Rheology of Immiscible Polymer Blends under Electric Fields

::: Application Report

5. 3P PIV Measurements

Optical Microrheology of Biopolymers

Fundamentals of Polymer Rheology. Sarah Cotts TA Instruments Rubber Testing Seminar CUICAR, Greenville SC

Stokes and Newton s Viscous Drag

Effect of Liquid Viscosity on Sloshing in A Rectangular Tank

Problem: What affect does the force of launch have on the average speed of a straw rocket?

Chapter 2. Dielectric Theories

Sensing and Sensors: Fundamental Concepts

Linear viscoelastic behavior

Characterization of the structure at rest in foods (Example: Ketchup)

You may not start to read the questions printed on the subsequent pages until instructed to do so by the Invigilator.

Software Tools and Guide for Viscoelastic Creep Experiments

Coherent X-ray Scattering and X-ray Photon Correlation Spectroscopy

Rheometry. II.1 Introduction

CHAPTER V. Brownian motion. V.1 Langevin dynamics

Measuring particle aggregation rates by light scattering

Chapter 1. Continuum mechanics review. 1.1 Definitions and nomenclature

Analysis of Thermal Diffusivity of Metals using Lock-in Thermography

Supporting Information

Cover Page. The handle holds various files of this Leiden University dissertation

Emergence of Strong Nonlinear Viscoelastic Response of Semifluorinated Alkane Monolayers

Handle Food Samples with Care for Reliable Rheological Results

Rheology of Soft Materials. Rheology

Chapter 1: Electrostatics

Industrial Applications of Computational Mechanics Extended Civil Engineering Problems. Prof. Dr.-Ing. Casimir Katz SOFiSTiK AG

Measurements of Turbulent Pressure Under Breaking Waves

Synergy of the combined application of thermal analysis and rheology in monitoring and characterizing changing processes in materials

GEM4 Summer School OpenCourseWare

Microrheology: Basic Principles Translational and Rotational Motion of Probe Particles in Soft Materials

Rheology. What is rheology? From the root work rheo- Current: flow. Greek: rhein, to flow (river) Like rheostat flow of current

Part III. Polymer Dynamics molecular models

In Situ Imaging of Cold Atomic Gases

Approximate Linear Relationships

Lecture 15: Optoelectronic devices: Introduction

Rheological And Dielectric Characterization of Thermosetting Polymers. Jeffrey Gotro, Ph.D.

XPCS and Shear Flow. Wesley Burghardt Department of Chemical & Biological Engineering Northwestern University

Coherence properties of red blood cell membrane motions

Name :. Roll No. :... Invigilator s Signature :.. CS/B. Tech (New)/SEM-1/PH-101/ PHYSICS-I

Error Budgets, and Introduction to Class Projects. Lecture 6, ASTR 289

Introduction to Dynamic Light Scattering with Applications. Onofrio Annunziata Department of Chemistry Texas Christian University Fort Worth, TX, USA

Viscoelasticity, Creep and Oscillation Experiment. Basic Seminar Applied Rheology

For one such collision, a new particle, "k", is formed of volume v k = v i + v j. The rate of formation of "k" particles is, N ij

X-ray Intensity Fluctuation Spectroscopy. Mark Sutton McGill University

is the minimum stopping potential for which the current between the plates reduces to zero.

Chapter 17: Waves II. Sound waves are one example of Longitudinal Waves. Sound waves are pressure waves: Oscillations in air pressure and air density

Biological Process Engineering An Analogical Approach to Fluid Flow, Heat Transfer, and Mass Transfer Applied to Biological Systems

Realization of Marin Mitov Idea for the Stroboscopic Illumination Used in Optical Microscopy

MSE 383, Unit 3-3. Joshua U. Otaigbe Iowa State University Materials Science & Engineering Dept.

Micromechanics of Colloidal Suspensions: Dynamics of shear-induced aggregation

Jessica Gwyther. Characterisation of Plasticised Nitrocellulose using NMR and Rheology

Introduction to Dynamic Light Scattering for Particle Size Determination

Geology Geomath Computer Lab Quadratics and Settling Velocities

Georgia Institute of Technology. Nonlinear Dynamics & Chaos Physics 4267/6268. Faraday Waves. One Dimensional Study

Response of an elastic Bingham fluid to oscillatory shear

A Comprehensive Approach to Barite Sag Analysis on Field Muds

Chapter 11. Intermolecular Forces and Liquids & Solids

Transcription:

Center of Life and Food Sciences Weihenstephan Lehrstuhl für Brau- und Getränketechnologie Univ.-Prof. Dr.-Ing. Thomas Becker Combination of laser-optical methods for inline dough rheology monitoring Perez Alvarado, F., Hussein, M. A., Becker T.

Index Camera Camera + Laser Direct sample visual inspection (camera) Visual inspection analysis Backer master inspection Torque curve Analysis Z- Kneader analysis Spiral Industrial mixer analysis Texture feature (camera based) analysis Co-occurrence matrix extraction Homogeneity analysis Running research (camera-laser) Rheology analysis Intensity Correlation Function Particle mean square Displacement Dynamic light scattering (DLS) () + i Speckle Autocorrelation Visual recognition Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-2

Experimental Setup Visual recognition Visual recognition Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-3

Master Bakers Visual Inspection for T-160 For sample experiments in z kneader Average decision provided by 5 Master Bakers versus the one given by the power curve ±200 Average = 300 sec Mas. Bak. 1 Mas. Bak. 2 Mas. Bak. 3 Mas. Bak. 4 Mas. Bak. 5 Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-4

Decision time. Z- Kneader by Torque (Nm) 1600 1400 1000 mnm = 1 Nm = 500 FU After 10 experiments the maximal torque average value was obtained as decision time 1200 1000 800 600 400 ±40 Exp_1 Exp_2 Exp_3 Exp_4 Exp_5 Exp_6 Exp_7 Exp_8 Exp_9 200 Average value 355,4 seconds 0 0 100 200 300 Time to stop the 400 500 600 process Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-5

Homogeneity analysis Image is captured every 5 sec. during the mixing process Color is converted to gray scale, and region of interest is selected Co-occurrence matrix (, ) is calculated which defines the texture according to the times a color appears in the neighbourhood of color,,, Image Color 1 Color 2 Afterwards, homogeneity (H) is calculated as a statistics measure of co-occurrence H " # ",# $"%# where ",# is the i, j element of the normalized cooccurrence matrix at row (i) and column (j) Color 8 Color 1 Color 2 Color 8 Homogeneity refers to the uniformity of dough during mixing time, emulating the decision done by backers visual inspection. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-6

Homogeneity Analysis Homogeneity values are plotted along the mixing period Vector projecting from time - to each instantaneous homogeneity value is measured Steady-state is reached when the difference between to neighbor vectors has fixed increment Homogeneity / 0 1 0 1 time (s) Steady-state time Decision time by power curve Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-7

Homogeneity Analysis The magnitude difference / between the current vector "3" and the last vector 3%1" is calculated to determine the steady-state time / 0 1 %0 1, / 1 $ 1 % 1 $ 1 Two thresholds bound the steady-state response (~ 3%) are defined [lower threshold, upper threshold] / / 0 1 0 1 Predicted interval by developed regression model Steady-state time Decision time by power curve time (s) Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-8

Homogeneity Analysis A regression model is developed to predict the decision time through the information of steady-state time Decision time = fn (steady-state time) 20 reference experiments are ran and the steady-state time is calculated The decision time is obtained from the power curve of each experiment A linear relation between both times is found with 5 0.96, as shown :;<"=">1?"@; =?;A: =?A?;?"@; ~<=? Exp. Steady-state time (sec.) Decision time (sec.) 1 2 20 Decision time (sec.) 750 700 650 600 550 500 450 400 y = 2,4131x + 42,225 R² = 0,963 150 200 250 300 Steady-state time (sec.) Images during mixing Gray scale/roi Homogeneity calculation Decision time Regression model Steady-state time Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-9

Results: Offline Experiments Algorithm tested in over 23 trials to extract the curve features Validation Experiments 10 trials Experiment n Maximal torque time (s) Homogeneity analysis (s) Difference from maximal torque (s) Difference from torque Average (s) T-160_1 402,0 432,9 30,98 77,52 T-160_2 343,8 326,5-17,20-28,87 T-160_3* 310,8 439,6 128,83 84,16 T-160_4 348,0 326,5-21,40-28,87 T-160_5 367,2 343,2-23,98-12,24 T-160_6 403,8 329,9-73,88-25,54 T-160_7 355,8 393,0 37,28 37,62 T-160_8 291,0 379,7 88,78 24,32 T-160_9 376,8 343,2-33,58-12,25 Average 355,4 359,4 40,88 30,9 (*) outlier value Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-10

Decision time. Industrial spiral kneader Power (J/s) ±40 Time to stop the process Average value 564,8 seconds Time (s) Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-11

Results: Offline Experiments For sample experiments in Spiral Kneader Results obtained by homogeneity analysis vs power curve Experiment n Maximal power time (s) H. algorithm time (s) Difference from torque (s) Difference from torque Average (s) T-160_1 602 568,07-33,92 3,27 T-160_2 538 517,73-20,26-47,06 T-160_3 566 560,83-5,16-3,96 T-160_4 630 653,77 23,77 88,97 T-160_5 502 466,17-35,82-98,62 T-160_6 557 574,09 17,09 9,29 T-160_7 566 541,06-24,93-23,73 T-160_8* 611 673,66 62,66 108,86 T-160_9 529 531,24 2,24-33,55 T-160_10 547 561,32 14,32-3,47 Average 564,8 552,70 11,50 34,66 (*) outlier value Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-12

Camera optimum vs. Mixer optimum TA 160 Mixing Time Standard Camera 529s ± 36s 520s ± 34s spec. volume (dm 3 g -1 ) 4 3 2 1 a b Crumb hardness (N) 8 6 4 2 a b 0 Standard (529s) Camera (all) 0 Standard (529 s) Camera (all) Both parameter bread volume and bread crumb hardness where analyzed, and there is a significant improvement in those quality parameters by using the camera homogeneity system on baguette bread. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-13

KameraStop vs. Knetoptimum TA 165 Standard Kamera Knetzeit 607s ± 52s 724s ± 38s spec. volume (dm 3 g -1 ) 5 4 3 2 1 a a Crumb hardness (N) 6 4 2 a a 0 Standard (607 s) Camera (all) 0 Standardl (607 s) Camera (all) Both parameter bread volume and bread crumb hardness where analyzed, and there is a significant improvement in those quality parameters by using the camera homogeneity system on 65% water content baguette bread. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-14

KameraStop vs. Knetoptimum Laugengebäck (TA 155) Standard Kamera Knetzeit 463s ± 44s 501s ± 21s spec. volume (dm 3 g -1 ) 5 4 3 2 1 a b Crumb hardness (N) 3 2 1 a b 0 Standard (607 s) Camera (all) 0 Standardl (607 s) Camera (all) Both parameter bread volume and bread crumb hardness where analyzed, and there is a significant improvement in those quality parameters by using the camera homogeneity system on 55% water content Pretzel dough bread. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-15

Index Camera Camera + Laser Direct sample visual inspection (camera) Visual inspection analysis Backer master inspection Torque curve Analysis Z- Kneader analysis Spiral Industrial mixer analysis Texture feature (camera based) analysis Co-occurrence matrix extraction Homogeneity analysis Running research (camera-laser) Rheology analysis Intensity Correlation Function Particle mean square Displacement Dynamic light scattering (DLS) () + i Speckle Autocorrelation Visual recognition Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-16

Camera-laser analysis Establishing the relationship between rheological properties of dough and fast on line image processing analysis. Related to: Development of an Algorithm based on a Camera-Laser Sensing System for: Estimating dough optimal mixing time (on line) Estimating rheology of dough during mixing (on line) Understanding Intermolecular kinetics Interested in what happens during deformation of the medium. Mechanical testing device. Rheometer. The frequency dependent viscoelastic modulus is measured. Where: () + i () 2πE Elastic - storage modulus Viscous - loss modulus Angular frequency Proposed Camera-Laser system. The generalized Stokes-Einstein relation provide the modulus in terms of the mean square particle displacement F G Where: P Q R HIJ Boltzmann constant Temperature K L M NA O? S T Fluid viscosity Particle radius Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-17

Mechanical testing device. Rheometer. The frequency dependent viscoelastic modulus is measured. () + i Where: () Elastic - storage modulus Viscous - loss modulus 2πE Angular frequency If a substance is purely viscous then the phase shift angle δ is 90 : 0and If the substance is purely elastic then the phase shift angle δ is zero: and 0 With the complex modulus G* one can define the frequency dependent complex viscosity S : S /V Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-18

Proposed Camera-Laser system Laser He-Ne Laser Wavelength 632,8 nm Coherent length 1m Point diameter 1mm 600 s picturing time at 333 fps Acquisition system Camera Basler View angle 45 Resolution 2 MP Grabbing at 333 fps Picturing distance: 20 cm The generalized Stokes-Einstein relation provide the modulus in terms of the mean square particle displacement F G Intensity Correlation Function HIJ K L M NA F G W X?? $? Y";Z=? Y";Z=? $? Y";Z= Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-19

Theoretical background Fick's laws of diffusion Fick s law Concentration In a complex fluid particles move from high concentration to low concentration places Slope = % l lm diffusion direction b %c d df Where: z n y Diffusion Flux \ghijgt3j^ T`kh3Ga/\]^3G_ GV`^a Particle position \]^3G_a Concentration \ghijgt3j^ T`kh3Ga Diffusion coefficient \]^3G_ /GV`^a n o Particle position n n p The diffusion coefficient is proportional to the mobility of the diffusing particles, the Boltzmann constant and the medium temperature, according to the Einstein relation (kinetic theory) : c {K L M Where: Mobility of an spherical particle P Q Boltzmann constant R Medium Temperature Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-20

Theoretical background Einstein-Stokes relation Einstein-Stokes relation The diffusion coefficient is proportional to the velocity of the diffusing particles, which depends on the medium temperature, viscosity of the fluid and the size of the particle according to the Einstein relation (kinetic theory) c {K L M Einstein-Stokes relation: P Q R Mobility of an spherical particle Boltzmann constant Temperature Stokes demonstrates that the mobility for a spherical particle with radius a is proportional to the viscosity S: { }N~A S T Fluid viscosity Particle radius The Einstein-Stokes diffusion-viscosity relation is: K LM }N~A Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-21

Theoretical background. Mean square displacement (MSD) Mean square displacement (MSD) In 1956 Einstein demonstrate that the diffusion is related to the Mean square particle displacement (MSD) in 3 dimensions by: c F G n p %n }? By solving the equality: D r t 6G k Τ 6πηa In the time domain the viscosity is related to the MSD of the particle, the temperature and the particle size. ~ K LM? NA F G Where: P Q R S T Mobility of an spherical particle Boltzmann constant Temperature Fluid viscosity Particle radius Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-22

Theoretical background. Viscoelastic modulus (s) Viscoelastic modulus The frequency dependent viscoelastic modulus is obtained by the Laplace transform of the time domain viscosity L S in the Laplace plane"j" with J V. Laplace transform of the viscosity G (J)=L S J G J L P Q Τ G ŠT F G J Using the generalized Stokes-Einstein relation provide a physical interpretation of the modulus in terms of the mean square particle displacement F G HIJ K L M NA F G The mean square particle displacement F G is deduced from the Dynamic light scattering theory. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-23

Theoretical Background. Intensity Correlation Function Describes the rate of change in scattering intensity by comparing the intensity at time t to the intensity at a delay time (Gk $ G), providing a quantitative measurement of the flickering of the light. Mathematically, the correlation function is written as an integral over the product of intensities at some time into the mixing process and with some delay time Gk$ G, Which can be visualized as taking the intensity atg times the intensity at Gk$ G - red), followed by the same product at Gk$ G - blue, and so on W X?? $? Y";Z=? Y";Z=? $? Y";Z= Oriented particles create interference patterns, each bright spot being a speckle. The speckle pattern moves as the particle move, creating flickering. Generates a speckle pattern Various points reflect different scattering angles Where: G Lag time =? $? (ms) G - Lag time = 0 ms Camera sensor Intensity value normalized from no light 0 to high sensitivity 255. G Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-24

Deduction of mean square particle displacement The mean square particle displacement MSD is deduced from the Dynamic light scattering theory Intensity Correlation Function Dynamic light scattering (DLS) G - G - $ G Œ mž W X W c X G 1$^? G - Œ mž G - $ G Œ mž The intensity fluctuations I(t) are measured as a function of delay time (G - $G),, and the normalized intensity correlation function, (t), is calculated where the brackets indicate an average over time. Where: P is the laser wave number (15822,78j` ) 3 is the refractive index of dough (still in in research) MSD? is deduced from the equality. HIJ K L M NA F G Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-25

Experimental design To analyze the dough development 30 experiment will be done. Standard white dough (60% water content): 3000 gr Flour 1800 gr Water 20 C 30gr Yeast 45gr Salt Mixing process: 25 Hz, 30 second premixing to avoid dust problems 50 Hz, 600 second mixing (process in the graphic below) Initial temp: 21 C ± 1 C Final temperature: 32 C ± 1 C Laser He-Ne Laser Wavelength 632,8 nm Coherenz 1m Point diameter 1mm Acquisition system Camera Basler Resolution 2 MP Grabbing at 300 fps Picturing distance: 20 cm For every experiment the Rheological parameter of dough at the time point will be extracted by using the Rheometer in the Rheology lab. This results will be used for correlation and validation. Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-26

Rheology correlation and validation Rheometer Camera-Laser-System Images during mixing Intensity features extraction Intensity Autocorrelation function Rheometer Complex modulus Correlation and validation Einstein- Stokes rheology MSD deduction For every experiment the Rheological parameter of dough at the six mixing time points will be extracted by using the Rheometer in the Rheology lab. This results will be used for correlation and validation of the Camera-Laser System. Intensity Correlation Function W X Perez Alvarado, F. - 3rd European Conference on Process Analytics and Control Technology - 6 9 May 2014-27