OPTIQUAD Spectroscopic Inline Analyzer

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Günter Pinkowski 2011-11-08 OPTIQUAD Spectroscopic Inline Analyzer Dipl.-Inf. Günter Pinkowski Managing Director KROHNE Optosens GmbH Kantstraße 22 41 464 Neuss Germany Tel.

1 Günter Pinkowski OPTIQUAD Spectroscopic Inline Analyzer Dipl.-Inf. Günter Pinkowski Managing Director KROHNE Optosens GmbH Kantstraße Neuss Germany Tel.: Mobil: Fax: g.pinkowski@krohne.com Measurement Solutions for the Water and Wastewater Industr y

2 1. KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement OPTIQUAD Agenda KROHNE Overview 15 Production Companies in 10 Countries 43 KROHNE Companies 55 Representatives Turnover (2010): 331 Mio / MUSD 465 Employees: 2658 Equity-to-assets ratio: 41 % Owner: The KROHNE Group is 100% owned by family Rademacher-Dubbick 4Overview

3 KROHNE in Europe Production KROHNE Sales Companies 5Overview KROHNE Rest of World Production KROHNE Sales Companies 6Overview

4 KROHNE Product Portfolio for Dairies/Cheese Factories Flow Level/ Pressure Temperature/ Analysis 7 KROHNE Mission To provide the right measurement solution for applications in process measurement for our customers around the world. We will achieve this by way of: technically innovative and high quality products qualified and competent employees long-term, reliable partnerships 8 November 9, 2011

5 1. KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement OPTIQUAD Agenda KROHNE Optosens GmbH KROHNE Optosens GmbH is a subsidiary of KROHNE Messtechnik GmbH with 2 offices in Neuss and Berlin with R&D and Production of OPTIQUAD with 15 employees Neuss Berlin with more than 50 man years of experience in optical spectroscopy 10 November 9, 2011

Two major versions of OPTIQUAD Measurement of protein,

water of dairies and cheese factories OPTIQUAD-M

Spectroscopic Inline Analyzer 3. Measurement Principle 4.

6 Two major versions of OPTIQUAD Measurement of protein, fat and lactose in milk Measurement of COD in waste water of dairies and cheese factories OPTIQUAD-M OPTIQUAD-WW 11 November 9, KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement OPTIQUAD Agenda

Measurement Principle Depending on the application OPTIQUAD uses up to 4 optical principles And up to 12 dedicated wave lengths, using LED s and Laser diodes typically being used by competition with

7 Measurement Principle Depending on the application OPTIQUAD uses up to 4 optical principles And up to 12 dedicated wave lengths, using LED s and Laser diodes typically being used by competition with complete spectrum 13 November 9, 2011 Transmission / Absorption Measurement of loss of light energy within a medium Transmission / Absorption can be used to measure e.g. the turbidity or the color of the medium 14 November 9, 2011

8 Scattering OPTIQUAD measures scattering of particles like fat particles within the milk November 9, 2011 Fluorescence UV light is send to the medium and certain molecules answer on a lower energy level (higher wave length), known as fluorescence This effect lasts approx. for one micro second only Bank note under UV light Intensity UV light Visible fluorescence Wave length [nm] 16 November 9, 2011

$Refraction OPTIQUAD measures the refractive index at the interface between two different mediums, especially between gl$

9 Refraction OPTIQUAD measures the refractive index at the interface between two different mediums, especially between glass and e.g. milk This can be used to measure the content of sugar e.g. Lactose (= milk sugar) in milk The principle is known from a prism or from a stick in the water Surface Air Water 17 November 9, KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement OPTIQUAD Agenda

OPTIQUAD-M (Milk products) Measurement of protein, fat and lactose in milk products in dairies and in cheese factories 19 November 9, 2011 OPTIQUAD-M: Spectroscopic Analyzer for Milk Products Inline

10 OPTIQUAD-M (Milk products) Measurement of protein, fat and lactose in milk products in dairies and in cheese factories 19 November 9, 2011 OPTIQUAD-M: Spectroscopic Analyzer for Milk Products Inline measurement of ingredients like protein, fat and lactose in milk By using up to 4 optical principles Hygienic, contact-free analysis within few seconds High precision same range as reference lab s Fat ± 0,03 % * Protein ± 0,02 % * Lactose ± < 0,1 % * Long term stability (no moving parts) No operating costs for chemicals, reagents, cleaning agents Excellent price-performance ratio * Standard deviation RMSE under reference c onditions 20 November 9, 2011

OPTIQUAD-M: System Overview Operating unit Analyzer unit Water cooling & air flushing Temperature sensor 24 VDC RS 422 4-20 ma and Binary outputs Sampling

can be calculated OR To separate the high quality milk to produce products with higher margins Fat Standardization of fresh milk Measure the real fat value in

11 OPTIQUAD-M: System Overview Operating unit Analyzer unit Water cooling & air flushing Temperature sensor 24 VDC RS ma and Binary outputs Sampling valve Varinline process connection 21 November 9, 2011 Application Examples Whole Milk Reception By knowing the fat and protein content the yield of the plant can be calculated OR To separate the high quality milk to produce products with higher margins Fat Standardization of fresh milk Measure the real fat value in the fresh milk stream in order to save fat to produce other products Increased Cheese Yield By measuring and controlling the fat and protein ratio 22 November 9, 2011

Cooling Raw Milk 23 November 9, 2011 Typical application Fresh Milk Fat standardization by real fat measurement in the final

12 Typical application Raw Milk Reception Fat and Protein measurement allows differentiation between low and high quality milk which allows Storage in different tanks and subsequent processing of different final products OPTIQUAD in-line analysis unit Cooling Raw Milk 23 November 9, 2011 Typical application Fresh Milk Fat standardization by real fat measurement in the final standardized milk rather than density measurement in the cream phase only OPTIQUAD in-line analysis unit 24 November 9, 2011

Typical application Cheese Milk Higher yield in cheese production due to standardized fat to protein ratio OPTIQUAD in-line analysis unit 25 November 9, 2011 Ammerland, Protein

13 Typical application Cheese Milk Higher yield in cheese production due to standardized fat to protein ratio OPTIQUAD in-line analysis unit 25 November 9, 2011 Ammerland, Protein Measurement Installation of OPTIQUAD in March 2009 Inline installation after separation and pre-heating (55 C / 130 F) but before homogenization Installation in a vertical pipe 26 November 9, 2011

method Number of samples On site lab analyzer Transmission 225 LKV Transmission 223 LUFA Kjeldahl 122 MLUA Kjeldahl 57 MUVA Kjeldahl 16 Total 643 27

14 Protein Measurement: Which Reference to use? First of all we wanted to define the calibration reference for OPTIQUAD We compared the following 5 different references: Laboratories Analytical method Number of samples On site lab analyzer Transmission 225 LKV Transmission 223 LUFA Kjeldahl 122 MLUA Kjeldahl 57 MUVA Kjeldahl 16 Total Protein Measurement: There is no real Reference! We found big deviations among reference labs even based on Kjeldahl method Biggest deviation was approx. 0,15% between dairy lab and MLUA! Deviation 0.1%!! (lab analyzer) (lab analyzer) 28 November 9, 2011

15 Protein Measurement: Lab Analyzer vs. LUFA Dairy lab device vs. LUFA; Standard deviation (RMSE) = 0,03 % Protein (%) 3,63 3,61 3,59 3,57 3,55 3,53 3,51 3,49 3,47 3,45 3,43 3,41 3,39 3,37 3,35 3,33 3,31 3,29 3,27 Molkerei-Labor, analyzer Foss FT120 LUFA (Kjeldahl) November 9, 2011 Protein Measurement: OPTIQUAD vs. LUFA Seasonal effect was measurable with no maintenance and no recalibration Standard deviation (RMSE): 0.03 % Protein (%) 3,63 3,61 3,59 3,57 3,55 3,53 3,51 3,49 3,47 3,45 3,43 3,41 3,39 3,37 3,35 3,33 3,31 3,29 3,27 LUFA (Kjeldahl) OPTIQUAD (gegen D LUFA kalibriert) Is this correct? November 9, 2011

16 Protein Measurement Best Case Lab analyzer vs. OPTIQUAD (after calibration), Standard deviation (RMSE) = 0.017% Protein (%) 3,650 3,600 3,550 3,500 3,450 3,400 3,350 3,300 3,250 3,200 3,150 Lab FOSS analyzer OPTIQUAD D Sample 31 November 9, 2011 Protein Measurement Ammerland: Protein OPTIQUAD vs. lab analyzer ( ) RMSEP = 0,031% Without questionable samples: 0,025% Protein lab analyzer Fat lab analyzer 32 November 9, 2011

17 Protein Measurement - Conclusion OPTIQUAD has shown accurate and stable protein measurements within 7 months No recalibration and No maintenance within the whole 7 months Standard deviation under reference conditions = 0,02% Long term standard deviation (RMSE) = 0,03% Repeatability (RMSE) = 0,01% Protein measurements from accredited reference labs showed severe differences up to 0,1% Therefore: There is No real reference available! We have to calibrate OPTIQUAD against the reference the customer has to select Inline measurement is not influenced by sample extraction, transportation, and sample handling 33 November 9, 2011 Ammerland, Fat Measurement ESL milk production with Mikro Filtration, homogenization and pasteurization of cream phase Cream Pasteur. Separator Skim milk In a vertical pipeline of DN 80 / 3 Raw milk MF Different treated mediums will be mixed like: - Skim milk through MF - Cream via homog. Homo OPTIQUAD 34 November 9, 2011

18 Fat Measurement: Unstable Fat Measurement At a glance the measurement performance of fat looked quite OK, but Customer was not satisfied with our unstable fat measurement Test run May 17, 2010 Fat [%] Lab device 12:00 16:00 35 November 9, 2011 Fat Measurement: Unstable Fat Measurement Yes, the customer was right, the fat trend was too unstable Test run May 17, 2010 Lab analyzer Fat [%] 12:00 16:00 36 November 9, 2011

19 Fat Measurement: Unstable Fat Measurement We took 18 samples in 1:25 min Result: The process was unstable, OPTIQUAD simply followed the reality Eng.company changed the process afterwards Problem solved 3,58 3,56 3,54 Lactoscop Lab analyzer OPTIQUAD 3,52 Fat Fettgehalt [%] [%] 3,50 3,48 3,46 3,44 3,42 14:54:00 14:56:00 14:58:00 Uhrzeit 37 November 9, 2011 Ammerland Fat Measurement After Fat Lab analyzer 38 November 9, 2011

20 Fat Measurement Ammerland: Fat OPTIQUAD vs. Lab analyzer ( ) RMSEP = 0.023%; 1.5% milk = 0.019%; 3.5% milk = 0.026% Before cleaning and zeroing 39 November 9, 2011 Fat Measurement Ammerland: Fat OPTIQUAD vs. Lab analyzer ( ) RMSEP = 0.021%; 1.5% milk = 0.012%; 3.5% milk = 0.025% After cleaning and zeroing 40 November 9, 2011

time would be a good idea to keep the OPTIQUAD up to date We recommend a 6 month maintenance cycle Standard deviation under

21 Fat Measurement - Conclusion OPTIQUAD has shown accurate and stable fat measurement The fat measurement has been used to control the fat standardization automatically Re-calibration: Depending on the application to enter samples from time to time would be a good idea to keep the OPTIQUAD up to date We recommend a 6 month maintenance cycle Standard deviation under reference conditions = 0.03 % Repeatability = % 41 November 9, 2011 KRAFT Foods: Fat and Protein Measurement 42 November 9, 2011

22 Kraft Foods, Fat and Protein Measurement Raw milk and skim milk and cream will be mixed in one of two tanks at 7 C / 45 F After the tank our OPTIQUAD is being installed in a vertical pipe The milk will be pumped through our meter to cheese production. Temperature is still 7 C / 45 F Three kind of cheese are being produced. Subsequently milk with either 2.9% or 2% or 1.5% will be used. Customer want to measure the fat and protein content to also control the ratio. 43 November 9, 2011 Kraft Foods, Fat and Protein Measurement 44 November 9, 2011

23 Conclusion Fat, Protein, Lactose Measurement OPTIQUAD has been proven to provide an accurate and stable Protein and Fat measurement in several milk applications We gained experience in several milk applications so far. Other applications are possible of course but might need application engineering OPTIQUAD can be considered as accurate as the lab and reference devices! Lactose (milk sugar) now released; Dry solid under test actually 45 November 9, KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement OPTIQUAD Agenda

mechanical holding system Operating unit Analytical Unit Cooling water connections 24 VDC RS422

24 OPTIQUAD-WW (Waste Water) Measurement of Chemical Oxygen Demand (COD) in waste water channels of dairies and cheese factories 47 November 9, 2011 OPTIQUAD-WW: System Overview Fixings for mechanical holding system Operating unit Analytical Unit Cooling water connections 24 VDC RS422 Temperature sensor 4 x 4-20 ma analogue outputs Compressed air cleaning nozzle Protective cover 48 November 9, 2011

OPTIQUAD-WW Additional Equipment Mechanical construction to hold the OPTIQUAD 49

typical waste water channel OPTIQUAD can easily be pulled out of the waste water

in front of our OPTIQUAD For certain applications we recommend a sample system

25 OPTIQUAD-WW Additional Equipment Mechanical construction to hold the OPTIQUAD 49 November 9, 2011 OPTIQUAD-WW Additional Equipment Complete construction to for a typical waste water channel OPTIQUAD can easily be pulled out of the waste water chamber with a steel rope For bigger dirt particles we recommend a guide plate in front of our OPTIQUAD For certain applications we recommend a sample system to pump medium out of the channel (calibration & validation) 50 November 9, 2011

Measurement of COD (chemical oxygen demand) We sold 6 devices

water channels and at the input of the waste water plant

to a small measuring gap) Customer is satisfied and we got

26 Measurement of COD (chemical oxygen demand) We sold 6 devices to a big dairy in Germany to measure COD within several waste water channels and at the input of the waste water plant Devices from two competitors did not work well (maintenance due to a small measuring gap) Customer is satisfied and we got final approval 51 November 9, 2011 Typical Installation 52 November 9, 2011

Measurement of COD (chemical oxygen demand) Continuous CSB-Monitoring (Measuring cycle within a few seconds) Measurement directly in the waste water No small measuring gap which would

27 Measurement of COD (chemical oxygen demand) Continuous CSB-Monitoring (Measuring cycle within a few seconds) Measurement directly in the waste water No small measuring gap which would need much maintenance Big measuring range (up to now up to mg/l) Automatic, cyclic cleaning of the measuring window by compressed air 53 November 9, 2011 Thank you for your attention!

28 1. KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement 6. OPTIQUAD Versatility OPTIQUAD Agenda Measurement of FFA (free fatty acids) Measurement of FFA in a staple chips production facility Reason: Quality control and to save fresh oil Customer will order the next device now 56 November 9, 2011

OPTIQUAD versatile measurements OPTIQUAD is able to be used in many other applications BUT we have to concentrate on the released applications only.

29 OPTIQUAD versatile measurements OPTIQUAD is able to be used in many other applications BUT we have to concentrate on the released applications only. Some examples where OPTIQUAD has been installed: Colour measurement Degree of whiteness of a liquid (big German dairy) Degree of yellow color on plastics (BASF) Biofouling thickness in water pipes (IWW) Population of bacteria in water applications (IWW) Suspended Oil in Water (BASF) Oil layer above water (NWKG) 57 November 9, KROHNE Introduction 2. Spectroscopic Inline Analyzer 3. Measurement Principle 4. Fat, Protein, Lactose Measurement 5. COD Measurement 6. OPTIQUAD Versatility 7. KROHNE Product Portfolio OPTIQUAD Agenda

Variable Area Flow Meter H 250 Reference for the Competiton Variable area meters are volumetric flow meters and can measure liquids and gases. H250 F is the meter from KROHNE for food applications.

30 Variable Area Flow Meter H 250 Reference for the Competiton Variable area meters are volumetric flow meters and can measure liquids and gases. H250 F is the meter from KROHNE for food applications. Through the modular design, the meter can have a local display and /or current and frequency outputs. Meters are used for hygienic applications and in utility processes on air, carbon dioxide and water. With EHEDG approval 59 Hygienic Magnetic Flow Meter OPTIFLUX 6000 Reference for the Competiton Electro Magnetic Flow meters are volumetric flow meters and measure conductive liquids up to a minimum conductivity of 5µS/cm. OPTIFLUX 6000 is the hygienic flow meter from KROHNE for all food and pharmaceutical processes. The combination of a sensor designed to the latest hygienic regulations and a powerful electronic makes this the optimum meter for hygienic process. Nominal size from DN 2.5 to

Process Adapter Metallic stop for precise compression and deformation of the L shaped gasket Highest sealing force at the

6000 Diameter: DN 2,5 150 (1/10 6 ) Flow range: Process temp.

Connections: DIN11850, DIN 11851, DIN 11864-2,DIN 32676 ISO 2037, ISO 2852, Tri Clover and SMS Material: AISI 316L,

31 Process Adapter Metallic stop for precise compression and deformation of the L shaped gasket Highest sealing force at the edge of the pipe Expansion of sealing at CIP/ SIP backwards, easy to clean Connection between EMF body and pipe OPTIFLUX 6000 Diameter: DN 2,5 150 (1/10 6 ) Flow range: Process temp.: 6 l/hr 763 m 3 /hr (0, USGal/min) -60 to +180 C (-76 to +356 F) (= remo te) Accuracy: < ± 0,2% of MV (IFC 300) Connections: DIN11850, DIN 11851, DIN ,DIN ISO 2037, ISO 2852, Tri Clover and SMS Material: AISI 316L, roughness (R a ) < 0,8 µm Liner: PFA (FDA conform), roughness (R a ) < 0,8 µm Electrodes: Approvals: Standard: Hastelloy C4 Optional: Stainless Steel, Titanium 3A, EHEDG, Pasteurized milk ordinance (PMO)

Converter features Batch Flow Meter BATCHFLUX 5500 C The Standard for Filling Machines Since the period of filling beverages in PET bottles, magnetic flow meters are used for precise dosing of the

32 Converter features Batch Flow Meter BATCHFLUX 5500 C The Standard for Filling Machines Since the period of filling beverages in PET bottles, magnetic flow meters are used for precise dosing of the liquid. compact housing in stainless steel fully welded and leak proof no risk of moisture ingress through lids and gaskets highest protection class IP69K Low power consumption Highest Accuracy/ Repeatability 64

Batch Flow Meter BATCHFLUX 5500 C Long term

temperature shock resistant hightech ceramic compared

results in excellent measuring accuracy and

Optimized flow tube tapered shape produces venturi

33 Batch Flow Meter BATCHFLUX 5500 C Long term reliability Measuring tube made of robust and temperature shock resistant hightech ceramic compared to fluoroplastic materials does not leak or creep results in excellent measuring accuracy and repeatability suitable for hot filling applications Optimized flow tube tapered shape produces venturi effect flow profile optimized for better accuracy 65 Hygienic Mass Flow Meter OPTIMASS range 66

Hygienic Mass Flow Meter OPTIMASS 7000 Inventor of Coriolis Straight Tube Meters Coriolis Mass Flow meters are flow meters which can measure

Through its features of measuring with one tube, the meter is highly appreciated at Food and Pharma applictaions.

density meter Sizes from DN 6 to 80 Custody transfer 67 Hygienic Mass Flow Meter OPTIMASS 7000 Features Only meter with integrated heating

34 Hygienic Mass Flow Meter OPTIMASS 7000 Inventor of Coriolis Straight Tube Meters Coriolis Mass Flow meters are flow meters which can measure precisely mass flow of liquids/gases/slurries and also the actual density. KROHNE invented the straight tube coriolis meter. Through its features of measuring with one tube, the meter is highly appreciated at Food and Pharma applictaions. Self draining; easy to clean High density / high viscosity applications No pressure drop is allowed Good for sheer sensitive products Precise density meter Sizes from DN 6 to 80 Custody transfer 67 Hygienic Mass Flow Meter OPTIMASS 7000 Features Only meter with integrated heating system All kinds of hygienic connections available Only single straight tube with Custody Transfer Approval; this for mass and volume applications Sizes from DN 6 to 80 Custody transfer 68

Encapsulated antenna, CIP cleanable and with hygienic process connections.

35 Hygienic Continous Level Meter OPTIWAVE 7300 Technological Leader in Radar For difficult applications and easy operation. Non contact measurement for liquids /slurries/ powders. Precise level mangement on liquids and solids. Encapsulated antenna, CIP cleanable and with hygienic process connections. CIP/ SIP cleanable 69 Pressure Transmitter PTD 500 Pressure transmitters are used to measure pipe pressure and also as a tank measurement for mixing and storage tanks. compact housing in stainless steel Hygienic process connections High overload protection High Resistance against condensate Highest Accuracy/ Repeatability 70

36 Applications Blending of syrup Producing different kinds of beverages Mixing the ingredients concentated syrup water vitamines and flavour additives. Applications Cream cheese Producing cream cheese milk vegetable oil additives final product

Applications Brewery Most of the liquids in breweries are measured by electromagnetic flow

37 Applications Chocolate Chocolate is a product with a high viscosity and therefore can only be pumped at higher temperatures. Here a heating jacket is required. Applications Brewery Most of the liquids in breweries are measured by electromagnetic flow meters example given : Water Mash water Wort measurement Yeast flow Flow of filtration aid Beer filtrate CIP liquids

and flavour additives CIP Applications Beverages Mixing tank where the

38 Applications Eckes Granini Producing Fruit juice Mixing the various ingredients of juices like concentated orange juice water vitamines and flavour additives CIP Applications Beverages Mixing tank where the various ingredients are mixed according to the recipe. Water Syrup Vitamines

39 Applications Juices Mixing tank where the various ingredients are mixed according to the recipe. Juice Additives Vitamines

OPTIQUAD Application list January 2016

OPTIQUAD Application list January 2016 Table of contents 1 OPTIQUAD-M 4050 W to measure Fat, Protein, Lactose, Total Solids,... 2 2 OPTIQUAD-WW 4050 W to measure COD in industrial waste water applications...