gunther pinkowski - krohne · 27.03.2009 08.04.09 24.04.2009 07.05.2009 19.05.2009 16.06.2009...

OPTIQUADSpectroscopic Inline Analyzer

Günter Pinkowski2011-11-08

Dipl.-Inf. Günter PinkowskiManaging Director

KROHNE Optosens GmbHKantstraße 2241 464 NeussGermany

Tel.: +49 203 301 429 1Mobil: +49 177 209 414 6Fax: +49 203 301 102 91

[email protected] www.krohne.com

| 2011-10-262 | Measurement Solutions for the Water and Wastewater Industr y

OPTIQUADAgenda

1. KROHNE Introduction

2. Spectroscopic Inline Analyzer

3. Measurement Principle

4. Fat, Protein, Lactose Measurement

5. COD Measurement

4

Owner: The KROHNE Group is 100% owned by family Rademacher-Dubbick

KROHNE Overview

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 %

5

KROHNE in Europe

Overview

Production

KROHNE Sales Companies

6

KROHNE Rest of World

Overview

Production

KROHNE Sales Companies

7

Flow

Level/Pressure

Temperature/Analysis

KROHNE Product Portfolio for Dairies/Cheese Factories

KROHNE Mission

To provide the right measurement solution for applications in process measurementfor 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

November 9, 20118 OPT IQU AD

OPTIQUADAgenda





5. COD Measurement

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

� … with more than 50 man years of experiencein optical spectroscopy

November 9, 2011

Berlin

Neuss

10 OPT IQU AD

Two major versions of OPTIQUAD


� Measurement of protein, fat and lactose in milk

� Measurement of CODin waste water of dairiesand cheese factories

OPTIQUAD-M OPTIQUAD-WW

OPTIQUADAgenda





5. COD Measurement

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

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


Scattering

� OPTIQUAD measures scattering of particles like fat particles within the milk

November 9, 2011

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15 OPT IQU AD

� 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

Fluorescence

November 9, 2011

UV light

Visiblefluorescence

16 OPT IQU AD

Bank note under UV light

Inte

nsity

Wave length [nm]

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

Water

Air

OPTIQUADAgenda





5. COD Measurement

OPTIQUAD-M (Milk products)


� Measurement of protein, fat and lactose

− in milk products

− in dairies and

− in cheese factories

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 condit ions

OPTIQUAD-M: System Overview


Temperature sensor

Samplingvalve

Varinline ®process connection

Water cooling & air flushing

Operating unit

Analyzer unit

4-20 mA andBinary outputs

24 VDC

RS 422

Application Examples


� Whole Milk Reception

− By knowing the fat and protein contentthe yield of the plant can be calculatedOR

− To separate the high quality milk toproduce products with higher margins

� Fat Standardization of fresh milk

− Measure the real fat value in the fresh milk streamin order to save fat to produce other products

� Increased Cheese Yield

− By measuring and controlling the fat and protein ratio

Typical application Raw Milk Reception


Cooling

Raw Milk

OPTIQUAD in-line analysis unit

� Fat and Protein measurement allows differentiation between low and high quality milk which allows

� Storage in different tanks and subsequent processingof different final products

Typical application Fresh Milk


� Fat standardization by real fat measurement in the final standardized milk rather than density measurement in the cream phase only


Typical application Cheese Milk


� Higher yield in cheese production due to standardized fat to protein ratio


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


27

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 643

Protein Measurement: There is no real Reference!


Deviation 0.1% !!

� We found big deviations among reference labs – even based on „Kjeldahl“ method

� Biggest deviation was approx. 0,15% between dairy lab and MLUA!

(lab analyzer)

(lab analyzer)

3,273,293,31

3,333,353,373,393,41

3,433,45

3,473,493,51

3,533,55

3,573,593,61

3,63

Pro

tein

(%)

Molkerei-Labor, Foss FT120

LUFA (Kjeldahl)

27.03.2009 24.04.2009 08.04.09 07.05.2009 19.05.2009 16.06.2009 08.07.2009

Protein Measurement: Lab Analyzer vs. LUFA

� Dairy lab device vs. LUFA; Standard deviation (RMSE) = 0,03 %


Lab analyzer

LUFA (Kjeldahl)

Protein Measurement: OPTIQUAD vs. LUFA

� Seasonal effect was measurable with no maintenance and no recalibration

� Standard deviation (RMSE): 0.03 %


3,273,293,313,333,353,373,393,413,433,453,473,493,513,533,553,573,593,613,63

Pro

tein

(%)

LUFA (Kjeldahl)

OPTIQUAD (gegen LUFA kalibriert)

27.03.2009 24.04.2009 08.04.09 07.05.2009 19.05.2009 16.06.2009 08.07.2009

Is this correct?

LUFA (Kjeldahl)

OPTIQUA D

3,150

3,200

3,250

3,300

3,350

3,400

3,450

3,500

3,550

3,600

3,650

1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31

Sample

Pro

tein

(%

)

FOSS

OPTIQUAD

Protein Measurement – Best Case

Lab analyzer vs. OPTIQUAD (after calibration), Standard deviation (RMSE) = 0.017%


OPTIQUA DOPTIQUA D

Lab analyzer

Protein Measurement


Ammerland: Protein OPTIQUAD vs. lab analyzer (15.2. – 17.2.2011)RMSEP = 0,031% Without questionable samples: 0,025%

Fat lab analyzer

Protein lab analyzer

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


Ammerland, Fat Measurement

� ESL milk production with MikroFiltration, homogenization andpasteurization of cream phase

� In a vertical pipeline of DN 80 / 3“

� Different treated mediums will be mixed like:- Skim milk through MF- Cream via homog.


Homo

Pasteur.

Separator

MF

CreamSkim milk

Raw milk

OPTIQUAD

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”


12:00 16:00

Test run May 17, 2010

Fat

[%]

Lab device


� Yes, the customer was right, the fat trend was too unstable


12:00 16:00

Test run May 17, 2010

Fat

[%]

Lab analyzer

14:54:00 14:56:00 14:58:00

3,42

3,44

3,46

3,48

3,50

3,52

3,54

3,56

3,58

Lactoscop OPTIQUAD

Fet

tgeh

alt [

%]

Uhrzeit



� We took 18 samples in 1:25 min

� Result: The process was unstable, OPTIQUAD simply followed the reality

� Eng.company changedthe process afterwards

� Problem solved

Fat

[%]

Lab analyzer

Ammerland Fat Measurement


� After

Fat Lab analyzer

Fat Measurement


Ammerland: Fat OPTIQUAD vs. Lab analyzer (2.2. – 17.2.2011)RMSEP = 0.023%; 1.5% milk = 0.019%; 3.5% milk = 0.026%

Before cleaning and zeroing

Fat Measurement


Ammerland: Fat OPTIQUAD vs. Lab analyzer (2.2. – 17.2.2011)RMSEP = 0.021%; 1.5% milk = 0.012%; 3.5% milk = 0.025%

After cleaning and zeroing

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 = 0.015 %


KRAFT Foods: Fat and Protein Measurement


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.

Kraft Foods, Fat and Protein Measurement


� OPTIQUAD has been proven to provide an accurate and stable Protein and Fatmeasurement 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

Conclusion – Fat, Protein, Lactose Measurement


OPTIQUADAgenda





5. COD Measurement

OPTIQUAD-WW (Waste Water)


� Measurement of Chemical Oxygen Demand (COD) in

− waste water channels of

− dairies and

− cheese factories


OPTIQUAD-WW: System Overview

24 VDC

RS422

4 x 4-20 mA analogue outputs

Analytical Unit

Compressed air cleaning nozzle

Operating unit

Temperature sensor

Protective cover

Cooling water connections

Fixings for mechanical holding system

OPTIQUAD-WW Additional Equipment


� Mechanical construction to hold the OPTIQUAD

OPTIQUAD-WW Additional Equipment


� Complete construction to for a typical waste water channel

� OPTIQUAD can easily be pulled out of thewaste water chamber with a steel rope

� For bigger dirt particles we recommenda guide plate in front of our OPTIQUAD

� For certain applications we recommenda sample system to pump medium out of the channel (calibration & validation)

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


Typical Installation


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 70.000 mg/l)

� Automatic, cyclic cleaning of the measuring window by compressed air


Thank you for your attention!

OPTIQUADAgenda





5. COD Measurement

6. OPTIQUAD Versatility

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


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)


OPTIQUADAgenda





5. COD Measurement

6. OPTIQUAD Versatility

7. KROHNE Product Portfolio

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 fromDN 2.5 to 150

60

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

61

Diameter: DN 2,5 – 150 (1/10” – 6” )

Flow range: 6 l/hr – 763 m3/hr (0,02 – 3361 USGal/min)

Process temp.: -60 to +180°C (-76 to +356°F) (= remo te)

Accuracy: < ± 0,2% of MV (IFC 300)

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

Material: AISI 316L, roughness (Ra) < 0,8 µm

Liner: PFA (FDA conform), roughness (Ra) < 0,8 µm

Electrodes: Standard: Hastelloy C4 Optional: Stainless Steel, Titanium

Approvals: 3A, EHEDG, Pasteurized milk ordinance (PMO)

OPTIFLUX 6000

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 reliability

Measuring tube

●made of robust and temperature shock resistant high-tech 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 MeterOPTIMASS range

66

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 coriolismeter. 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 80Custody 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 80Custody transfer

68

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

ApplicationsBlending of syrup

Producing different kinds of beverages

Mixing the ingredients

●concentated syrup

●water

●vitamines and

●flavour additives.

ApplicationsCream cheese

Producing cream cheese

●milk

●vegetable oil

●additives

●final product

ApplicationsChocolate

Chocolate is a product with a high viscosity and therefore can only be pumped at higher temperatures.

Here a heating jacket is required.

ApplicationsBrewery

Most of the liquids in breweries aremeasured by electromagnetic flow meters example given :

●Water

●Mash water

●Wort measurement

●Yeast flow

●Flow of filtration aid

●Beer filtrate

●CIP liquids

ApplicationsEckes Granini

Producing Fruit juice

Mixing the various ingredients ofjuices like

●concentated orange juice

●water

●vitamines and

●flavour additives

●CIP

ApplicationsBeverages

Mixing tank where the various ingredients are mixed according to the recipe.

●Water

●Syrup

●Vitamines

ApplicationsJuices

Mixing tank where the various ingredients are mixed according to the recipe.

●Juice

●Additives

●Vitamines

gunther pinkowski - krohne · 27.03.2009 08.04.09 24.04.2009 07.05.2009 19.05.2009 16.06.2009...

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