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www.anton-paar.co Comparing measurement principles for alcohol, extract and CO 2 and a new, low cost method for inline alcohol measurement Ottakringer Brewery, Vienna September 9, 2014

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Comparing measurement principles for alcohol, extract and CO2 and a new, low cost method for inline alcohol measurement

Comparing measurement principles for alcohol, extract and CO2 and a new, low cost method for inline alcohol measurement

Ottakringer Brewery, ViennaSeptember 9, 2014

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www.anton-paar.com

Company ProfileMeasurement PrinciplesDensity, sound velocity and refractive indexOptical Infrared (IR) absorptionTransmissionAttenuated Total Reflection (ATR)Temperature/pressureA new method for process alcohol measurementHow to compare different principlesContents

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Company Profile

Establishment1922OwnerCharitableSantner FoundationCEODr. Friedrich SantnerChairman of the BoardUlrich SantnerEmployees worldwide (*as of the end of 2013) 892* in Graz1.913* worldwideTurnover 2013202 million EuroExports> 94 %Investment in R&D19 % of annual turnoverQuality managementISO 9001:2008

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www.anton-paar.comAll important company details:

1922 established as a one-man locksmiths workshopToday active globally, network of sales and service subsidiaries and distripution partnersSince 1997 Management: Dr. Friedrich SantnerNew subsidiaries have been establishedSystematic expansion of sales networkStrengthening Anton Paars position2003: Establishment of the charitable Santner Foundation

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~20 years ago, density/sound velocity and the alcohol combustion cell replaced RI and density/distillation in the laboratory.

~10 years ago, optical infrared spectroscopy (IR) and density became the preferred technology in the lab (Alcolyzer)

Process sensors continuously evolve and optical IR methods using Attenuated Total Reflection (ATR) are now available

Measurement Principles: In the Beginning

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Traditional measurement methods excel with:Robust & proven designVery long life spanHigh accuracyDrift free measurementMeasurement Principles: Today

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Optical methods also have definite benefits:Highly selectiveEasy to installCompact sizeMaintenance-freeLow cost of ownershipMeasurement Principles: Today

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U-tube filled with air

U-tube filled with sample

Measurement Principles: DensityDensity one of the most important parameters in lab and process

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www.anton-paar.comWie funktioniert nun die Dichtemessung mit Anton Paar Dichtemessgerten?Alle Anton Paar Dichtemessgerte basieren auf der Biegeschwingermethode. Es handelt sich dabei um ein U Rohr aus Glas, das in das Gert eingebaut ist und das in Schwingungen versetzt ist.Ist nun zum Beispiel das U Rohr mit Luft gefllt, so ist es leicht und schwingt schnell mit hoher Frequenz. Fllt man hingegen Probe ein, so ist das U Rohr entsprechend schwerer und schwingt langsamer. Je schwerer die eingefllte Probe, je hher die Dichte, desto niedriger die Frequenz.Daraus kann man deutlich entnehmen, dass sich die Probe in einem einfllbaren d.h. in einem flssigen oder pastsen Zustand befinden muss, da man Feststoffe nicht in das U Rohr einbringen kann. Wir werden spter Beispiele sehen, wie das in der Praxis aussieht.2 Becherglser; eines leer, eines mit 200 mL Wasser; Spatel

The propagation of a sound pulse through a sample

The sample flows between a transmitter and a receiver

The propagation time directly correlates to the concentrationMeasurement Principles: Sound Velocity

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A refractometer measures the critical angle of total reflection

The position of the light/dark line is detected by an optical Charged Coupled Device (CCD)

The concentration is calculated based on the location of the line on the sensor

Measurement Principles: Refractive Index

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IR is selective, has a very wide range of applicationsWorks best when the absorption peak is clearly visibleThe physics of optical process measurement remain difficultMinor temperature changes influence the measurementWater, extract and CO2 absorb light, so a reference wavelegnth is required

Measurement Principles: A Look at the IR Method

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Only a few wavelengths exist where the ethanol absorption is higher than water

Not all wavelengths are equally suited for accuracy

Clearly defined peaks work bestMeasurement Principles: IR Wavelengths

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Highly temperature dependentEspecially at modern beer production temperaturesInfluenced by the extract concentrationInfluenced by process and batch extract variationsHence, Anton Paars Alcolyzer replaced sound velocity in lab onlyMeasurement Principles: IR Alcohol Measurement

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All sugars have different but similar wavelengths

The absorption peaks are small

All are temperature dependent

The mash, extract efficiency, enzyme activity, and feedstock influence the sugar composition and change batch to batch

A mathematical model is required to measure the cumulative extract

This model is used to compensate the alcohol measurementMeasurement Principles: IR Extract Measurement

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Measurement Principles: IR absorption ATR

wavelength in nm referenced absorptionVarious CO2 concentrations at a specific wavelengthLarge absorption peakClearly defined wavelengthMostly free of other influencesThis allows for a strong, accuratesignal with little interference.

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Various sugar concentrations at a given CO2 concentrationAlcohol, extract and temperatureinfluence absorptionA reference wavelength isneeded to compensate1Plato 0.2 g/l CO2Measurement Principles: IR absorption ATR

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Low wavelengths require transmission method~1200nm transmission length is 8mmUsed in Anton Paars AlcolyzerMeasurement Principles: IR Transmission

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Measurement Principles: IR ATRHigher wavelengths require Attenuated Total Reflection (ATR)~2230nm transmission length is 1 mm

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Measurement Principles: IR ATRThe NIR absorption takes place in the surface layer (evanescent wave)

IR light sourceDetectorATR crystalFilterBeer

BeerEvanescent fieldIinIoutBoundary surfacePenetration depth 0.05 mm 2 mm Sapphire

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Most instruments typically use Henrys lawA chamber is filled with sample, temperature and pressure are measuredCO2 solubility is temperature and composition dependentTemperature: 0.05C = 0.1 g/LSugar: 1Brix = 0.1 g/LSolubility coefficients of beverage types are stored in the instrumentMeasurement Principles: Pressure / Temperature

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Anton Paars at-line and lab instruments combine the temperature/pressure and Multiple Volume Expansion (MVE) methods

MVE measures the temperature and pressure equilibrium at two different volume expansions

This method eliminated the influence of all other dissolved gasesMeasurement Principles: Pressure / Temperature / MVE

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www.anton-paar.comWhy?The Beer Monitor has been the standard over 20 years!BecauseSome installations only require the alcohol value (pre filler)Some breweries do not need the highest accuracySome breweries want an entry level system (beer monitor light)Compact size is easier to install and integrateLower cost of ownership & zero maintenanceA New, Low Cost Alcohol Sensor

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Introducing: Beer Monitor Basic

The classic Beer Monitor: accurate, robust and proven

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Introducing: Beer Monitor Basic

The classic Beer Monitor: accurate, robust and proven

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www.anton-paar.com

Introducing: Beer Monitor Basic

Beer Monitor Basic: compact, easy to install, low cost of ownership

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www.anton-paar.com

Introducing: Beer Monitor Basic

Beer Monitor Basic: compact, easy to install, low cost of ownership

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www.anton-paar.com

Introducing: Beer Monitor Basic

An upgrade is always possible should needs change

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Similar principle to the Original Extract MonitorAlcohol and OE are determined via sound velocity and a stored average brand densityDensity is not measured, so real extract can not be determinedCO2 compensation optional but not necessaryBeer Monitor Basic: How Does it Work?

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Maximum deviation in comparison to the Alcolyzer*:Beer Monitor Basic: How Well Does it Work?Beer MonitorBeer Monitor Basic Alcohol0.030.06Original extract0.060.10Extract0.040.15**

*Lab reference: DMA 4500 M and Alcolyzer Beer **Calculated from stored value

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Deviations between methods:Density, sound velocity, IR transmission, IR ATR, temperature/pressure, MVE, in-line, at-line, laboratory

all may show small deviations in their results.

Why?How do you minimize them?

Comparing Different Principles

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In-line, at-line vs. package:After filling, the CO2 changes

Head space volume and beverage temperature influence CO2 content

At higher temperatures more CO2 moves from the beverage to the head space

Comparing Different Principles: Why?

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Comparing Different Principles: A Head to Head TestHow do you compare different measurement methods?With a head to head test!

In-line data was recorded every 15 secondsAt-line measurements were made every 3 minutes

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What did we compare?As many methods as possible!

Carbo 520 Optical(process, ATR CO2)CarboQC (at-line & lab, temp/pres. MVE CO2)Beer Monitor (process, density/sound velocity)Beer Monitor Basic (process, sound velocity)Alcolyzer Beer (laboratory, NIR meter)DMA 4500 M(laboratory, density meter)

Comparing Different Principles: A Head to Head Test

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The Carbo 520 optical ATR sensor is factory adjusted with a standard CarboQC using the MVE method

The Beer Monitor (density/sound velocity) is calibrated using DMA 4500 M (density) and Alcolyzer Beer (NIR)

The Beer Monitor Basic (sound velocity) is calibrated using the Alcolyzer Beer (NIR)

Comparing Different Principles: ATR vs. MVE CO2

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Comparing Different Principles: ATR vs. MVE CO2So what happened?Between tank changes high variations in CO2 were seen due to residual CO2 gas in the pipe.

Very short and high peaks are only seen with in-line sensors.

Long flow stops and high, quick temperature changes did not affect the in-line optical sensor.

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Comparing Different Principles: ATR vs. MVE CO2

CO2 peak due to gas pocket after tank change

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Comparing Different Principles: ATR vs. MVE CO2

Quick temperature changesProduct warming due to flow stop

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Summary:Optical in-line sensor correlates extremely well with at-line temperature/pressure/MVE meterOptical in-line sensor is drift freeOptical in-line sensor tracks quick changes accuratelySOPs and Best Practice are key to consistent resultsATR vs. MVE CO2 Test Summary

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6 weeks & four beer styles later at a craft brewery in PennsylvaniaTrial Criteria:Overall measurement stabilityCorrelation to lab referenceInfluence of batch to batch variationsComparing Different Principles: Beer Monitor Basic

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Excellent measurement stabilityComparing Different Principles: Beer Monitor Basic

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How does it correlate to the lab reference?

Comparing Different Principles: Beer Monitor BasicLab reference: DMA 4500 M and Alcolyzer BeerAlcolyzer Alc. %v/vBeer Monitor Alc. %v/vDeviation Alc.Beer 14,514,55-0,04Beer 25,155,090,06Beer 25,145,090,05Beer 25,325,320,00Beer 25,325,33-0,01Beer 36,716,75-0,04Beer 36,716,76-0,05Beer 36,726,75-0,03Beer 49,439,370,06Beer 49,429,380,04Beer 49,429,360,06Min-0,05Max0,06Std. Dev.0,05

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Filtered and bottle conditioned beer tested with equal accuracyGood accuracy and repeatabilityDensity and RE variations have only minor alcohol influence0.001 g/cm = 0.06 % ABVEasy to install, low cost solutionIdeal for final alcohol check before packagingZero maintenance

Beer Monitor Basic: Trial Installation Summary

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We have existing formulas for:Beer, wine, spirits, soft drinks, beer mix drinks, FABs, malternatives, RTDs, cider, liquorsIf you are unsure, give us a callFeasibility study costs nothing and lasts only 2-6 weeks!Existing and New Applications

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www.anton-paar.comPresenter & Co-Author:Daniel L. Gore, Brewer & MalterApplication Specialist - Process Instrumentation+43 0316 / 257 [email protected]

Co-Author:Josef Bloder, DIKey Projects - Process Instrumentation +43 0316 / 257 [email protected] Information

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