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Biodiesel NIR Seminar

“Biodiesel production control with NIR- Quality in your hands”

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Biodiesel NIR Seminar – May 27, 2009

“Biodiesel production control with NIR- Quality in your hands”

Ronny Pradon Market Manager BiofuelFOSS Analyticalrpn@foss.dkwww.foss.dk

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Agenda – Biodiesel Seminar 2009-05-27

Where NIR can be of a benefit in Biodiesel production

FOSS in Biofuel and a brief introduction to Near Infrared Technology

Questions & Answers

XDS Biodiesel Analyzer TM can make a difference

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Our Biofuel solutions are leveraged by our vast experience in a number of related industries

Edible oils

GrainFeed & forage

Flour

Beer Sugar (Petro-)Chemicals

Referenceanalysis

Biofuel

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A leading player in the global NIR market

• Innovator in utilizing NIR technology for more than 35 years

• Strong software platform for routine operation and calibration development

• Research partnerships with leading international universities and technology groups

• Combines chemical analysis, precision mechanics, electronics, software, optics and advanced chemometrics

Highlights :• 100+ patents relating to NIR technology• 20+ world first introductions• 45 state-of-the-art solutions• First to introduce advanced analysisoutside of safe laboratory environment

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The advantages of NIR for routine analysis

• No sample preparation is required

• Measurement takes less than two minutes

• Multiple parameters in one measurement

• Only limited training of end-user required

• No chemicals or pollutants

• Entirely safe

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The principles of NIR technology

Light source

Detector

Light source

Detector

• Near Infrared Technology is based on a combination of sophisticated spectrometry and powerful mathematics

• Near Infrared light is exposed onto a sample

• Light is modified according to the composition of the sample (using reflection or transmission)

• The spectral information is converted to composition of the sample

• These conversion algorithms are called calibrations

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Where NIR can be of a benefit in Biodiesel production

FOSS in Biofuel and a brief introduction to Near Infrared Technology

Questions & Answers

XDS Biodiesel Analyzer TM can make a difference

Agenda – Biodiesel Seminar 2009-05-27

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Where NIR is used in the “Oilseed to Biodiesel” value chain?

Oil seed intake- Quality and Yield assessment

Press cake - Process control- QA

Oil intake- QA - Feed forward to process (both to pre-refining and biodiesel process)

Process monitoring- Maintaining high efficiency- Reduce catalysts

B100 final product control- Quality control

Biodiesel plant

Oil refining Trans-esterification

FinalBiodiesel

Oil Seed Crushing

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Why measure on Biodiesel?

Intake control of feedstock– Knowing what comes in and how to best treat it

Optimizing conversion (efficiency)– Increased utilization of expensive feedstock

Increase productivity (uptime)– Reduce time-below-target at start-up phase

– e.g. new plants; after expansions/changes; maintenance– Avoid unwanted production stops due to out-of-spec production

Optimizing catalyst dosage (cost reduction)– Challenge is to reduce catalyst without affecting yield

Assuring final quality– Meeting the standards

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Where to measure ?

Crude oil

Decanter 1Reactor 1 Decanter 2Reactor 2

Glycerol

Catalyst / Methanol

Catalyst / Methanol

MethanolWater

Wash water

WaterSemi-refining

Biodiesel

Critical control points – where rapid & accurate analysis is needed

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1. Handling multiple sources of raw material

• A wide range of feedstocks are used for making biodiesel

- Rapeseed, Sunflower, Soybean- Used Cooking Oil, Animal fats- Others

• Oils from each feedstock has different characteristics and must therefore be monitored closely

• A number of components are detrimental to an optimal process and will severely reduce the efficiency of the plant

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NIR in the crude oil intake/pre-refining step

• Fast, up-front determination of

- Free Fatty Acids

- Phosphorous

- Water content

Key challenges

• Feedstock quality and pre-refining needs

• Validation of pre-refining process outcome

Advantages with NIR analysis

Decanter 1Reactor 1 Decanter 2Reactor 2

Glycerol

Catalyst/ Methanol

Oil/Feed-stock

Catalyst/ Methanol

MethanolWater

Wash water

Water

B100Bio-diesel

Pre-refining

Glycerol

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2. Tracking effectiveness of the conversion process

• Optimized conversion (leading to higher yield)- Every liter of crude oil that is not converted

to Biodiesel is lost revenue- Finding the time optimum of the trans-

esterification process

• Optimizing catalyst dosage- Catalyst is the most expensive reagent used

in the process- Challenge is to optimize catalyst addition

without affecting yield

• Reduced downtime- Less time used on trouble shooting

exercises

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NIR in the transesterification process

• Fast determination of e.g. Di-glyceride levels

• Continuous monitoring to avoid under-dosing or over-dosing catalyst

• Shorter analysis cycles enable fast tuning of the process (hours rather than days or weeks)

Key challenges

• Optimization of the conversion process (yield vs. time)

• Optimization of catalyst dosage

• Reduction of down-time (and start-up time from repairs/ maintenance)

Advantages with NIR analysis

Decanter 1Reactor 1 Decanter 2Reactor 2

Catalyst/ Methanol

Oil/Feed-stock

Catalyst/ Methanol

MethanolWater Water

B100Bio-diesel

Pre-refining

Glycerol Glycerol Wash water

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Adjusting catalyst based on DG levels (Di-glyceride)

Limit for Di-glyceride in Biodiesel according to EN 14214 is 0,20%

• Under-dosing of catalyst leads to reduced conversion (yield loss)

• Over-dosing of catalyst leads to increased cost (cost of e.g. base catalyst + cost of acid to neutralize after the process)

0,04

0,06

0,08

0,10

0,12

0,14

0,16

0,18

0,20

0,22

0,24

Upper action limit

Lower action limit

Di-glyceride (%)

Increase of catalyst dosage

Decrease of catalyst dosage

Maximum allowed (EN14214)

Time

EXAMPLE

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Reduce “below-target” production efficiency

1. Shorten time to react2. Measure effect of 1st action3. Measure effect on 2nd

action4. Measure effect on 3rd action5. Continuous monitoring of

efficiency

Using rapid analysis in this work process could reduce total time from days to hours.

95,00

95,50

96,00

96,50

97,00

97,50

98,00

98,50

99,00

99,50

100,00

Conversion rate [%]

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Catalyst dosage increased

Agitation / Stirring increased

Temperature adjusted

Time

E.g. Yield drop due to process problems or adjusting process to new feedstock.

EXAMPLE

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Start-up phase

80,00

82,00

84,00

86,00

88,00

90,00

92,00

94,00

96,00

98,00

100,00

Conversion rate [%]

Time

Starting up and fine-tuning a new factory takes months.

Similar start-up / tuning after a plant expansion / repair takes days / weeks.

Any reduction of “time below target” is money in the bank.

1-2 hour analysis by reference or

1-2 minutes analysis by XDS ??

EXAMPLE

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3. Checking that final product meets expectations

• Out of spec batches are often discovered too late for corrective actions- Need to store and blend sub-standard

Biodiesel with good Biodiesel

• Increased internal control of final product reduce need for sending samples to external laboratories for costly analysis

• Testing methyl esters/biodiesel purchased from other manufacturers direct at gate allows you to accept/reject incoming goods

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NIR in for final product screening

• Fast, continuous screening of all Biodiesel produced

• Reduced amount of reference analysis

• Very limited room for human error due to simple operation

Key challenges

• Validation of final product quality

• High cost of reference analyses

• Possibilities of human error adds to the uncertainty of reference methods

Advantages with NIR analysis

Decanter 1Reactor 1 Decanter 2Reactor 2

Catalyst/ Methanol

Oil/Feed-stock

Catalyst/ Methanol

MethanolWater Water

B100Bio-diesel

Pre-refining

Glycerol Glycerol Wash water

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For Quality control of final productAcid value

Iodine value

Linolenic Acid

Methylester

Density

Viscosity

Flash point

Sulfur

Tar remnant

Cetane number

Sulfated ash content

Water / Water & Sediment

Total contamination

Copper band corrosion

Thermal Stability

Oxidation stability

Methanol

Monoglyceride

Diglyceride

Triglyceride

Free Glycerine

Total Glycerine

Alkali Metals

Phosphorus

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Where NIR can be of a benefit in Biodiesel production

FOSS in Biofuel and a brief introduction to Near Infrared Technology

XDS Biodiesel Analyzer TM can make a difference

Questions & Answers

Agenda – Biodiesel Seminar 2009-05-27

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Analysis with current laboratory set up

In-house lab• Each test is very time & resource consuming (labor costs)• Long response time for results (hours)• Low sampling frequency• Significant laboratory expertise needed• Consumable costs • Plant operates 24/7, while lab often is 1 or 2 shift

External lab• High cost per sample • Long response time for analysis (days) • Low sampling frequency

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Benefits of using a XDS Biodiesel Analyzer

Analyses in < 2 minutes – allows more frequent controls

Offers easy-to-use operation for anyone in the plant

Reproducible results – not operator dependant

Remove workload from the reference analyzers

Reduces labor cost due to time savings

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XDS Biodiesel AnalyzerParameters in B100

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XDS Biodiesel Calibration range

Parameter N Min Max

Acidity 2082 0.02 1.94

Mono-glyceride 490 0.22 0.80

Di-glyceride 518 0.003 0.44

Tri-glyceride 674 0.0008 1.80

Total glycerine 518 0.028 0.49

Free glycerine 473 0.001 0.032

Moisture [ppm] 2126 6 1590

Iodine Value 243 71 131

Linolenic Acid 190 4.6 11.0

Methanol 127 0.01 1.29

Ester 262 95 100

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XDS Biodiesel Analyzer – evaluation

Parameter N Acc. Min Max RSQ

Aciditiy 283 0.044 0.06 1.73 0.94

Mono-glyceride 66 0.055 0.25 0.80 0.72

Di-glyceride 69 0.025 0.008 0.38 0.90

Tri-glyceride 84 0.045 0.001 1.08 0.96

Total glycerine 69 0.019 0.087 0.28 0.82

Free glycerine 67 0.003 0.001 0.029 0.84

Moisture [ppm] 278 28 10 440 0.81

Iodine Value 29 0.46 99 130 1.00

Linolenic Acid 22 0.23 5.8 9.2 0.92

Methanol 15 0.01 0.01 0.20 0.97

Ester 29 0.73 96.7 99.6 0.27

Evaluation done on an independent test set.(i.e. on samples not included in the calibration model)

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Predicted vs. Reference Lab

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Increasing analytical capacity by implementing a fast, reliable and easy-to-use XDS Biodiesel Analyzer

Estimated investment: 65’000 USD

Benefits- Capacity increase x10 (due to speed ; 2 minutes / sample)- Allowing more staff to carry out analysis (due to ease-of-use)- Immediate response (due to speed)

Savings:No investment needed in a second Gas Chromatograph or adding lab resources

Increased sampling frequency from conversion process and faster response time (near-real time)

Tighter process control – leading to savings in catalysts

Allowing all plant staff to carry out routine analysis 24/7 and faster response time (near-real time)

Reduced down-time and periods with below target production

Increased confidence in Final Quality by increased internal testReducing samples sent to external lab(20 samples less / year = 20 * 900 USD = 18.000 USD)

EXAMPLE

GC~ 40.000 –45.000 $

Lab resource (1 full time employment)

Process improvement (plant specific)

External Lab costs ~18.000 $

>> 60.000 $

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Biodiesel NIR Seminar – May 27, 2009

Questions & Answers

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Thank you for your attention !

Biodiesel NIR Seminar – May 27, 2009