Dr. Egbert Stärk 2. European Bioethanol Technology Meeting in Detmold Near Infrared Spectroscopy for the Bioethanol Industry
Dr. Egbert Stärk
2. European Bioethanol Technology
Meeting
in Detmold
Near Infrared Spectroscopy for the
Bioethanol Industry
1. Company Perten Instruments
2. NIR Spectroscopy
3. NIR for Bioethanol industry
4. Whole grain analyser for incoming materials
5. New NIR technology and applications
6. Diode Array benefits
7. On-line measurements
Overview
2. European Bioethanol Technology Meeting
1. Perten Instruments I
• founded in 1962 by Harald Perten• head office in Stockholm (Sweden)• today approx. 90 employees• branch offices in Germany (Hamburg), USA, China
Switzerland, France, Australia, …
• The first focal point : Quality Control of Flour• traditional products:
- Falling Number - Glutomatic- Lab mills
• today mainly Near Infrared (NIR)
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1. Perten Instruments II
2. European Bioethanol Technology Meeting
More than 25 years experience in NIR technology
• focal point today : Quality Control of Flour, Grain, Food and Feed
• NIR products: - Inframatic systems for Flour, Powder, Meals - Inframatic systems for Whole grain, Corn, Oil seed- Diode Array (DA) for Food, Feed and more- DA on-line for Flour, Grain and Feed
• cooperation with Buehler regarding On-line systems• approx. 20.000 NIR systems world wide installed
2. NIR Spectroscopy• Interaction of near infrared light and the sample• Diffuse reflected light offer sample information• Chemometric models make results available
Parameter:Protein, Moisture, Fat, Starch, Fiber, Oil, (Ash), Glucose, Ethanol, Amino acids, Energy, …
Products:Single products: all Grain, Corn, Oil seeds, … Raw materials: Soybean & Rapeseed flour, Silage, .. By-products: DDG, Fermentation broth, …Finished products: Feed, Food, Liquid feed
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2. Advantage of NIR vs. Lab
• Very fast method (results in seconds)
• Several components simultaneously
• No time delay - Process control possible
• High throughput means very cost-effective
• No use of chemicals
• Easy handling - no or less sample preparations
2. European Bioethanol Technology Meeting
2. European Bioethanol Technology Meeting
3. NIR Spectroscopy for the Bioethanol Industry
Measurements for a fast qualityand process control:
1. Incoming Grain / Corn - Moisture, Protein, Starch, Oil
2. Fermentation broth, Beer well- Glucose, Ethanol, Maltose,
Lactic Acid, …
3. Process control - Moisture in DDGS at the
centrifuge, Distillers samples
4. Co-products: Dry & Wet Distiller’s Grain- Moisture, Protein, Fiber, ADF, NDF, …
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4. Incoming Grain / Corn
Inframatic 9200:
Products: Wheat, Rye, Triticale, Oats, Corn, Barley, Rapeseed
Parameter: Protein, Moisture, Starch, Oil, Hectoliter weight
Inframatic 9200
Fast quality control at the receiving office
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4. Inframatic 9200 - Results
Products and Parameter with IM 9200- Standard Error of Prediction (SEP):
ParameterProduct
Starch Protein Moisture Fat
Wheat 0.65 0.23 0.20 -Rye 0.87 0.24 0.22 -Triticale 0.85 0.24 0.21 -Corn 0.95 0.34 0.28 0.32
useable at- Grain traders - Mills - Bioethanol IndustryIM 9200
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5. New NIR Technology for moreapplications
DA 7200 Spectrometer:
• based on Diode Array Technology• analysis time approx. 5 seconds • all wavelengths in milliseconds • developed for many applications• non moving optical parts inside• better wavelength accuracy and
reproducibility
DA 7200
5. Diode Array 7200
2. European Bioethanol Technology Meeting
DA 7200 advantages: • nonnon--contact contact measurement from above from above • no sample grinding and preparation• easy to use (two button analysis)• rotating sample cups• multi-component analysis in 5 seconds• no cleaning work
DA 7200: wide application possibilitiesFlour, Powder, Wholemeal, Pellets,Kernels, Pasta, Butter, Liquid feed,finished Food and Feed
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5. DA 7200 – Results
Income Wheat - Protein - vary useable instrument
Samples: 786Range: 9.2 - 22.2%R2 : 0.98SEP : 0.26
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Reference
NIR
5. DA 7200 – Results
2. European Bioethanol Technology Meeting
Income Wheat – Starch- whole grain, meal, pellets, butter, … with one sample cup
60
63
66
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61 64 67 70 73
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61 64 67 70 73
1
234 5
6
78 9
10
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2122
23
2425
2627
28
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3839
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4445
464748
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51 52
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54 55
5657
58
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6162
6364
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6768
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72 73
74757677
78
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82 838485
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674 675676677
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60
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61 64 67 70 73
Reference
NIR
Samples: 683Range: 61.1 – 72.7%R2 : 0.89SEP : 0.85
2. European Bioethanol Technology Meeting
5. DA 7200 – Results
Income Corn - Moisture, Protein, Oil, Starch- all parameters simultaneously
Parameter Range [%]
Samples R2 SECV
Moisture 8.2 – 15.8 241 0.99 0.18
Protein 5.6 – 13.8 241 0.99 0.29
Oil 3.0 – 7.2 241 0.67 0.30
Starch 72.4 – 74.2 143 0.75 0.29
5. DA 7200 – Results Dried Distiller’s Grain (DDG)
- fast quality control - measurement of dry and wet
Distiller’s Grain possible
Protein:Samples: 683Range: 28.0 – 38.1%R2 : 0.98SEP : 0.30
2. European Bioethanol Technology Meeting
28
31
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28 31 34 37
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28 31 34 37
1
2 3
45
67
89
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Reference
NIR
2. European Bioethanol Technology Meeting
5. Analysis of Fermentation Broth
DA 7200 for further applications:
- disposal cups for liquid feed- changeable in seconds- fast measurements of fermentation broth- non-contact, no cleaning work
Disposal cup with Fermentation Broth
DA 7200Non-contact samplingwith disposal cup
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5. Analysis of Fermentation Broth
DA 7200:
Ethanol, Glucose, Maltose, …
in Fermentation Broth
ParameterProduct
Range[%]
Sample R2 SECV
Ethanol 0.2 – 13.4 235 0.99 0.28Glucose 0.1 – 11.6 230 0.98 0.46Maltose 0.4 – 5.2 230 0.96 0.32Lactic Acid 0.1 – 1.3 221 0.79 0.10
Et h a n o l in Fe rm e n t a t io n B ro t h
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00
La b
NIR
Disposal cup
2. European Bioethanol Technology Meeting
- very fast measurements (5 seconds)
- new technology - vary useable
- stand alone instrument
- easy software and handling
- less sample preparation - no cleaning
- to handle also complex material
DA 7200
6. DA 7200 – Benefits:
7. Perten Instruments On-line History
2. European Bioethanol Technology Meeting
Cooperation with Bühler for On-line started in 1990
Myra: Measurement in flour millsParameter: Moisture, Protein, Ash, Others …
Myre: A whole grain version wasintroduced for grain intake at flour mills in 2000
Parameter:Moisture, Protein, Starch, ...
Approximately 500 units supplied
7. Why On-line measurements?
2. European Bioethanol Technology Meeting
Example: 100 to / day capacity- Manually: 10 meas. / day means 1 per 10 to- On-line: > 150 meas. per 10 to
• Every min one measurement or faster
• Average specifications of whole tonnage
• Starch content in the fermenter is exactly known
• Reliable calculation of produced ethanol and yield rate
• DA on-line instrument available
• Calibrations transfer from lab instrument possible
Thank you for your attention!
2. European Bioethanol Technology Meeting
DA 7200