Ethanol Plant Testing
-samples
-instruments
-astm
-tests
-services available
-training


Testing includes:

Grain
 Mash
 Ethanol
 Feed
 Wastewater
 Methanator
 Ethanol
 Microbiology ?

Typical Inbound Grain Tests
Include:

Moisture (test weight lb/bu), crude
protein, crude fat or oil, starch, damage
and fo...
Maize is
composed of
approx. 70 %
starch, 8 %
protein and 4 %
fat/oil. The rest is
composed of
water, fibers, sug
ar and
v...
Typical test I have
done:
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Moisture NIR
Crude Protein NIR
Starch NIR
Crude Fiber NIR
Crude Fat/Oil N...
Grain/Feed Data
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Moisture (overnight)
Crude Protein (LECO)
Crude Fat
Ash
Crude Fiber
Acid Detergent Fiber
(ADF)
Neutra...
Environmental Labs need
to be state certified:
Midwest Labs
SDK Labs
Servi-tech
*Magellan
Local??
Color (L* Value)
Moisture
Crude Protein
Crude Fat
Ash
Crude Fiber
Acid Detergent Fiber
(ADF)
 Neutral Detergent .
 Fiber...
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Moisture (Vacuum oven)
Crude Protein (Kjeldahl)
Acid Hydrolysis Fat
Ash
Crude Fiber
Acid Detergen...
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Whole Corn –
Moisture, protein, oil, and
starch.
Ground Corn –
Moisture, protein, oil, and
starch.
M...
MASH TESTING
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Solids
Brix
HPLC
FAN
pH
HPLC
NIR (as hplc)
DE
Yeast Counts
Microbiology
?

ETHANOL TES...
ASTM REQUIREMENTS
FOR ETHANOL?
In House or Send Out?
Required ASTM (D4806)
Testing on Ethanol and Denatured Ethanol
ASTM D5580 Aromatics
ASTM D5580 Benzene
ASTM D6650 Olefins
...
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ASTM D4806 for ethanol used for fuel Property
Limits
Units
Ethanol 92.1 min. % v/v
Methanol 0.5 max. ...
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*Quarterly Denatured Ethanol Testing Requirements:
Proof
Apparent Proof
AST...
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ASTM D 4806
Standard Specification
for Denatured Fuel
Ethanol for Blending with
Gasolines for use as
...
ASTM D4806 (California)
Parameter Limits Test Method Frequency
Each batch
“calculated”
Olefins, 0.5 D6550-00
vol%, max
Eac...


California Denaturant Standards
Parameter Limits Test Method
Frequency

Olefins, 10 D6550-00 Each batch
vol%, max
 Aro...
Producer name and
location
 Traceable lot number
 Load date
 Quality results, limits
and test method
used
 Quarterly t...
Shipping Samples:
DOT Information:
UN
1987, Alcohols, n.o.s.(e
thanol, gasoline),
Hazard Class 3, Packing
Group II
Shippin...
DOT and Placards
UN1987;
Alcohols, (ethanol,
gasoline)
or
NA1987; Denatured
Alcohol

Fuel Ethanol E10 or E85?
Place card: ...
DP

HPLC

DP1=glucose
DP2=maltose
DP3=maltotriose
DP4=maltotetraose
DP5=maltopentaose
DP6=maltohexaose
DP7=maltoheptaose
D...
DP = Degree of
Polymerization
number of dextrose
molecules linked together
examples:
DP1, DP2, DP3, DP4…DP10…
The extent of starch hydrolysis is expressed as Dextrose Equivalent
(DE). DE is the percentage of glucosyl bonds that have...
DEXTROSE
EQUIVALENT (DE)
When the DE is 100, all of the bonds between glucose units in
the starch have been hydrolyzed. Ab...
Estimation of DE from
HPLC results
%DP1 * 100 + %DP2 * 50 + %DP3*33+
%DP4*10
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___
% S...
Milling
Mixing
Gelatinization
Cooking
Conversion
Saccharification
Fermentation
Distillation
Milling: Grind size effects
–

A large particle size can be more difficult to gelatinize
since enzyme cannot react with th...
Slurry: Gelatinization
The mash is cooked at 170 – 185 degrees to
gelatinize most of the starch and break the viscosity
en...
Liquefaction

Alpha amylase is denatured in
Liquefaction primarily because of
heat.
The heat further breaks down
starch mo...
Purpose of Fermentation:
To produce ethanol through the anaerobic
conversion of glucose by yeast.
51% of the glucose is co...
Cara 's ethanol laboratory testing requirements
Cara 's ethanol laboratory testing requirements
Cara 's ethanol laboratory testing requirements
Cara 's ethanol laboratory testing requirements
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Cara 's ethanol laboratory testing requirements

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Cara 's ethanol laboratory testing requirements

  1. 1. Ethanol Plant Testing -samples -instruments -astm -tests -services available -training
  2. 2.  Testing includes: Grain  Mash  Ethanol  Feed  Wastewater  Methanator  Ethanol  Microbiology ? 
  3. 3. Typical Inbound Grain Tests Include: Moisture (test weight lb/bu), crude protein, crude fat or oil, starch, damage and foreign material, dry matter, crude protein, crude fiber, calcium, phosphorus, sulfur, and ash.
  4. 4. Maize is composed of approx. 70 % starch, 8 % protein and 4 % fat/oil. The rest is composed of water, fibers, sug ar and various mineral nutrients.
  5. 5. Typical test I have done:            Moisture NIR Crude Protein NIR Starch NIR Crude Fiber NIR Crude Fat/Oil NIR Ash NIR Calcium Phosphorus Sulfur Aflatoxins? KIT Antibiotic residue? Exp Wet Feed/Dry Feed/Syrup/Grain
  6. 6. Grain/Feed Data
  7. 7.           Moisture (overnight) Crude Protein (LECO) Crude Fat Ash Crude Fiber Acid Detergent Fiber (ADF) Neutral Detergent . Fiber (NDF) Net E nergies (NEL, NEM, NEG ) Total Digestible              Nutrients (TDN) Digestible Energy Metabolizable Energy Sulfur Calcium Phosphorus Potassium Magnesium Sodium Iron Manganese Copper Zinc Wet Distillers Grain (WDGS) Package
  8. 8. Environmental Labs need to be state certified: Midwest Labs SDK Labs Servi-tech *Magellan Local??
  9. 9. Color (L* Value) Moisture Crude Protein Crude Fat Ash Crude Fiber Acid Detergent Fiber (ADF)  Neutral Detergent .  Fiber (ADF)  Net E nergies (NEL, NEM, NEG )                     Nutrients (TDN) Digestible Energy Metabolizable Energy Sulfur Calcium Phosphorus Potassium Magnesium Sodium Iron Manganese Copper Zinc Typical Tests for DDG Package
  10. 10.             Moisture (Vacuum oven) Crude Protein (Kjeldahl) Acid Hydrolysis Fat Ash Crude Fiber Acid Detergent Fiber (ADF) Neutral Detergent . Fiber (NDF) Net E nergies (NEL, NEM, NEG ) Total Digestible Nutrients (TDN) Digestible Energy            Metabolizable Energy Sulfur Calcium Phosphorus Potassium Magnesium Sodium Iron Manganese Copper Zinc Syrup Typical Package
  11. 11.         Whole Corn – Moisture, protein, oil, and starch. Ground Corn – Moisture, protein, oil, and starch. Mash – Total Solids. We will develop other HPLC test if you so desire Cooker/Yeast Prop – Brix, DP4, DP3, glucose, maltose , glycerol, acetic acid, lactic acid, ethanol Fermentation Samples – (same as above). Beer Well - (same as above). Wet Cake – Moisture, protein, oil/fat, crude fiber, Acid Detergent Fiber (ADF), Neutral Detergent Fiber (NDF), starch, and ash. Dried Distiller Grains – Moisture, protein, oil/fat, crude fiber, ADF, NDF, starch, and ash. NIR or Send Out?
  12. 12. MASH TESTING            Solids Brix HPLC FAN pH HPLC NIR (as hplc) DE Yeast Counts Microbiology ? ETHANOL TESTING                Acidity Moisture Karl Fisher Apparent Proof pHe Chloride Levels Sulfate Levels Denaturant Heptane Methanol Specific gravity Gum IC Copper C of A’s ? ?
  13. 13. ASTM REQUIREMENTS FOR ETHANOL? In House or Send Out?
  14. 14. Required ASTM (D4806) Testing on Ethanol and Denatured Ethanol ASTM D5580 Aromatics ASTM D5580 Benzene ASTM D6650 Olefins ASTM 5453 Sulfur ASTM 5191 Vapor Pressure ASTM D4052 Specific Gravity  ASTM D4815 Higher Alcohols  ASTM D130 Copper Corrosion  ASTM D86 Distillation Curve to include: initial boiling point 10% recovery, 50% recovery, 90% recovery and end point.                   ASTM D5501 Ethanol & Methanol by GC ASTM D7319 Chloride & Sulfate by IC ASTM D6423 pHe ASTM E1064 Water ASTM D381 Gum (washed/unwashed) ASTM D1613 Acidity ASTM D5453 Sulfur ASTM E1688 Copper ASTM D4052 Specific Gravity Hydrometer Proof VISUAL Appearance Calculation Denaturant Concentration
  15. 15.           ASTM D4806 for ethanol used for fuel Property Limits Units Ethanol 92.1 min. % v/v Methanol 0.5 max. (5,000 ppm) % v/v Water 1.0 max. (10,000 ppm) % v/v Solvent-washed gum 5 max. (50 ppm) mg/100 mL Chloride ion 40 max. (40 ppm) mg/L Copper content 0.1 max. (0.1 ppm) mg/kg Acidity as acetic acid 0.007 max. (70 ppm) % w/w Appearance Visibly free of suspended or precipitated contaminants Denaturant Minimum 1.96% v/v and maximum 4.76% v/v natural gasoline, gasoline components or unleaded gasoline.
  16. 16.                        *Quarterly Denatured Ethanol Testing Requirements: Proof Apparent Proof ASTM E1064 Water by Coulometric Karl Fischer ASTM D5501 Ethanol Purity ASTM D6423 Determination of pHe ASTM D381 Existent Gum ASTM D512 Chloride ion ASTM D1613 Acidity of Ethanol ASTM D1688 Copper ASTM D5453 Sulfur **Monthly Denatured Ethanol Testing Requirements: Proof Apparent Proof ASTM E1064 Water by Coulometric Karl Fischer ASTM D5501 Ethanol Purity ASTM D6423 Determination of pHe ASTM D1613 Acidity of Ethanol Optional testing for an additional: ASTM D5827 Sulfate by Ion Chromatography ***Denaturant Testing Requirements: ASTM D5580 Benzene, Total Aromatics ASTM D6550 Olefins Optional testing for an additional:: ASTM D5453 Magellan E85 and Ethanol Testing
  17. 17.           ASTM D 4806 Standard Specification for Denatured Fuel Ethanol for Blending with Gasolines for use as Automotive SparkIgnition Engine Fuel ASTM D 5798 Standard Specification for Fuel Ethanol (Ed75Ed85) for Automotive Spark-Ignition Engines ASTM Standards for Fuel Ethanol Performance Specifications
  18. 18. ASTM D4806 (California) Parameter Limits Test Method Frequency Each batch “calculated” Olefins, 0.5 D6550-00 vol%, max Each batch “calculated” Aromatics, 1.7 D5580-00 vol%, max Each batch “calculated” Benzene, 0.06 D5580-00 vol%, max Quarterly Third party Sulfur, ppm 10 D5453-93 California Requirements Differ
  19. 19.  California Denaturant Standards Parameter Limits Test Method Frequency Olefins, 10 D6550-00 Each batch vol%, max  Aromatics, 35 D5580-00 Each batch vol%, max  Benzene, 1.1 D5580-00 Each batch vol%, max 
  20. 20. Producer name and location  Traceable lot number  Load date  Quality results, limits and test method used  Quarterly third party lab results statement  Certificate of Analysis
  21. 21. Shipping Samples: DOT Information: UN 1987, Alcohols, n.o.s.(e thanol, gasoline), Hazard Class 3, Packing Group II Shipping
  22. 22. DOT and Placards UN1987; Alcohols, (ethanol, gasoline) or NA1987; Denatured Alcohol Fuel Ethanol E10 or E85? Place card: 1987
  23. 23. DP HPLC DP1=glucose DP2=maltose DP3=maltotriose DP4=maltotetraose DP5=maltopentaose DP6=maltohexaose DP7=maltoheptaose DP8=maltooctaose DP9=maltononaose DP10=maltodecaose Degree of Polymerization by HPLC
  24. 24. DP = Degree of Polymerization number of dextrose molecules linked together examples: DP1, DP2, DP3, DP4…DP10…
  25. 25. The extent of starch hydrolysis is expressed as Dextrose Equivalent (DE). DE is the percentage of glucosyl bonds that have been broken. Dextrose is another word for D-glucose. So, DE will be low (4 - 6) at the beginning of the process such as the Slurry tank outlet. Meaning: Mostly large molecules exist and not many molecules of glucose.
  26. 26. DEXTROSE EQUIVALENT (DE) When the DE is 100, all of the bonds between glucose units in the starch have been hydrolyzed. About 10% of the starch bonds are broken by the end of Conversion and up to half of the bonds are broken coming out of Saccharification. If half of the starch bonds are hydrolyzed the average DP is 2 and the DE = 50 example: 25% DP1 + 25% DP3 + 50% DP2 = 50 DE If a fourth of the starch bonds are broken the average DP is 4 and the DE = 25. DE determines the average DP length of the liquefied mash.
  27. 27. Estimation of DE from HPLC results %DP1 * 100 + %DP2 * 50 + %DP3*33+ %DP4*10 _____________________________________ ___ % Solids = est. DE
  28. 28. Milling Mixing Gelatinization Cooking Conversion Saccharification Fermentation Distillation
  29. 29. Milling: Grind size effects – A large particle size can be more difficult to gelatinize since enzyme cannot react with the substrate efficiently. This can result in yield loss (up to 10%). – A small particle size (< 200 mesh) can also cause problems: Mixing of floured grain in water may be more difficult. Small particles will also cause problems in centrifugation, evaporation, and drying. May have some positive effect on theoretical yield due to enzymes’ ability to react with starch. Typical Size : Mill grain to 100% thru 16 mesh
  30. 30. Slurry: Gelatinization The mash is cooked at 170 – 185 degrees to gelatinize most of the starch and break the viscosity enough to be pumpable. Alpha-amylase and water molecules together are randomly breaking down (or hydrolyzing) the amylopectin (branches) part of the starch structure. The alpha amylase produces a mixture of short sugar molecules (e.g. maltose, maltotriose), and some dextrin molecules (longer molecules of sugar). 4 - 6 DE mash
  31. 31. Liquefaction Alpha amylase is denatured in Liquefaction primarily because of heat. The heat further breaks down starch molecules for the second addition of alpha amylase. DE of 12 – 14
  32. 32. Purpose of Fermentation: To produce ethanol through the anaerobic conversion of glucose by yeast. 51% of the glucose is converted to ethanol and 49% is converted to carbon dioxide Ethanol Level at end of Fermentation is typically 12 15% v/v.

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