INTERNATIONAL STANDARDS DEVELOPMENT

REGARDING BIOFUELS

Gina Clapper, AOCS Technical Services

CABER: Bioenergy Seminars

Urbana, IL

25 February2013

AOCS MISSION

AOCS advances the science and technology of oils, fats, surfactants and related materials, enriching the lives of people everywhere.

As an international professional organization, we

provide current and emerging information and disseminate research results in oils, fats, lipids, proteins, surfactants and related materials, through our meetings, publications, and web presence;

develop and uphold methods of analysis used in global trade and research, conduct proficiency testing, provide reference materials, and coordinate with other standards developers including ISO and Codex Alimentarius;

facilitate and strengthen interactions among professionals through meetings, specialized interest groups and other networking opportunities; and,

collaborate with other scientific societies and related organizations to promote the advancement of science.

AOCS TECHNICAL SERVICES EXPERTISE

World authority in the development and

implementation of methods of analysis for fats,

oils and oilseeds

Publisher of Official Methods and Recommended

Practices of the AOCS

Provider of the AOCS Laboratory Proficiency

Program (LPP)

US Administrator for ISO TC 34 (Food Products)

FEEDSTOCK ASSESSMENT

AOCS methods are prescribed for quality determinations in tallow and grease industry specifications

Equally important in feedstock assessment considering the wide range of fat-containing products which may be used as source material

Color

a. FAC

Cc 13a-43

b. R & B Color Cc 8d-55

Fatty acid profile Ce 1h-05

Free fatty acids Ca 5a-40

Iodine value (IV) Cd 1d-92

Lead content Ca 18c-91

Moisture Ca 2c-25 / Ca 2b-38

Unsaponifiable matter Ca 6a-40

Insoluble impurities Ca 3a-46

Peroxide value (PV) Cd 8b-90

Polyethylene (PE) Ca 16-75

Rate of filtration

Saponification value (SV) Cd 3-25

Titer Cc 12-59

Methods in bold text are recommended

for use in the Tallow and Grease Series of

the AOCS Laboratory Proficiency Program

(LPP), respectively.

AOCS METHODS FOR TALLOW AND GREASE QUALITY

PARAMETERS

WHY IS IT IMPORTANT TO ASSESS THE FEEDSTOCK

QUALITY?

Pretreatment can be critical and can increase the cost of

production

Need for complete reaction to FAMEs

Glycerin removal

Catalyst removal

Alcohol removal

Free Fatty Acid

ANALYTICAL PRIORITIES

Guidelines for feedstock quality New Recommended Practice published April 2007

Free, total glycerol…etc by GC/FID Cooperating with ASTM D2.06 to improve the current

D6584 method for collaborative study

Glycerol enzymatic Alternative method for glycerin

Potential for collaborative study

ANALYTICAL PRIORITIES (3)

% ester to test for major contaminants

Precipitates and cold flow

Stability

Peroxide values of raw materials

Flash point AOCS to adopt changes to ASTM D 93 method C

AOCS RECOMMENDED PRACTICE CK 1-07

Recommended Practices for Assessing Feedstock to Ensure Biodiesel Quality

lists those methods which may be used to assess the quality of oils and fats used in the production of biodiesel.

SCOPE

restricted to triglyceride feedstocks for biodiesel manufacture , including vegetable oils (soybean oil, rapeseed oil, palm oil, etc.), animal fats (tallow, lard, etc.) and triglyceride greases (yellow grease, etc.).

Critical attributes of the triglycerides are considered in light of the requirements of the most common biodiesel process - the alkaline transesterification of the triglyceride feedstock with methanol to produce fatty acid methyl esters.

CK 1-07 (2)

Sampling

Cleanliness

Purity

Impurities

Oxidative Stability

Fatty Acid Composition

TABLE 1. METHODS TO ASSESS FEEDSTOCK QUALITY. Test Method

Sampling AOCS C 1-47

Insoluble impurities AOCS Ca 3a-46

Sediment by centrifugation AOCS Ca 3d-02

Unsaponifiable matter AOCS Ca 6b-53

Polar compounds in frying fats AOCS Cd 20-91

Soap in Oil AOCS Cc 17-95

Polymerized triglycerides by gel-

permeation HPLC

AOCS Cd 22-91

Water by modified Karl Fischer

method

AOCS Ca 2e-84

Modified moisture and volatiles AOCS Ca 2f-93

TABLE 1. METHODS TO ASSESS FEEDSTOCK QUALITY (2)

Acid value AOCS Cd 3d-63 Sulfur - elements in oil by ICP-OES (use general guidance) AOCS Ca 17-01 Phospholipids in vegetable oils AOCS Ca 19-86 Phosphorus in oil by ICP-OES AOCS Ca 20-99 Phosphorus content – colorimetric method; AOCS Ca 12a-02 Phosphorus AOCS Ca 12-55 Fat stability, Oil Stability Index (OSI) AOCS Cd 12b-92 Fat stability, peroxide value AOCS Cd 8-53 or Cd 8b-90 p-Anisidine value AOCS Cd 18-90 Polymerized triglycerides by gel-permeation HPLC AOCS Cd 22-91 Polar compounds in frying fats AOCS Cd 20-91 Fatty acid composition AOCS Ce 1-62 Methyl ester preparation AOCS Ce 2-66

WHY STANDARDS?

WHAT IS THE PURPOSE OF STANDARDS?

For engine performance

For fuel quality

Measurement of input/output quality

Products and services are safe

Level the playing field

Facilitate free and fair global trade

WHO DEVELOPS THE STANDARDS?

Industry experts involved in this process can bring significant

advantages to your business. For example by:

Giving early access to information that could shape the market in

the future

Giving your company a voice in the development of standards

Helping to keep market access open.

Getting involved in standards development brings your concerns

and needs to bear on a process that will affect you in the future.

WHO DEVELOPS BIODIESEL STANDARDS?

International Organizations based in the US

AOCS (American Oil Chemists’ Society)

ASTM International

EMA (Truck and Engine Manufacturers Association™)

International Organizations based elsewhere

ISO (International Organisation for Standardisation)

CEN (European Committee for Standardisation)

WHAT IS BIODIESEL?

ASTM definition of biodiesel (adopted by EPA):

“fuel comprised of mono-alkyl esters of long chain fatty acids

derived from vegetable oils or animal fats, designated B100.”

Biodiesel is not:

Raw Vegetable Oils and Fats Non-Esterified Oils

Partially Esterified Oils Coal Slurries

Blends of above with Diesel Other ‘Biomass Based Diesel’

Thank you to Kyle Anderson for

this slide.

STATUS OF CURRENT ASTM SPECIFICATIONS FOR

BIODIESEL AND BIODIESEL BLENDS

ASTM D6751 is the specification for B100 for use as a blend

stock up to B5.

ASTM D7467 is the B6-B20 specification.

EN14214 is the European specification

There are differences between the ASTM and EN specifications

because EN14214 is based on RME (rapeseed methyl esters)

and the ASTM specifications are feedstock neutral.

Thank you to Steve Howell for this

slide.

STATUS (2)

ASTM D975 (on/off road diesel) allows up to 5% biodiesel and

ASTM D396 (heating fuels) allows up to 5% biodiesel without

labeling

Performance based for engines/burners

Must meet the same specification as the petro-only option

B100 must meet D6751 prior to blending

B5 is now fungible with diesel and heating fuel, just like other

components that are used in D975 and D396 fuels

Thank you to Steve Howell for this

slide.

STATUS (3)

As is the case with other fuels, D6751 continues to improve and

evolve over time

Especially as petro-diesel and engines change

Ultra low sulfur diesel is different today than when it was

introduced and is experiencing its own deficiencies

Internal injector coking

Corrosion in tanks and piping

Diesel engine temperatures and pressures are up

Clearances are down, filter pore-sizes are smaller

After-treatment systems are sensitive to metals that previously

had no impact

Thank you to Steve Howell for this

slide.

STATUS (4) RECENT IMPROVEMENTS TO D6751

Lowered the acid number to 0.5 mg KOH/g max from 0.8

Added a stability spec.of 3 hr minimum induction period

Developed and added the cold soak filtration test (D7501), 360 s

max or 200 s max if using below -12 ºC

This is to further control minor components that cause filter

clogging above the cloud point in some blends in the field

This phenomenon was not observed before ULSD

Adopted a new stability method (EN15751) which provides more

consistent results for biodiesel blends

Adopted AOCS Ck 2-09 IR method as an option for cloud point,

total glycerine, free glycerine, and methanol content

Adopted D6890, constant volume chamber derived cetane

number as an option for D613 cetane engine number.

Thank you to Steve Howell for this

slide.

BIODIESEL AND JET FUEL

B5 is shipped on the same pipelines as jet fuel in Europe

The US limits B5 to non-jet lines only (biodiesel in jet fuel must

be no more than 5 ppm

Currently there is a large, multinational program to generate

the data necessary to secure formal approval to increase to

100 ppm

USD 2 million effort

Air Force is re-running the thermal stability studies

If data are positive, a new level of 100 ppm biodiesel in jet

would be balloted into the jet fuel specifications

Thank you to Steve Howell for this

slide.

ACTIVITIES AT ISO

ISO/TC 28/SC 7 Liquid Biofuels

Secretariat: ANSI

Secretary: Mr. Todd Sandler

Chairperson: Mr. Sergio A. M. Fontes (Brazil) until end 2013

ISO Central Secretariat contact: Mrs. Kirsi Silander

Creation date: 2007

Standards and projects under the direct responsibility of

ISO TC 28/SC 7 Secretariat

Project Number Project name

ISO/NO 17306 Biodiesel – Determination of free glycerin,

monoglycerides, diglycerides, triglycerides

and total glycerin by gas chromatography

ISO/NP 17307 Biodiesel – Determination of total esters

content by gas chromatography

ISO/NO 17308 Ethanol – Test method for electrical

conductivity

ISO/CD 17315 Ethanol – Determination of total acidity by

potenciometric titration

TC 248 PROJECT COMMITTEE: SUSTAINABILITY CRITERIA

FOR BIOENERGY

Secretariat: DIN (Germany) Twinned secretariat: ABNT (Brazil) Secretary: Dipl.-Geoök. Reiner Hager Twinned secretary: Mr. Cláudio Guerreiro Chairperson: Mr. Humberto Siqueira Brandi (Brazil) until end 2015 ISO Central Secretariat contact: Mrs. Kirsi Silander Creation date: 2009

Scope: Standardization in the field of sustainability criteria for production, supply chain and application of bioenergy. This includes terminology and aspects related to the sustainability (e.g. environmental, social and economic) of bioenergy.

ISO/CD 13065 Sustainability criteria for bioenergy

THANK YOU!

For more information or to become involved

please contact:

Gina M. Clapper

AOCS Technical Services

Gina.Clapper@aocs.org

+1 217 693 4809