B

Appendix BBiodiesel Standards

This section contains the specications of the following biodiesel standards: ASTM D6751 (United States), entitled Standard Specication for Biodiesel (B100) Blend Stock for Distillate Fuels, see Table B-1; ASTM D7467 (United States), entitled Standard Specication for Diesel Fuel Oil, Biodiesel Blend (B6 to B20), see Table B-2; EN 14213 (Europe), entitled Heating fuels - Fatty acid methyl esters (FAME) Requirements and test methods, see Table B-3; EN 14214 (Europe), entitled Automotive fuels - Fatty acid methyl esters (FAME) for diesel engines - Requirements and test methods, see Table B-4; Provisional Australian biodiesel standard, see Table B-5. Brazilian biodiesel standard NBR 15512, see Table B-6. South African biodiesel standard SANS 1935, see Table B-7. Analytical standards developed usually for the sake of inclusion in full biodiesel standards, see Table B-8. The specications in these standards may change with time. As it is not possible to reprint this book every time a change occurs, the user is encouraged to check the websites of the corresponding standards organizations for any newer versions of these standards. While there is a separate standard in the United States concerned with B6 to B20 blends, blends of up to 5% biodiesel in petrodiesel (B5) are covered by the petrodiesel standard ASTM D975. The European standard EN 14214, which went into eect in 2003, supersedes the biodiesel standards in the European countries which are members of the European Committee for Standardization (CEN). Therefore, no standards from individual European countries are given. CEN standards apply in the following member countries: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, and the United Kingdom. Besides the biodiesel standards, analytical standards have been developed in the United States and Europe for the purpose of including them as prescribed methods in biodiesel standards. Table B-6 lists such relevant analytical standards. The biodiesel standards can vary by properties, methods and limits. The biodiesel standards given are elaborated upon in the full standards available from the corresponding standardization organizations.

469

470

Appendix B

The European standard EN 14214 contains a separate section (not given in the table) for low-temperature properties. National standardizing committees are given the option of selecting between six CFPP (cold-lter plugging point; method EN 116) classes for moderate climates and ve for arctic climates. The total temperature range for these CFPP classes is from +5C to 44C. Relatedly, as the requirements regarding low-temperature properties vary, the standard ASTM D6751 has a report requirement for its cloud point parameter. A signicant number of specications in the standards deal with completion of the transesterication reaction. These are the specications related to free and total glycerol or content of mono- di- and triglycerides. Analytical standards based on gas chromatography are utilized in the standards for these specications (see also Chapter 5). Standards related to these analyses have been developed and are included in Table B-8.

Appendix BBiodiesel Standards 471

Table B-1. Biodiesel standard ASTM D6751 (United States).

Property Flash point (closed cup) Alcohol control One of the following must be met: 1. Methanol content 2. Flash point Water and sediment Kinematic viscosity, 40C Sulfated ash Sulfur Copper strip corrosion Cetane number Cloud point Cold soak filterability Carbon residue (100% sample) Acid number Free glycerin Total glycerin Distillation temperature, atmospheric equivalent temperature, 90% recovered Oxidation stability Calcium and Magnesium, combined Sodium and Potassium, combined Phosphorus content Test Method D 93 Limits 93 min Units C

EN 14110 D 93 D 2709 D 445 D 874 D 5453 D 130 D 613 D 2500 Annex A1 D 4530 D 664 D 6584 D 6584 D 1160 EN 14112 EN 14538 EN 14538 D 4951

0.2 max 130 min 0.050 max 1.9-6.0 0.020 max 0.0015 max or 0.05 maxa) No. 3 max 47 min Report 360 max 0.050 max 0.50 max 0.020 max 0.240 max 360 max 3 min 5 max 5 max 0.001 max

mass % C % volume mm2/s % mass % mass

C seconds % mass mg KOH/g % mass % mass C h ppm (m/g) ppm (m/g) % mass

a) The limits are for Grade S15 and Grade S500 biodiesel, respectively. S15 and S500 refer to maximum sulfur specifications (in ppm).

472

Appendix B

Table B-2. Biodiesel blend (B6-B20) standard ASTM D7467 (United States). Property
Flash point (closed cup) Water and sediment One of the following must be met: 1. Cetane index 2. Aromaticity Kinematic viscosity, 40C Ash content Sulfur content
a)

Test Method
D 93 D 2709 D976-80 D1319-03 D 445 D 482 D 5453 D 2622 D 129 D 130 D 613 D 2500 D 524 D 664 D 1160 EN 14112 D 6079 D 7371

Limits
52 min 0.05 max 40 min 35 1.94.1 0.01 max 15 max 0.05 max a) 0.50 No. 3 max 40 min Report 0.35 max 0.3 max 343 max 6 min 520 max 620

Units
C volume %

% vol mm2/s mass % g/g mass % mass %

Copper corrosion Cetane number Cloud point Ramsbottom carbon residue on 10% bottoms Acid number Distillation temperature, atmospheric equivalent temperature, 90% recovered Oxidation stability Lubricity, HFRR at 60C Biodiesel content

C mass % mg KOH/g C h Micron (m) % (v/v)

a) Different limits for blends with petrodiesel fuels of varying sulfur content.

Appendix BBiodiesel Standards 473

Table B-3. European Standard EN 14213 for Biodiesel as Heating Oil.

Property Test Method Limits min. Ester content Density; 15C Viscosity; 40C Flash point Sulfur content Carbon residue (10% dist. residue) Sulfated ash Water content Total contamination Oxidative stability, 110C Acid value Iodine value Content of FAME with 4 double bonds Monoglyceride content Diglyceride content Triglyceride content Free glycerine Cold-filter plugging point Pour point Heating value EN 14105 EN 14105 EN 14105 EN 14105 EN 14106 EN 116 ISO 3016 DIN 51900-1 DIN 51900-2 DIN 51900-3 35 0 EN 14103 EN ISO 3675 EN ISO 12185 EN ISO 3104 EN ISO 2719 EN ISO 3679 EN ISO 20846 EN ISO 20884 EN ISO 10370 ISO 3987 EN ISO 12937 EN 12662 EN 14112 EN 14104 EN 14111 4.0 0.50 130 1 0.80 0.20 0.20 0.02 96.5 860 3.5 130 10.0 0.30 0.02 500 24 900 5.0 max. % (m/m) kg/m3 mm2/s C mg/kg % (m/m) % (m/m) mg/kg mg/kg h mg KOH/g g iodine/100g % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) C C MJ/kg Units

474

Appendix B

Table B-4. Biodiesel Standard EN 14214 (Europe).

Property Test Method min. Ester content Density; 15C Viscosity; 40C Flash point Sulfur content Carbon residue (10% dist. residue) Cetane number Sulfated ash Water content Total contamination Copper strip corrosion (3h, 50C) Oxidative stability, 110C Acid value Iodine value Linolenic acid content Content of FAME with 4 or more double bonds Methanol content Monoglyceride content Diglyceride content Triglyceride content Free glycerine Total glycerine Sodium and Potassium Calcium and Magnesium Phosphorus content EN 14110 EN 14105 EN 14105 EN 14105 EN 14105 EN 14106 EN 14105 EN 14108 EN 14109 EN 14538 EN 14107 EN 14103 EN ISO 3675 EN ISO 12185 EN ISO 3104 EN ISO 2719 EN ISO 3679 EN ISO 20846 EN ISO 20884 EN ISO 10370 EN ISO 5165 ISO 3987 EN ISO 12937 EN 12662 EN ISO 2160 prEN 15751 EN 14112 EN 14104 EN 14111 EN 14103 1 6.0 0.50 120 12 1 0.20 0.80 0.20 0.20 0.02 0.25 5.0 5.0 4.0 h mg KOH/g g iodine/100g % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) mg/kg mg/kg mg/kg 51 0.02 500 24 % (m/m) mg/kg mg/kg 96.5 860 3.5 101 10.0 0.30 900 5.0 Limits max. % (m/m) kg/m3 mm2/s C mg/kg % (m/m) Units

Appendix BBiodiesel Standards 475

Table B-5. Australian Biodiesel Standard (Fuel Standard (Biodiesel) Determination 2003; approved under the Fuel Quality Standards Act 2000 by the Australian Minister for the Environment and Heritage).
Property Test Method Limits min Sulfur Density, 15C Distillation T90 Sulfated ash Viscosity; 40C Flash point Carbon residue 10% dist. residue 100% dist. sample Water and sediment Copper strip corrosion Ester content Phosphorus Acid value Total contamination Free glycerol Total glycerol Cetane number Cold-filter plugging point Oxidation stability ASTM D5453 ASTM D1298 EN ISO 3675 ASTM D1160 ASTM D 874 ASTM D445 ASTM D93 EN ISO 10370 ASTM D4530 ASTM D2709 ASTM D130 pr EN 14103 ASTM D4951 ASTM D664 EN 12662 ASTM D5452 ASTM D6584 ASTM D6584 EN ISO 5165 ASTM D613 TBA pr EN14122 ASTM D2274 (as relevant to biodiesel) prEN 14108 pr EN 14109 prEN 14538 6 C 51 96.5 10 0.80 24 0.02 0.25 3.5 120 0.30 or 0.05 0.50 No. 3 % (m/m) mg/kg mg/kg % mass % mass 860 max 50 10 890 360 0.20 5.0 mg/kg mg/kg kg/m3 C % mass mm2/s C % mass % mass % vol. September 18, 2003 February 1, 2006 September 18, 2003 September 18, 2003 September 18, 2003 September 18, 2003 September 18, 2003 September 18, 2003 Units Date of effect

September 18, 2003 September 18, 2003 September 18, 2003 September 18, 2003 September 18, 2004 September 18, 2004 September 18, 2004 September 18, 2004 September 18, 2004 September 18, 2004

mg KOH/g September 18, 2003

Metals - Group I (Na, K) Metals - Group II (Ca, Mg)

5 5

mg/kg mg/kg

September 18, 2004 September 18, 2004

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Appendix B

Table B-6. Brazilian Biodiesel Standard NBR 15512.

Property Flash point (C) Water content (mg/kg) Kinematic viscosity, 40C (mm2/s) a Specific gravity (kg/m3) Sulfated ash (%, m/m) a Sulfur (mg/kg) Copper corrosion 3h, 50C Cetane number Cold filter plugging point (C) Carbon residue (% mass) Acid number (mg KOH/g) a Free glycerin (%, m/m) Total glycerin (%, m/m) Total contamination (mg/kg) Ester content (% mass) Phosphorus (mg/kg) Methanol or ethanol (% mass) Iodine number Mono-, di-, triacylglycerols (% mass) Na + K (mg/kg) Ca + Mg (mg/kg) Oxidation stability 110C (h)
a

Limits 100 min. 500 max. 3.06.0 850900 0.02 max. 0.001 max. No. 1 max. Report 19 0.05 max. 0.50 max. 0.02 max. 0.25 max. 24 max 96.5 min 10 max. 0.20 max. Report Report. 5 max. 5 max 6 min.

Method ASTM D93, EN ISO 3679; NBR 14598 ASTM D6404; EN ISO 12937 ASTM D445; EN ISO 3104; NBR 10441 ASTM 1298, ASTM 4052, EN ISO 3675, EN ISO 12185; NBR 7148, NBR 14065 D874; EN ISO3987; NBR 6294 ASTM D5453; EN ISO 20846, 20884 D130; EN/ISO 2160 ASTM D613, D 6079; EN ISO 5165 ASTM D6371; EN 116; NBR 14747 ASTM D4530 ASTM D664; EN 14104; NBR 14448 ASTM D6854; EN 14105, 14106; NBR 15341 ASTM D6854; EN 14105; NBR 15344 EN ISO 12662 EN 14103; NBR 15342 ASTM D4951; EN14107; NBR 15553 EN 14110; NBR 15343 EN 14111 ASTM D6584; EN 14105; NBR 15342, 15344 EN 14108, EN 14109, EN 14538; NBR 15553, 15554, 15555, 15556 EN 14538; NBR 15553, 15556 EN 14112

Appendix BBiodiesel Standards 477

Table B-7. South African Biodiesel Standard SANS 1935a).

Property Test Method Limits min. Ester content Density; 15C Viscosity; 40C Flash point Sulfur content Carbon residue (10% dist. residue) Cetane number Sulfated ash Water content Total contamination Copper strip corrosion (3h, 50C) Oxidative stability, 110C Acid value Iodine value Linolenic acid content Content of FAME with 4 or more double bonds Methanol content Monoglyceride content Diglyceride content Triglyceride content Free glycerine Total glycerine Sodium and Potassium Calcium and Magnesium Phosphorus content Cold Filter Plugging Point (CFPP) EN 14103 ISO 3675, ISO 12185 ISO 3104 ISO 3679 ISO 20846, ISO 20884 ISO 10370 ISO 5165 ISO 3987 ISO 12937 EN 12662 ISO 2160 EN 14112 EN 14104 EN 14111 EN 14103 EN 14110 EN 14105 EN 14105 EN 14105 EN 14105, EN 14106 EN 14105 EN 14108, EN 14109 prEN 14538 EN 14107 EN 116 6.0 0.50 140 12 1 0.20 0.80 0.20 0.20 0.02 0.25 5.0 5.0 10.0 4 (winter) +3 (summer) 51 0.02 500 24 1 h mg KOH/g g iodine/100g % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) % (m/m) mg/kg mg/kg mg/kg C % (m/m) mg/kg mg/kg 96.5 860 3.5 120 10.0 0.30 900 5.0 max. % (m/m) kg/m3 mm2/s C mg/kg % (m/m) Units

a) Note that the South African biodiesel standard in its current version is virtually identical to the current version of the European biodiesel standard EN 14214 except for the specifications concerning the flash point, iodine value, phosphorus and cold filter plugging point.

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Appendix B

Table B-8. Analytical Standards Developed Usually for the Sake of Inclusion in Full Biodiesel Standards.
Standard ASTM D6584 ASTM D7371 Title Determination of Free and Total Glycerine in B-100 Biodiesel Methyl Esters by Gas Chromatography Standard Test Method for Determination of Biodiesel (Fatty Acid Methyl Esters)Content in Diesel Fuel Oil Using Mid Infrared Spectroscopy (FTIR-ATR-PLS Method) Standard Test Method for Boiling Range Distribution of Fatty Acid Methyl Esters (FAME) in the Boiling Range from 100 to 615C by Gas Chromatography Standard Test Method for Determination of Fuel Filter Blocking Potential of Biodiesel (B100) Blend Stock by Cold Soak Filtration Test (CSFT) Liquid petroleum products - Determination of fatty acid methyl esters (FAME) in middle distillates - Infrared spectroscopy method Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of ester and linolenic acid methyl ester contents Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of acid value Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of free glycerol content Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of phosphorus content by inductively coupled plasma (ICP) emission spectrometry Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of sodium content by atomic absorption spectrometry Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of potassium content by atomic absorption spectrometry Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of methanol content Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of iodine value Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of oxidation stability (accelerated oxidation test) Liquid petroleum products - Separation and characterization of fatty acid methyl esters (FAME) by liquid chromatography / gas chromatography (LC/GC) Fat and oil derivatives - Fatty acid methyl esters (FAME) - Determination of Ca and Mg content by optical emission spectral analysis with inductively coupled plasma (ICP OES)

ASTM D7398

ASTM D7501 EN 14078 EN 14103 EN 14104 EN 14105 EN 14106 EN 14107

EN 14108 EN 14109 EN 14110 EN 14111 EN 14112 EN 14331

EN 14538