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Analyzing Biodiesel: Standards and Other Methods Gerhard Knothe* National Center for Agricultural Utilization Research, ARS, USDA, Peoria, Illinois 61604

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Analyzing Biodiesel: Standards and Other Methods Gerhard Knothe* National Center for Agricultural Utilization Research, ARS, USDA, Peoria, Illinois 61604 REVIEW Analyzing Biodiesel: Standards and Other Methods Gerhard Knothe* National Center for Agricultural Utilization Research, ARS, USDA, Peoria, Illinois 61604 ABSTRACT: Biodiesel occupies a prominent position among are also contained in Table 2. A brief discussion of the differ- the alternatives to conventional petrodiesel fuel owing to various ences in the specifications of EN 14213 vs. EN 14214 can be technical and economic factors. It is obtained by reacting the par- found at the end of this article. ent vegetable oil or fat with an alcohol (transesterification) in the Biodiesel is produced by transesterifying the parent oil or presence of a catalyst to give the corresponding monoalkyl es- fat with an alcohol, usually methanol, in presence of a catalyst, ters, which are defined as biodiesel. Because of the nature of the usually a strong base such as sodium or potassium hydroxide, starting material, the production process, and subsequent han- or, preferably and increasingly more commonly, alkoxides. The dling, various factors can influence biodiesel fuel quality. Fuel quality issues are commonly reflected in the contaminants or resulting product therefore can contain not only the desired other minor components of biodiesel. This work categorizes both alkyl ester product but also unreacted starting material (TAG), the restricted species in biodiesel and the physical properties pre- residual alcohol, and residual catalyst. Glycerol is formed as scribed by the standards, and details the standard reference meth- by-product and separated from biodiesel in the production ods to determine them as well as other procedures. Other aspects process, however, traces thereof can be found in the final of biodiesel analysis, including production monitoring and as- biodiesel product. Since transesterification is a stepwise sessing biodiesel/petrodiesel blends, are also addressed. The process, MAG and DAG formed as intermediates can also be types of analyses include chromatographic, spectroscopic, physi- found in biodiesel. Accordingly, these aspects have been ad- cal properties-based, and wet chemical methods. The justifica- dressed in biodiesel standards. The analysis, fuel quality, and tions for specifications in standards are also addressed. production monitoring of biodiesel have been discussed (see Paper no. J11420 in JAOCS 83, 823–833 (October 2006). articles in Refs. 1–5), but not all aspects of standards were con- KEY WORDS: Biodiesel, biodiesel blends, diesel fuel, fuel sidered, especially in light of their recent adoption, various as- properties, gas chromatography, infrared spectroscopy, liquid pects were categorized differently and new developments have chromatography, near infrared spectroscopy, nuclear magnetic occurred. resonance, standards. Besides these aspects, other issues need to be considered, such as fuel and physical properties as well as storage and han- dling issues. For example, biodiesel can absorb a certain Biodiesel (1,2), defined as the monoalkyl esters of vegetable amount of water during storage. Another example is the sus- oils or animal fats, is steadily gaining interest and significance ceptibility, of linoleic and linolenic acid esters especially, to ox- in light of recent developments such as the upsurge in petro- idation. Other storage parameters also can affect fuel quality. leum prices and the implementation of financial incentives for Such issues are also addressed in biodiesel standards. its use. With the increasing interest and use, the assurance of Some specifications in biodiesel standards are carryovers fuel properties and quality has become of paramount interest to from petrodiesel standards. However, not all test methods car- the successful commercialization and market acceptance of ried over from petrodiesel standards into biodiesel standards biodiesel. Accordingly, biodiesel standards have been estab- are well suited for biodiesel analysis. To account for the nature lished or are being developed in various countries and regions of biodiesel, many different specifications related to the items around the world, including the United States (ASTM D 6751), just discussed have been introduced into standards. There are Europe (EN 14214), Brazil, South Africa, Australia and else- often methods that have been developed by oleochemical asso- where. This article details the specifications in biodiesel stan- ciations and societies, such as the American Oil Chemists’ So- dards in ASTM D 6751 and EN 14214, the standards com- ciety, that may be more suitable. monly used as reference or base for other standards, and their The present article categorizes biodiesel analysis according analysis. Table 1 lists the specifications in the ASTM biodiesel to the nature of the materials or properties to be analyzed. Al- standard, and Table 2 gives corresponding information for the though the standard methods used for analyzing the various European standards, both for diesel fuel and for heating oil use. specifications will be mentioned, emphasis is placed on meth- For some specifications, alternative methods may be used as ods discussed in the scientific literature. Some specifications in discussed in the standards. biodiesel standards are straightforward and there is no or only Biodiesel can also be used as heating oil. Accordingly, a very little discussion in the scientific literature when relating separate standard (EN 14213) exists in Europe for biodiesel them to biodiesel. that is to be used as heating oil. The specifications of EN 14213 Since potential contaminants of biodiesel can arise during *Address correspondence at USDA/ARS/NCAUR, 1815 N. University St., the transesterification reaction, it is important for biodiesel pro- Peoria, IL 61604. E-mail: [email protected] ducers to be able to monitor the status of biodiesel production Copyright © 2006 by AOCS Press 823 JAOCS, Vol. 83, no. 10 (2006) 824 REVIEW TABLE 1 ASTM Biodiesel Standard D 6751a Property Test method Limits Units Flash point (closed cup) D 93 130.0 min °C Water and sediment D 2709 0.050 max % volume Kinematic viscosity, 40°C D 445 1.9–6.0 mm2/s Sulfated ash D 874 0.020 max % mass Sulfur D 5453 0.0015 max (S15) 0.05 max (S500) % mass (ppm) Copper strip corrosion D 130 No. 3 max Cetane number D 613 47 min Cloud point D 2500 Report °C Carbon residue D 4530 0.050 max % mass Acid number D 664 0.50 max mg KOH/g Free glycerin D 6584 0.020 % mass Total glycerin D 6584 0.240 % mass Phosphorus content D 4951 0.001 max % mass Sodium/potassium UOP 391 5 max. combined ppm Distillation temperature, atmospheric equivalent temperature, 90% recovered D 1160 360 max °C aThe limits are for Grade S15 and Grade S500 biodiesel, with S15 and S500 referring to maximum sulfur specifications (in ppm). in order to recognize and correct any problems at an early The use of biodiesel/petrodiesel blends also has been in- stage. Accordingly, this article also summarizes results on creasing significantly. Therefore, the verification of blend lev- monitoring of the transesterification reaction. els is another important aspect of biodiesel analysis. Different TABLE 2 European Biodiesel Standards EN 14214 for Vehicle Use and EN 14213 for Heating Oil Use Limits Property Test method EN 14214 EN 14213 Unit Ester content EN 14103 96.5 min 96.5 min % (mol/mol) Density; 15°C EN ISO 3675, EN ISO 12185 860–900 860–900 kg/m3 Viscosity; 40°C EN ISO 3104, ISO 3105 3.5–5.0 3.5–5.0 mm2/s Flash point EN ISO 3679 120 min 120 min °C Sulfur content EN ISO 20846; EN ISO 20884 10.0 max 10.0 max mg/kg Carbon residue (10% distillation residue) EN ISO 10370 0.30 max 0.30 max % (mol/mol) Cetane number EN ISO 5165 51 min — Sulfated ash ISO 3987 0.02 max 0.02 max % (mol/mol) Water content EN ISO 12937 500 max 500 max mg/kg Total contamination EN 12662 24 max 24 max mg/kg Copper strip corrosion (3h, 50°C) EN ISO 2160 1 — degree of corrosion Oxidative stability, 110°C EN 14112 6.0 min 4.0 h h Acid value EN 14104 0.50 max 0.50 max mg KOH/g Iodine value EN 14111 120 max 130 max g I2/100 g Linolenic acid content EN 14103 12.0 max — % (mol/mol) Content of FAME with ≥4 double bonds 1 max 1 max % (mol/mol) Methanol content EN 14110 0.20 max — % (mol/mol) MAG content EN 14105 0.80 max 0.80 max % (mol/mol) DAG content EN 14105 0.20 max 0.20 max % (mol/mol) TAG content EN 14105 0.20 max 0.20 max % (mol/mol) Free glycerine EN 14105, EN 14106 0.020 max 0.02 max % (mol/mol) Total glycerine EN 14105 0.25 max — % (mol/mol) Group I metals (Na + K) EN 14108, EN 14109 5.0 max — mg/kg Group II (Ca + Mg) prEN 14538 5.0 max — mg/kg Phosphorus content EN 14107 10.0 max — mg/kg Cold filter plugging point EN 116 — °C Pour point ISO 3016 — 0 max °C Heating value DIN 51900-1 DIN 51900-2 DIN 51900-2 — 35 min MJ/kg JAOCS, Vol. 83, no. 10 (2006) REVIEW 825 methods for various situations have been developed, including GC using an FID in both ASTM D 6751 and EN 14214. ASTM detection of the blend level during use in an engine. Therefore, D 6751 uses ASTM D 6584, whereas there are several specifi- this article will also deal with blend level detection. cations in EN 14214 using GC-based methods. Methyl hep- tadecanoate is a common standard for FA components, al- though the stability of standard solutions is an issue (8); freshly RESULTS AND DISCUSSION prepared solutions should be used, and pyridine may be more Analysis of production-related and “natural” biodiesel conta- suitable as solvent than heptane. These aspects have found the minants. During the transesterification process, intermediate most attention in the scientific literature, and the GC methods MAG and DAG are formed, small amounts of which can re- in standards are often based on this literature.
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