The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

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The Phvsical & Chemical Characterization of Biodiesel Low w Sulfur Diesel Fuel Blends Sponsored by the National Biodiesel Board University of Missouri December 30,199s Final Report Principal Investigator Leon Schumacher and Research Associates Anand Chellappa, Will Wetherell, & Mark D. Russell

Transcript of The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

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The Phvsical & Chemical Characterization of Biodiesel Low w Sulfur Diesel Fuel Blends

Sponsored by the National Biodiesel Board University of Missouri

December 30,199s Final Report

Principal Investigator Leon Schumacher

and

Research Associates Anand Chellappa, Will Wetherell, & Mark D. Russell

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Executive Summary . . . . . . . . ..__._..._........__..._._.................. i.............. 1

1. INTRODUCTION...........................,.............................;

2. OBJECTIVES... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..~

3. RESULTS,RNDINGS. . . . . . . . _ . . . . . . _ . . . . _ . . . . . _ . . . . . . . . . . . . 3

3.1 A4STM Test Methods Selection ........................................ 3

3.2 Securing Fuel for Testing ............................................ -t

3.3 Preparation of Blends ............................................... 4

3.4 Analvsis and Oualitv Assurance ........................................ 4 3.5 Comnarison of Phvsicai\Chemical Properties .............................. 4

3.5.1 Refractive Index ............................................ 5

3.52 Fattv Acid Methvl Ester FAME) content ......................... 1 3.5.3 Distillation Curve ........................................... 5 3.5.4 Densim ................................................... 6 2.5.5 APIGravitv ............................................... 6

3.5.6 Cloud and Pour Points ....................................... 6 3.5.7 Cold Filter Plug Point ........................................ 6 3.5.5 FlashPoint ................................................ 7 3.5.9 Corrosion ................................................. 7 3.5.10 Viscosin, .............................................. ...7 3.5.11 Heat ofCombustion ........................................ 7

3.5.12 CetaneNumber ............................................ 7 3.5.13 Aromatics Content ......................................... 8

3.5.14 Olelinic Content ........................................... 8 3.5.15 Parafkls Content .......................................... 8 3.5.16 Carbon Content ........................................... 8 3.5.17 Hvdrogen Content ......................................... 9 3.5.18 OxvgenContent ........................................... 9 3.5.19 Sutir Content ........................................... .9 3.5.20 Neutralization Number ...................................... 9

3.5.21 IodineValue ............................................. 10 3.5.22 Conrad Carbon Residue .................................... 10 3.5.23 Ash Content ............................................. 10

4. CONCLUSIONS OF TIXIS PROJECT. ....................................... 10 Table 5. Summary of properties that were analyzed ........................... 12

Appendix A Fuel Properties (Tables 1 and 3) . . . _ . _ _ . . . . . . . . . . . . . _ _ . . . . . . . . _ . . . _ . . . . . . . 13

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Appendix B Regression Analysis Finding (Tables 2 and 3) . . . . . . . . . . _ . _ . . . . . . . . . . . . . . . . . . 14

Appendix C Certification Diesel Fuel Graphs . . . . . _ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . _ 15

Appendix D Locally Purchased Diesel Fuel Graphs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

Appendix E Data Forwarded by Cleveland Technical Center . . . . . . . _ _ . . . . . , . . _ . . . . . . . . . 17

Appendix F Cleveland Technical Center Quality Assurance Report . . . . . . . . . . . . . . . . . . . . . . . . . IS

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The Physical Characterization of BiodieseU Low Sulfur Diesel Fuel Blends

Sponsored by the National Biodiesel Board University of Missouri

December 30,1995 Final Report

Executive Summary

The University of ?+fissouri Department of Agricultural En-tiesring was contracted to examine the physical characteristics of biodiesel when mixed with low 4fi-x diesel tieI. Engine manufacturers remain concerned about the physical and chemical makeup of the fuel used to power the eqgines that they manufacture and sell C ummins Engine Company is particularly interested in the oxidative stability, thermal stability, cold flow propekes, and water separability of each respective blend.

Cummins, the EPA and the National Renewable Energ Laboratory requested that speciiic characteristics about the biodiesel and biodiesel blends be well documented. Their suggestions enabled the Agricultural Engineering Department to compile the list of physical and chemical characteristics found in Table 5 of this final report.

Anand Chellappa prepared three identical samples of 0, 20, 30, 50, 70, and 100 percent by volume blends using certikation diesel fuel purchased from Phillips 66. Two of these samples were analyzed by Cleveland Technical Center. The third sample remains on campus for backup purposes. Will Wetherell purchased petroleum diesel fuel local(v from MFA Oil Company. Will prepared three identical samples using the same percent by volume blend concentrations. TWO of these samples were analyzed by Cleveland Technical Center. The third sample remains on campus for backup purposes.

Anand Chellappa determined the pour point, cloud point, fatty acid content, refractive tide% viscosity, density and specdic gravity for the certification diesel-biodiesel blends. Cleveland Technical Center analyzed the balance of the certikation diesel-biodiesel chemical blend

properties found in Table 5. Cleveland Technical Center analyzed &I the diesel-biodiesel chemical blend properties found in Table 5 for the fuel blends that were prepared using the diesel fuel purchased from MFA Oil Company.

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The values associated with the chemical character&&s were systematically identified. Specific objectives of the project involved assessing these properties with 0, 20, 30, 50, 70, & 100 percent biodiesel blends. Regression analysis was conducted’with these data and it was determined that simple mathematical interpolation methods could be used to predict some of the characteristics. For example, the cloud and pour points that were measured varied in a linear fashion with the amount of biodiesel blended with the certification diesel fkeL Therefore it appears that simple mathematical interpolation could be used to estimate or predict the cloud and pour point characteristics for a _tien blend of diesel fuel and biodiesel, provided the researcher is able to determine the cioud and pour points of the parent fuels.

Respectfully submitted,

Leon Schumacher Principal Investigator

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1. INTRODUCTION. . .

Research funded by the National Biodiesel Board has shown that an engine tided with a 20

percent biodieseK30 percent low sulfix diesel blend exhibited exhaust emission levels that are much lower than that obtained when the engine was fueled with 100 percent low sulfirr diesel fuel. The potential exists that a 70 percent biodieselG0 percent low sulfkr diesel fuel blend could quaiiry as an alternative fire1 for federal fleets that have been mandated to use alternate fuels. Such an increasing interest in blended fuels calls for detailed information concerning the physical and chemical properties of fuel blends that range f?om 100 percent biodiesel to 100 percent low sulfur diesel me!. This knowledge would facilitate a more effective commercialization of biodiesel as a me1 for modem diesel en-ties.

For the most part, properties have been estimated on a proportional basis (proportional to content of biodiesel in the blend) between the properties of 100 percent biodiesel and 100 percent low sulfur diesel fiteL However, properties do not always change in a linear fashion with blend composition. As an example, Van Gerpen (1994) found that flashpoint changed in a non-linear fashion when increasing the concentration of biodiesel in the fuel. In this project, various blends of biodiesel and low sulfur diesel me1 were systematically characterized, so that correlations between the fuel properties could be derived.

2. OBJECTIVES.. .

The overall goal for this research activity was to characterize various biodieseUlow sulfur diesel fuel biends. Specific activities that were conducted to attain this goal are listed below:

1. Experimental measurement of fuel related variables, as outlined by the fuels division of the EPA, for blends of 20, 30, 50, and 70 percent biodiesel/diesel fuel blends.

2. Analysis of the data obtained to determine whether the variables vary in a linear fashion with blend composition Corn 100 percent biodiesel fuel to 100 percent low sulfix diesel fuel.

3. To determine if one can accurately predict a range of values that can be expected for the various fire1 related variables, in blends ran-&g from 100 percent biodiesel fuel to 100 percent low sulfk diesel fuel.

4. The data were analyzed using statistical methods to provide a measure of accuracy of the experimental procedures that were followed.

3. RESULTS/FINDINGS.. .

3.1 ASTM Test Methods Selection The physical and chemical properties were identified in the work proposed by MU. The ASTM

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test method that would be used to determine these qualities are outlined in Table 5. Rich Heiden of Heiden and Associates and James Gardner, NBB subcontractors, reviewed these test procedures and reponed that these were adequate to assess the physical and chemical characteristics of the biodieseVdiese1 fuel blends.

3.2 SecurinF Fuel for Testing The me1 used to prepare the blends for our Batch 1 analysis was low sulfur Xi! diesel certification fuel. This was procured ii-om Phillips 66 Company in Bagor, Texas. The low suifk #2 diesel used to prepare Batch 2 for analysis was purchased locally from MZFA Oil in Columbia, MO. The biodiesel fuel was manufhcrured by Proctor & Gamble and procured f?om Midwest Biofiels.

3.3 Freuarstion of Blends When preparing the blends for this analysis, the specihc gravity (gramsIliter) of the parent fkel was used to insure that each blend was a 20, 30, 50 or 70 volume percent blend ofbiodiesel and petroleum diesel fuel. These blends were prepared using a Sartorius digital balance that is accurate to 0.1 mg. This method of preparing a blend is commonly used when preparing small blends (volume) of a _&en liquid. \

3.1 Analvsis and Oualitv Assurance Anand Chehappa determined the pour point, cIoud point, fatty acid content, refractive index, viscosity, density and specific gravity for the certification diesel-biodiesel blends. Cleveland Technical Center analyzed the balance of the chemical properties found in Table 5 for the biodiesel/certitication diesel fuel blends. Cleveland Technical Center analyzed & the chemical properties found in Table 5 for the biodiesel/diesel fuel blends that were purchased f?om MFA Oil company.

Cleveland Technical Center performed quality assurance tests to determine the repeatability of the tidings the reported for each blend. A summary of this report can be found in Appendix F. As noted in this report, ASTM DS6, D93, D130, D3338, D613, D13 19, D4294, D4S2, D664, D2075, and DIS9 were re-analyzed and the results of each second arklysis can be found in this report.

3.5 ComDarison of Physical\Chemical Prooerties Linear regression analysis was used to determine the relationship between the blend and the chemicaUphysica1 characteristics that were evaluated as a part of this investigation. The ‘R’ ” of each analysis was examined to determine the strength of each relationship. Variables that had an R’ that was less than .950, although strongly correlated, were deemed to have curvilinear tendencies. This tendency is clearly evident as one reviews the graphs that are found in Appendix C and D of this report. As such, variables that had an R* that was less than .950 were deemed curvilinear. Simple interpolation of the chemical/physical properties of a biodieseYdiese1 fuel blend was not an appropriate when the R* was less than .950. a’ . . .._

‘.’ __

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3.5.1 Refractive Index

The refractive index of the mei samples was determined using an Abbe Digital Refractometer and a Haake Constant Temperature Bathe (precision 0.2”C). Ref?actie index was found to vary in a linear fashion with the amount of biodiesel bIended with the fuel The correlation coefficient R2 of the linear fit was found to be greater than 0.999.

An accurate reading concerning the concentration of the blend, however, can only be accomplished when the refractive index of the parent fuels are predetermined.

3.5.2 Fam Acid Methvl Ester (FAME) content

Analysis of the fuel blends for Fatty Acid Methyi Ester (FAME) content was done using gas chromatographic (G-C) techniques. A 6’ X l/S” stainless stee1 column packed with GP 3% SP-23 10 / 2% SP-2300 on 100/120 Chromosorb was procured from Supelco Inc. This column was mounted in a Varian 3700 GC. The GC is equipped with a Flame Ionization Detector (FID) and is connected to a Hewlett Packard integrator. Calibration was accomplished using standard ester samples. The column oven temperature was maintained at 190’ C for 2 min and then ramped to 220’ C at 2’ C/m& with nitrogen as the carrier gas at 20 ml/min.

The FAME content was found to vary in a linear fashion with the amount of biodiesel blended with the ftreL The GC chain ler@ distribution (Oh by weight) averaged over two analysis for the biodiesel was:

CHAW %bv wt. c14:o 0.278 CI6:O 10.779 Cl&O 4.225 C18:l 20.253 ClS:2 54.096 C18:3 9.436 c2o:o 0.395

3.5.3 Distillation Curve

The data associated with the distillation points of the biodiesel blends are reported in Tables 1 and 3. The data varied in a curvilinear fashion as the concentration of biodiesel increased in relation to the petroleum diesel f$eL The linear regression coefficient R’ for each distillation point varied from 0.544 to .982 for the ZocafIy purchased low-sulfur diesel fuel (Table 4). The linear correlation coefficient for each distillation point of the certification diesel fuel ranged from .8 11 to .95 1 (Table 2) . Based on this analysis a simple mathematical interpolation is not an adequate method to determine the distillation curve of a biddiesel blend. Chemical analysis procedures or curvilinear regression analysis procedures must be used to determine the distillation-curve of a biodieseVdiese1 fuel blend (see Figures 1, la, 22, & 22a.).

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3.5.4 Densirv

Anand Chellappa used a quartz thermometer (Hewlett Packard) which has an accuracy of 0.00 1” C, and a Fisher Scientific thermostat for accurate temperature controL A Canon-Fenske viscometer was used to determine these characteristics.

Density was found to vary in a curvilinear fashion as the concentration of biodiesel increased in reiation to the petroleum diesel fuel The correlation coefficient R’ of the curve fit was found to be greater than 0.999. In other words, simple mathematical interpolation is not an adequate method to determine blend density. Chemical analysis procedures or curvilinear regession analysis procedures must be used to determine the density of a biodiesel/diesel fuel blend (see [email protected] 2 & 23).

3.5.5 API Gravitv

The data associated with the API Gravity of the biodiesel blends is reported in Tables 1 and 3. The data varied in a linear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fuel. The linear correlation coefficient R2 for API Gravity was .994 for the locally purchased low sulfur diesei me1 (Table 4). The linear correlation coefficient R2 for the certiiication diesel fuel was .999 (Table 2). A simple mathematical interpolation of the data, providing one knows the API Gravity of the blendstocks, can provide a good estimation of the calculated API Gravity for a biodiesel blend ( see Figures 4 & 25).

3.5.6 Cloud and Pour Points

Cloud point and pour point measurements for 0, 20, 30, 50, 70, and 100 percent biodieseudiesel fuel blends were carried out following the ASTM D2500 and D97 procedure. Three trials were carried out for each blend. Both cloud point and pour point varied in a linear fashion with the amount of biodiesel blended with the petroleum diesel fuel. The correlation coefficient R2 was found to be greater than 0.99 (see Figures 5, 6, 26, & 27). A simple mathematical interpolation of the data, providing one knows the cloud and pour points of the blendstocks, can provide a good estimation of the cloud and pour points for a biodiesel blend.

3.5.7 Cold Filter Plug Point

The data associated with the cold hlter plug point of the biodiesel blends are reported in Tables 1 and 3. The data varied in a curvilinear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient R* for the cold filter plug point of the certi&ation.diesel fuel was .964 (Table 2). The linear regression correlation coefficient R’, for the locally purchased low sulfur diesel fuel was .92 1 (Table 4). Simple mathematical interpolation is not an adequate method to determine the cold flter plug point of a biodiesel blend (see P&res 7 & 28). - ,,’ ej

.1 . . . -,

_

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3.5.8 Flash Point

The data associated with the flash point of the biodiesel blends are reported in Tables 1 and 3. The data varied in a cur+bnear fashion as the concentration ofbiodiesel increased in relation to the petroleum diesel me1 The linear regression correlation coefficient R’ for the flash point of the certification diesel fuel was .759 (Table 2). The linear regession correlation coefficient R’ for the locally purchased low sulfur diesel fuel was .809 (Table 4). Simple mathematical interpolation is nor an adequate method to determine the flash point of a biodiesel blend (see Fi,g.nes 8 & 29). Chemical analysis procedures or curvilinear regression analysis procedures must be used to determine the flash point of a biodiesel/diesel fuel blend.

3.5.9 Corrosion

The data associated with corrosion of the biodiesel blends are reported in Tables 1 and 3. The data reported concerning corrosion was 1A regardless of the blend or the diesel fuel that was used to prepare the blend. In this case, mathematical interpolation is a mute effort.

3.5.10 Viscositv

The data associated with the viscosity of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration of biodiesel increased in relation to the petroleum diesel meL The linear regression correlation coefficient R2 for the viscosity of the certiilcation diesel fuel was -962 (Table 2). The linear regression correlation coefficient Rz for the locally purchased low s&k diesel meI was ,99 1 (Table 4). Simple mathematica.I interpolation can be used to estimate the viscosity of a biodiesel blend (see Figures 9 & 30).

3.5.11 Heat of Combustion

The data associated with heat of combustion of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration ofbiodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient R2 for heat of combustion of the certihcation diesel fire1 was .990 (Table 2). The linear regession correlation coefficient R’ for the locally purchased low suIfix diesel fuel was .999 (Table 4). Simple mathematical interpolation can be used to estimate the heat of combustion of a biodiesel blend (see Figures 10 & 31).

3.5.12 Cetane Number

The data associated with the cetane number of the biodiesel blends are reported in Tables 1 and 3. The data varied in a curvilinear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient R’ for the cetane number of the certification diesel fuel was .595 (Table 2). The linear regression correlation coefficient R2 for the locally purchased low sulfur diesel fuel was .795- (Table 4). Simple mathematical

’ interpolation is not an adequate method to determine the cetane number of a biocliesel blend (see

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Figures 11 & 32). Cetane engine test procedures (D6 13) must be used to determine the cetane number for a given biodiesevdiesel mei blend.

3.5.13 Aromatics Content

The data associated with the aromatics content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration ofbiodiesel increased in relaticn to the petroleum diesel fkeL The linear regression correlation coefficient R’ for the aromatics content of the cetication diesel fuel was .998 (Table 2). The Linear regression correlation coefficient R2 for the locally purchased low sulfur diesel fuel was .997 (Table 4).

This test procedure (D13 19) does not measure the “real” aromatics associated with a biodiesel blend. D 13 19 mistakenly identiiies the double bonds commonly found in biodiesel as the double bonds (normally associated with benzene, or aromatics) that are attached to the diesel fuel molecule. Tn short, simple mathematical interpolation is not appropriate when D13 19 is used to determine the aromatics of a biodiesel/diesel fuel blend GC analysis procedures should be considered when determirk, - the aromatics of a biodiesel blend (see Figures 12 & 33).

3.5.14 Oleiinic Content

The data associated with the ole&ic content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a curvilinear f&&ion as the concentration of biodiesel increased in relation to the petroleum diesel fkeL The linear regression correlation coefficient R* for the olefinic content of the certification diesel fuel was .I336 (Table 2). The linear regression correlation coefficient R2 for the locally purchased low sulfur diesel fuel was -947 (Table 4). Simple mathematical interpolation is not an adequate method to estimate the oleSnic content of a biodiesel blend (see Figures 13 & 34).

3.5.15 ParafEns Content

The data associated with the paraflins content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear-fashion as the concentration ofbiodiesel increased in relation to the petroleum diesel meL The linear regression correlation coefficient R* for the parafFins content of the certikation diesel fuel was .998 (Table 2). The Linear regression correlation coefficient R* for the locally purchased low suLfurdiesel fuel was .997 (Table 4). Simple mathematical interpolation is an adequate method to estimate the parafEns content of a biodiesel blend (see Figures 14 & 35).

3.5.16 Carbon Content _. : ._ L.

The data associated with the carbon content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration ofbiodiesel increased in relation to the petroleum diesel fueL The linear regression correlation coefficient R* for the carbon content of the certification diesel fuel was .996 (Table 2). .The L&ear regression correlation coefficient R* for

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the locally purchased low .suKr diesei fbel was .985 (Table 4). Simple mathematical interpolation should provide a good estimate of the carbon content of a biodiesel blend (see Fi-gures 15 & 36).

3.5.17 Hvdrogen Content

The data associated with the hydrogen content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient Rz for the hydrogen content of the certification diesel fuel was .990 (Table 2). The linear regression correlation coefficient R?- for the locally purchased low sulfkr diesel fuel was .946 (Table 4). Simple mathematical interpolation should provide a good estimate of the hydrogen content of a biodiesel blend (see Fi-mes 16 & 37).

3.5.18 Oxvgen Content

The data associated with the o,xygen content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient RZ for the oxygen content of the certification diesel mei was .996 (Table 2). The linear regession correlation coefficient R for the locally purchased low sulfkr diesel fuel was .976 (Table 4). Simple mathematical interpolation should provide a good estimate of the oxygen content of a biodiesel blend (see Figures 17 & 38).

3.5.19 Sufir Content

The data associated with the m&r content of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration ofbiodiesel increased in relation to the petroleum diesel fuel. The linear regression correlation coefficient R* for the su.lfk content of the certikation diesel fuel was .972 (Table 2). The Linear regression correlation coefficient R* for the locally purchased low sulfix diesel fuel was .968 (Table 4). Simple mathematical interpolation should provide a good estimate of the sulfur content of a biodiesel blend (see Figures 18 & 39).

3.520 Neutralization Number

The data associated with the neutralization number of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration ofbiodiese1 increased in relation to the petroleum diesel fkeL The linear regression correlation coefficient R* for the neutralization number of the certification diesel he1 was .983 (Table 2). The linear regression correlation coefficient R’ for the locally purchased low sulfiu diesel fuel was -983 (Table 4). Simple mathematical interpolation should provide a good estimate of the neutralization number of a biodiesei blend (see Figures 19 & 40).

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3.5.21 Iodine Value

The data associated with the iodine value of the biodiesel blends are reported in Tables 1 and 3. The data varied in a linear fashion as the concentration of biodiesel increased in relation to the petroleum diesel fkeL The linear regression correlation coefficient Rz for the iodine value of the certitication diesel fuel was -968 (Table 2). The linear regression correlation coefficient R’ for the locally purchased low sulfur diesel fuel was .999 (Table 4). Simple mathematical interpolation should provide a good estimate of the iodine value of a biodiesel blend (see Figures 20 & 4 1).

Z 3.22 Conradson Carbon Residue

The data associated with the carbon residue ofthe biodiesel blends are reported in Tables 1 and 3. The linear regession zmlysis of the carbon residue for the certification diesel fuel and for the locally purchased low sulfur diesel Fidel was not statistically si@ticant. Simpie mathematical interpolation is not an adequate method to determine the Conradson carbon residue of a biodiesel blend (see Fi_gure 2 1).

3.5.23 Ash Content

The data associated with the ash content of the biodiesel blends are reported in Tables 1 and 3. No differences were noted, regardless of the blend. As such, mathematical interpolation is a mute e%ort.

4. CONCLUSIONS OF.THIS PROJECT.. . .

b. -

Industry (OEMs) and the Environmental Protection Agency requested information concerning the physical and chemical properties ofblends that ranged Corn 100 percent biodiesel to 100 percent low sulfur diesel fireL It was their perception that this knowledge would facilitate the commercialization of biodiesel as a fuel for modem diesel en_gines.

In this project, various blends of biodiesel and low sulfur diesel fuel were systematically characterized, so that correlations between the fuel properties could be derived. As was noted in the literature, the chemical properties of biodieseVdiese1 fuel blends do not always change in a linear fashion (Van Gerpen, 1994). -. ,.. ‘.._.’

E.xperimental blends of 0,20, 30, 50, 70 and 100 percent b&die&l were prepared by the researchers. Ceitification diesel meI arid locally purchased diesel fuel (MFA Oil Company) were blended with the biodiesel on a volume basis. Fuel related variables, as &tIined by the fuels division of the EPA, were analyzed by the University of Missouri Researchers and by Cleveland Technical Center. A total of seven chemical characteristics were analyzed by MU researcher Anand ChelIappa for the biodiesel/certifkation diesel Fidel bIends. The balance of the analysis for the biodieseYcertification diesel fire1 blends were completed by Cleveland Technical Center.

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Cleveland Technical Center performed all the analysis for the biodieseflocally purchased diesel he1 blends.

Several variables were found to vary in a linear fashion. The linear regression coefficients as noted in Tables 2 and 4 were quite high. However, one must interpret the linear regression coefficients (‘X2 “) with care. The ‘%I?’ for this study was small Only two different diesel fuels were used (certification LSD +2 and a locally purchased LSD g2). Further, only number two diesel fuel was tested. In short, additional analysis will be needed with a variety of diesel fuels (each with slightly different chemical properties) that are commonly available to the user. This would allow the researchers to develop a model that would accurately predict the chemical property in question.

Based on the aforementioned limitations of this study, several chemical characteristics of the bioclieseYdiese1 fuel blend will require additional data analysis due to the curvilinear tendencies noted in the data. The additional data will facilitate the statistical analysis of the data and eventually allow researchers to develop a curvilinear model that can be used to accurately predict these chemical characteristics for a given blend. Chemical characteristics that may require additional data to fhcilitate the development of a prediction mode1 include: distillation, cold filter plug-tig point, flashpoint, cecane number, olefinic content, and carbon residue.

It appears that simple mathematical interpolation (rather than linear regression) can be used to estimate some of the chemical characteristics for a given biodieseVdiese1 fuel blend. If the researcher lmows the chemical characteristic in question of the “parent” or ‘“olendstock” fuels, the following chemical characteristics can be mathematically interpolated: density, specsc gravity, MI gravity, viscosity, heat of combustion, pa&ins content, carbon, hydrogen, oxygen, neutralization number, sulfur, cloud point, pour point, and iodine value.

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Table 5. Summary of properties that were anaiyzed for each respective blend.

Phvsical Prouerties ASTM No.

1.

2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Dkxiition Initial BP, degrees C TlO, degrees C T50, degrees C T90, degrees C End BP, degrees C Density Specific Gravity API Gravity Cloud Point Pour Point Cold Filter Plug Point Flash Point corrosion Viscosity @ 40C Heat of Combustion Cetane Number

Chemical Composition 1. Aromatics Content (volume percent) 2. Olefinic content (volume percent) 3. Pa&ins content (volume percent) 4. Carbon and Hydrogen 5. Hydrogen 6. Oxygen(weight percent) 7. Sulfbr (iu % wt levels) 8. Neutralization Number 9. Iodine Value of Drying oils and Fatty Acids 10. Carbon residue 11. Ash

D 86

D 1298 D 1298 D 257 D 2500 D 97 D 4539 D 93 D 130 D 445 D 3338 D 613

D 13i9 D1319 D 1319 D 5291 D 5291 D 5291 D 4294 D 664 D 2075 D 189 D 482

Note. Physical properties 3 and 6 are used only for petroleum diesel fuels.

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‘I’nble 1. CllcniicnVl’llysic:11 Properties of Reference l)iesel/l~iotlicscl IWmls

ASTM No. Snulple 6 Simple 2 Simple 3 Salllple 4 Sillllplc 5 Sample I DFIOO LID20 13D30 BD50 131~70 BDIOO 0 20 30 50 70 100

Physical Compdsilioi~ I. Distnllatiorl - degrees C

IBP TIO 1‘50 T90 EBP

2. Detlsity 3. Specific Gravity 4. API Gravity 5. Cloud Poht “C 6. Pour Pohlt “C 7. Cold Filter Plug Poillt 8, Flash Poillt 9. Corrosioii IO. Viscosity @ 40 “C I I. Hent of Combustioil 12. Cetalle Number

Chemical Coiiipositioll I. Aromatics Colltellt (volume perceul) 2. OleTulic Cotrtelit (volume percellt) 3. Paraflitls Collleiit (volume percetll) 4. Carbon (weight percent) 5. I lydrogell (weight percetlt) 6. Oxygen (weight percellt) 7. Sulfur (in % weigh levels) 8. Neutralization Number 9, lodim Value IO. Carbon Residue

1~86

Dl298 D1298 D287 D2500 D97 D4539 D93 D130 D445 D3338 D613

D1319 Dl319 D1319 D5291 D5291 D5291 D4294 D664 D2075 Dl89

I59 197 192 201 222 229 227 243 259 273 282 312 309 328 332 339 336 342 342 343 0.8393 0.8478 0.8509 0.8586 0.8399 0.8485 0.8515 0.8592 36.9 35.3 34.7 33.2 - 12.2 -10 -7.7 -5.5 -16.1 -13.3 -I 1.6 -8.3 -2 4 6 10 I65 170 175 I80 IA IA IA IA 2.9 2.99 3.1 I 3.39 I9672 18981 I8681 I8368 47. I 51.9 47.8 49. I

28.3 4 I.3 4X.6 64. I 2.6 1.9 I.5 I.6 69. I 56.8 49.9 34.3 86.6 84.58 83.74 81.59 13.22 12.98 12.9 12.62 0.15 2.79 3.91 6.49 0.034 0.03 I 0.026 0.022 0.01 0.07 0. I4 0.25 18.4 36.6 43. I 61.8 0.02 0.03 0.02 0.03 co.01 0.02 0.01 001

206 293 256 326 323 334 33x 350 350 356 0.8675 0.8799 0.8682 0.8805 31.5 29.2 -3.3 I.1 -6.7 0 12 24 190 270 IA IA 3.69 4.3 I7850 17041 50.9 55

80.5 99.6 1.2 I 18.3 1 80.05 76.4 I 12.29 12.05 9.29 12.12 0.02 0.014 0.39 0.62 81.3 133.9 0.02 0.01 0.02 co.0 I 1 I. Ash D482

Page 17: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Squ;lretl, Conshnt, Stnntl:lrtl Error of Constant, S Coefficients, St;lntlwtl Error of Coefficients for Reference ~iesel/l~iorliescl Blends.

Variables R Squared Conslant Standard Error of Constant

X Coefficients Standard Error of Coefficienls

I. Initial Boiling Point ‘. TIO (Distillation) /. T50 (Distillation) I. T90 (Distillation) ;. End Boiling Point 1. Density ‘. Specific Gravity :. API Gravity ). Cloud Point IO. Pow Point I I. Cold Filter Plug Poiul 12. Flash Point 13. Viscosity @ 40 “C 14. Heat of Combustion I 5. Cetnne Number IO. Aromatics Conlenl 17. Oletinic Content 18. Parallins C0nlc11l 19. Carbon !O. Hydrogen ! I. Oxygen !2. Sulfur !3. Neutralization Number .!4. Iodine Value !5. Carbon Residue

0.811275 157.7786 21.78197 1.116031 0.811275 0.827791 206.3588 IS. IO466 0.9809 I6 0.223702 0.948089 260.7888 7.654598 0.808397 0.094581 0.856347 3 16.7964 5.8451 17 0.352672 0.072223 0.951018 336.2799 1.745587 0.190076 0.021569 0.998905 0.839141 0.000542 0.000404 6.7E-06 0.998774 0.839774 0.000573 0.000404 7. I E-06 0.999 I69 36.92926 0.089812 -0.07695 0.001 I I 0.994597 -12.2094 0.393862 0.132061 0.004867 0.98572 -16.3547 0.759955 0. I5603 I 0.00939 0.964925 -1.78626 I .849283 0.239695 0.02285 0.758884 149.0712 2 I .59069 0.946565 0.266775 0.962 2.752239 0.115174 0.014321 0.001423 0.990288 19563.25 100.7264 -25. I35 I 1.24458 0.594762 47.49008 2.08572 0.062443 0.02577 I 0.998 I 86 27.58779 1.258012 0.72916 0 015544 0.836162 2.279135 0.257063 -0.01435 0.003 I76 0.99672 I 69.79517 I.627956 -0.70177 0.0201 I5 0.996423 86.6675 I 0.242782 -0.10013 0.003 0.989503 13.22491 0.050778 -0.01218 0.000627 0.996077 0.321934 0.308689 0.12155 0.003814 0.97239 0.033534 0.001369 -0.0002 1.7E-05 0.98302 -0.03364 0.033 I28 0.006229 0.000409 0.967886 12.25064 8.233624 I.1 17023 0.101735 0.303098 0.0268 I9 0.007026 -0.000 I I 8.7E-05

ote: Nwnber of Observations is 6 per variable Degrees of Freedom is 4 per variable

Page 18: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Appendix B

Regression Analysis Findings

14 _ . .

Page 19: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

‘nl,lc 3.

~IlCllliC~llI’llySiCill i’ropertics of Loc:llly I’iwcllnsetl Low Sulfur Dicsel/Uiotlicscl Illc~~cls.

ASTM No. Smple I2 Satilple 8 Simple 9 Salllple IO Sarllplc I I Saliiple 7 DFIOO BD20 BD30 BDSO BD70 BDIOO 0 20 30 50 70 100

‘hysicrl Coiiiposilioii D86 Dislallalioli - degrees C 170 177 I80 197 204 311 IBI’ 209 214 219 236 260 329 ‘r I 0 259 280 291 302 316 334 1'50 317 332 334 339 339 351 T90 343 344 344 342 344 351 EBP Dl298 0.8469 0.8545 0.8577 0.866 0.8703 0.885

‘. Densit ry

Dl298 0.8473 0.855 0.8581 0.8665 0.8708 0.8855 ‘. S eci IC Gravity

i I)287 35.5 34 33.4 32 31 28.3

I. A I Gravity D2500 IX 20 I8 26 ;. Cloud Point “C D97 ‘to -15 5 IO 1; 1. Pour Point “C

%:‘” 6 4 14 f:

1, Cold Filler Plug Point 130 2

;:5 I60 E5 310 !. Flash Point Dl30 IA IA I. Corrosioil D445 2.55 2.77 it7 3. I8 :ps5 z3 10. Viscosity @ 40 “C D3338 19682 I9156 I8957 18466 I7999 I7272 1 I. Heat of Coiiibuslioii D613 43.5 47.3 48.9 48.3 49.7 51.1 1 2. Cetarre Number

IJllemical Coin ositioii 6

Dl319 25.9 37.8 44.1 61.6 75.8 99.4 I. Aronlalics onteut (volume pelcenl) Dl319 4.2 3.1 3.2 2.2 ) Olefmic Coiiteilt (vohie percenl) Dl319 69.9 59. I 52.7 36.2 z;’ t ii ParaUins Coiileiil (volume perceiil) D529l 86.21 84.04 83.69 81.24 80.35 76.48 I. Carboll (weight erceiil)

P D529 I 13.4 12.91 12.66 12.45 12.41 Il.78

i. t lydrogeil (weig it percent) D529l 0.15 * 3.41 2.69 5.74 8.25 12.83 4. Oxygeli (weight percent) D4294 0.036

3’ 0.03 I 0.025 0.016 0.012

I. Sullilr (iri % wei 1111 levels) A

II664 0.01 0. I I 0.2 03 0.48 3. Nerltralizatioll umber D2075 20.5 43.9 53.6 7'). I 102.9 1~10.9 ‘). Iodine Value Dl89 <O.Ol co.01 co.0 I W.01 <O.Ol co.0 I IO. Cal boil Residue D482 co.0 I <O.Ol <O.Ol <O.Ol <O.Ol co.0 I I I. ASII

Page 20: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

IlC 4.

cl~tnretl, Constant, Stnntlnrtl Et-tw of Constant, S Coefficients, Stantl:wtl Error of Coefficients for the LociIlly Pli~cllilsetl Low Sulfur

,;cl FoeVIIiodiesel INends.

I iables R Squared Corlslalll Slantlard Error of Conslalll

X Coefficienls Standard Error of Coeffkienls

lnitinl Boiling Point TIO (Distillntiou) T50 (Distillation) T90 (Distillation) htl Boilirlg Poillt Density Specific Gravity API Gravity Cloud Poht

Pow Poinl Cold Filter Plug Point Flash Point Viscosity @ 40 “C Heat of Combustion Cetane Nunlber Aromatics Content Olefinic Content Paraffins Content Carbon f-lydrogen Oxygen Sulfur Neutralization Number loditie Value

0.776571 148.687 27.8858 I 0.887394 191.3588 17.02289 0.981605 264.2977 4.02568 I 0.887036 322.2799 4.188923 0.544238 340.7252 3.92924 I 0.99 I364 0.846747 0.001398 0.991398 0.841 I72 0.001398 0.9935 I9 35.50636 0.22803 0.689232 13.04326 3. I94302 0.847614 -16.2214 7.138221 0.921 I I3 3.608 142 2.296141 0.808795 103.1043 32.89228 0.99092 2.476463 0.058696 0.999627 19665.09 18.69526 0.795094 45.24097 1.320382 0.99705 23.78295 1.645922 0.947204 3.979389 0.282235 0.996908 71.94198 1.592108 0.985 I I 86.22308 0.466702 0.945991 13.276361 0.142819 0.975553 -0.0412 0.790459 0.9676 12 0.037351 0.00 I95 0.982934 -0.008 I7 0.024666 0.999251 19.253 I8 I.330131

1.284733 0.344558 1.180316 0.210335 0.7267 I8 0.04974 I 0.290076 0.05 I759 0.106107 0.04855 0.000370 I .7E-05 0.00037 I I .7E-05 -0.06977 0.002818 0.1 17557 0.039469 0.4 1603 I 0.0882 0.193893 0.02837 I 1.671756 0.4064 18 0.015153 0.000725 -23.9206 0.230999 0.064275 0.016315 0.747786 0.020337 -0.02954 0.003487 -0.70649 0.019672 -0.0938 I 0.005767 -0.014771 0.001764 0. I23397 0.009767 -0.00026 2.4E-05 0.004626 0.000305 I.2051 I5 0.016435

:: Nwuber of Observations is 6 per variable Degrees of Freedom is 4 per val iable

Page 21: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Appendix C

Certification Diesel Fuel Graphs

Page 22: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Distillation Curve ASTM D86

400 I -’ ; - .- .’ T ---

350 0

IBP

g 300 a, b 250 a,

TIO I

T50 d 200

150 T90 20 40 60 l . ..-

EBP Percent Biodiesel

Page 23: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

\ / ;‘\ i ! ; i : ;- -_--

\ \! 1 :

Page 24: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

._ :-

Gl co d

: I ;

i.

03 a

d d d w6 ._ .-

0

Page 25: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I ,

I 1 Y’ :

_ _ _- --.1- -7 . . ! --- _

I i /’

! I I I

1 I I

,--i-L

/ i;

---i-p--,-- -

i/ i,’ I

/I , ! I

_ L-:-#,~ ..- -

: / .a.--. -_!

I -

I - _ --. - -- -- --A-

m

Page 26: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

,s n n

8

,bl

0 0

cl

> k cn 6

, , I

-

Page 27: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

i

co

-.L-.--- _ - -.- ___ -----I.-- - /

/ -

! ._I _-_L .--mm---. _. .~- _--

:

1 I

‘; 1 -- --‘-‘. - - _. .-. ..- -.

I I ‘\., I---

I I / I \ \ ,

I :<i _ __ ..- +- _e -+- - .--.--

I

-_

I / I

i ’ _..- --- I. I

__ ____. _ i ._.~. --‘, ..__.. -. -+ --

I

-.

Page 28: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Cold Filter; Plug Point

25 ; :....

20 :

ASTM D4539

_ ._ _! -._ -

I--

_... _.- - --.

! -

I ---.-

.-----;,-/: A’

----i----- --

Percent Biodiesel

_-

Page 29: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Co m

IL 1--------.-.. ;-

: I

. . !

m

Page 30: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

i.

il : i ; ;

;

--.. .-. - ..___ ..I ‘-- -_j-. /- I --;-i .-,

Page 31: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

0 0 0 0 0 0 0 0 0 0 0 m 0 m 0 0 a CD co 00 c\1\ \ \ 7

Page 32: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

--

_-

/ --

I\ I

/ I ‘.., I 2.. ---L- --- -.-.- -.- --:...-;-

\-T-

I

--

_--

--.! .-..--A -

4aqLU?-TN, I . .

Page 33: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Aromatics Content ASTM 81319

1 00 _. _ .__ .,~__ . -- ._...

al I

E 60 .. ..---.- . -, 3 ,

; I

20 40 60 80 100 Percent Biodiesel

Page 34: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

.: -I-- -.__

: -. .---.-_~_-I_

!. I I. --:--- : - ._’ -_ ;I’.. -- .- -- --+ --.+ I

,/’

I ._

0 CA

0

Page 35: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

t

: ’ (I /

: ,,’ ,,’ I

--

--- -7 ,z: i I I

Page 36: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

’ : !- -- ---- - ---

) 1 I

/ I / i ! :

I

! . - --i

.+-l--;--+’ - - --.- --.. .- .A+--

; I

i

T

T

L

Page 37: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

0 co

.- __ _-

> I-

/ /

NC7 ti-

\1 m \ ,_-_-

‘9 IG .- c

Page 38: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

:

d- \

:

? . . ..___ I.. _--. .-- ----j... ;

\ \

L

__. - . - . -

I

;

__. ~.. ii--- - . .

! I !

4 -.. -_

I

---.

!.

\ ‘I

0 _

Page 39: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

7

' I

-.

/’

I I .L--..

ii

.i

:

-.

nl 0

d

I .

Page 40: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I :

i -4 1 I i i ;

,

4

- 8

.

I

‘- .- - ____- -.-.- -.. .

\

I--.-.- .

.I..----‘~- . .- -

--@I

_. I

Page 41: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

; I ‘\

,\: \,I

! I 3 I +---_

j / /

a

0 d- \

1

_ .-

I

I

; . ,

0 xv

..--.- 1

:

0 0 \

P

-I

Page 42: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Ii!1 1, ; ./ 1.:. ,,

‘,/ ,’

. ___.-

_-

Page 43: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Appendix D

Locally Purchased Diesel Fuel Graphs

Page 44: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

__ _-. --

->

n -

n a

0 0 \I

I --.i. --

l

0 0 0 0 0 u-l 0 m 0 ul

__

0 0 \

0 co

Page 45: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

-

-

-

-

I -

s .I a- 0 m

Page 46: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

-

s > a” l- t3 0

6

i ;

i -- --_ ~

-

-

.-_- i-

-

i !

-_ --_...

Page 47: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

>r

i-

T

T i.

I -.

I- t

0 co

i

u .- au

0 .- m

L7- --..-.--_-~-~..---- - -

>

! /

.!

j-- 2.

I

0 ;-- -..

Page 48: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...
Page 49: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

mm 0

,Qm ,a

s 0

0

-

I

1

I -

I

I

4 -

L-- _ .- -L---- .I-

I

I , _ _ . __ -.-.-- . L

saaJ%a

Page 50: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I

- :

I

0

I

.:

. .- .

i : I

4

0 0 0 \

I c;’

Page 51: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

c

-.

1- /

_.

I

1

.-

n I

- 7.

,

t a

_ _ _--a-

I

I

m-

LL I-. - 1.. I ..--. - .- - - .-

-..

- :I

Page 52: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I I

; ---.---I.

I

- -A..

I -_I-- !._

_.- ;.-...

-.

0 0 \

Page 53: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

0 CO

0 .- m z

Page 54: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

’ il : /:

! ’

I : ! . . _

I ,

;

- .

!

I- _:.

/ I

I

.- 1

0 0 0 co \

i’

_-_.

1

T

i

I

- .

I I I

I / I

.-j .- .- -...-- L.

0 0 0 0

.m 0 b b

‘.\ \

Page 55: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

!

I

1.

‘-

l

!

/

:

cl Lo

-

_-

-

. .

0 m

, .i . - -.- -L-- ;.---.-.- ..~ i

I /

Page 56: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Aromatics Content AST’h Dl319

100

--

- .._._ i- -.-. .-:.. - -..- ---. -- .-.-- - -I- ..~~_ -

80: $! :

‘! 60 3

.._-. -- f i...-- .-_-.._ .-.- .-_.. ; I..-.-. - -._- b.. -..~ .__ --.-. _

..’ /”

,’

.- _L.

I I

,,’

_ . .

! , . ’

r

- :.- . _ _ I

‘0 > 40

._’

/ Ic - I

,.I’ ” I L- _ -,~,-~- -. _--_ 1 ._-.-. .._._~ _.. L--_- _-

A.--’ ! 1 I I- ~-.. -- l

, -- _-_... -_.-.--- ----I-.---.----

40 60 80 100 Percent Biodiesel

Page 57: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

45 I 4

35 . 3

25 . 2

15 . I

Olefinic Content ASTM Dl319

+ ._..___ - -.. - -. . . . _... ~. -._ __-- -i ._-..._. ~_- .-.. i..-~.- . -...I --. .--..-_--i__ ..__ _ ________...__._....... _ _..

I I 1 I J ..__ -- _ _ ..- _ _ -. . J ..-. -..-- . ..__. 1... .- ----.-..I .._ - --. _ I _~~~ -. _~ , _. L .--...- - ._ __._..__ -__

0 20 40 60 Percent Biodiesel

80 100

Page 58: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

, I !

i I ’

-!._ -. j ;

I

. - . .__..- .- -.

---- I

I

I __L

/

I

I

--i. I

I I

I

I 4

I I

0

Page 59: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

s 0 0 s 0

_ ----L I

i :

) ! --.-L--L.

I ,’ -1’

_-- -- _._- -.. --

- -. -

e

Page 60: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

i* ‘C

0 0 - - - - . ~- -

:

-.--i---.i---- --i--. -; : , ;I I / /I : ! ! / ._ -! &.-- -+-- ---A-

/j i ’ i / .i’i 1 m 1 j : i :-,;,‘- -- ,. -. ..+ --. ----.. L ----1.

.’ I

-- I

CY

Page 61: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

0 co

1 / ;

/ : I

\ ,

.-

--

I . !

I

I

0 0.l

i-1. . . 1 .

0

I--- (00 ; I” !Eb F; L- .

Page 62: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

> I- I L- co 4

I-

i

Y I .

.‘L..

/ ~

0 0 \

0 co

3 0 .a>

-E .- a

i= al

s* iii

CL

0 N

0

Page 63: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

~--- - -- I

0 .- m .i - . .-- - -4

n > I- O

-!-

a, - _-_- -I-.---.--

j

I

I

I ! ..I.-----

- I 1 1 .~. I- O

c-9 N 7 0 d d

m d

.

Page 64: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I L

I

I ! :

: ;

,

i ..-.- 1 :

L i -- --

. I

1 ; i 1 I :

! .~- .I -- :.--i.. . !

0000 d-c\1000 \ \ ?.

.- ..--

Page 65: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Appendix E

Data Forwarded by Clevehnd Technical Center

17

.

Page 66: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DIVISION OF CONAM INSPECTION INC. 935 Sunshine Road Kansas City, KS 661151122 (913) 281-9881 (800) 332-8055 FAX: (9 13) 28 l-9885

January 05, 1996

Dr. Leon Shumacher University of Missouri Department of Agriculture Engineering 235 Agriculture Engineering Building Columbia, MO 65211

RI!: Purchase Order Number W 1693 8

Enclosed are the revised test results for the biodiesel fuel samples and used oil samples that your Department submitted to us for testing.

We have corrected the Cloud Point test method &om ASTM D-2300 to ASTM D-2500. Also, the distillation temperatures for samples 8-12 (Batch 2) have been converted from degree Fahrenheit to degree Centigrade.

If you have any questions after reviewing your test results please do not hesitate contacting me at (9 13) 28 l-988 1. Thank you for considering Cleveland Technicai Center for this project.

Respectfilly,

Laboratory Supervisor

Enclosures:

CLEVELAND, OH - KANSAS CITY, KS. PHOENIX. Ai! - LINDEN. NJ. GOLDEN VALLEY, MN - SPOKANE, WA - ATLANTA. GA l PORTLAND. OR Expert Lubrication and Fuel Analysis Services

Page 67: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNiCAL CENTER A DIVLSION OF CONAM /NSPECTlON INC. 9% Sunshine Road

Kansas City, KS 66115-i 1~

(913) 281-9881 (800) 332-8055 FAX: (913) 281-9885

BATCH #l SAMPLE 1 (CAN#102-103) 100% SOYDIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM D-86 IBP ASTM D-86 10 % ASTM D-86 50% ASTM D-86 90 o/o ASTM D-86 EP ASTM D-86

COLD FILTER PLUG POINT ASTM D-4539 FLASH POJNT ASTM D-93 CORROSION ASTM D-130 HEAT of COMBUSTION ASTM D-3338 CETANE NUMBER ASTM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFIN CONTENT CAREION CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 99.6

ASTM D-1319 -4 .o

ASTM D-1319 4.0

CARLO EIWA 76.41

CARLO ERE!A 12.05

CARLO ERBA 12.12 ASTM D-4294 0.014

ASTM D-482 co.01 ASTM D-664 0.62 ASTM D-2075 133.9 ASTM D-l 89 co.01

293 326 ,334 350 356 +24

270

1A 17,041

55.0

N-IL STRAW

N-IL

DEG C. DEG C. DEG C. DEG C. DEG C. DEG F. DEG F.

BTU/lb

VOL % VOL % VOL % ‘4vr % WT % ‘NT % TivT % w-r % rqKOH/g

‘w-r %

CLEVELAND, OH l KANSAS CITY, KS - PHOENIX. AZ. LINDEN, NJ. GOLDEN VALLEY, MN. SPOKANE. WA. ATLANTA, GA l PORTLAND, OR

Expert Lubrication and Fuel Analysis Services

Page 68: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNlCAL CENTER A DlVlSlON OF CONAM INSPECTION INC. 935 Sunshine Road Kansas City. KS 66115-1122 (913) 281-9881 (800) 332-8055 FAX: (913) 281-9885

BAT& #l SAMPLE 2 (CAN#202-203) 20% BIODIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM D-86

IBP ASTM D-86

10 % ASTM D-86 50 % ASTM D-86

90 % ASTM D-86

EP ASTM D-86

COLD FILTER PLUG POINT ASTM D-4539

FLASH POINT ASTM D-93

CORROSION ASTlM D-130

HEAT of COMBUSTION ASTM D-3338

CETANE NUMBER ASTM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFTN CONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR

SEDIMENT

ASTM D-13 19 41.3 ASTM D-1319 1.9 ASTM D-13 19 56.8

CARLO ERBA 84.58

CARLO ER.BA 12.98

CARLO ERBA 2.79 ASTM D-4294 0.03 1 ASTM D-482 0.02

ASTM D-664 0.07

ASTM D-2075 36.6

ASTM D-l 89 0.03

197 229 273 328 342 +4

170

1A 18,98 1 51.9

NIL STRAW TRACE

DEG C. DEG C. DEG C. DEGC. DEG C. DEG F. DEG F.

BTU / lb

VOL % VOL % VOL % TNT% WI-% W-T % WT % w-r % rng KOH / g

w-r %

CLEVELAND, OH. KANSAS CITY, KS’. PHOENIX, AZ l LINDEN. NJ. GOLDEN VALLEY. MN. SPOKANE, WA l ATLANTA, GA l PORTLAND, OR . Expert Lubrication and Fuel Analysis Services

Page 69: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DIVISION OF CONAM INSPECTiON INC. 92.5 Sunshine Road Kansas CI’~. KS 66115-1 m (913) 281-9881 (800) 332-8055 FAX: (913) 28 I -9885

BATCH #l SAMPLE 3 (CAN#302-303) 30% BIODIESEL

PHYSICAL PROPERTIES

DISTILLATION IBP 10 % 50 % 90 0,/o EP

COLD FILTER PLUG POINT FLASH POINT CORROSION HEAT of COMBUSTION CETANE NUMBER

ASTM D-S6 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-4539 ASTiM D-93 ASTM D-130 ASTM D-3338 ASTM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFlN CONTENT PARAFFLN CONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 48.6 ASTM D-1319 1.5 ASTM D-13 19 49.9 CARLO ERBA 83.74 CARLO ERBA 12.90 CARLO ERBA 3.91 ASTM D-4294 0.026 ASTM D-482 0.01 ASTM D-664 0.14 ASTM D-2075 43.1 ASTM D-189 0.02

192 227 282 332 342 +6 175 1.4 15,681 47.8

NIL STRAW MODERATE

DEG C. DEG C. DEG C. DEG C. DEG C. DEG F. DEG F.

BTU/lb

VOL % VOL % VOL % WT % w-r % W-I-% WT % WT% mgKOH/g

WT %

. CLEVELAND, OH - KANSAS CITY: KS - PHOENIX. AZ - LINDEN, NJ l GOLDEN VALLEY, MN - SPOKANE, WA l ATLANTA, GA. PORTLAND, OR

., : b 1 Expert Lubrication and Fuel Analysis Services

Page 70: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

I - CLEVELAND TECHNICAL CENTER . : =, A UIVISION Of CONAM INSPECTION INC.

r 9% Sunshine Road Kansas City. KS 66115-i 122 (913) 281-9881 (800) 332-8055 FAX: (913) al-9885

BATCH #l SNW’LE 4 (CAN#401-402) 50% BIODIESE:L

PHYSICAL PROPERTIES

DISTILLATION ASTM D-36 IBP ASTM D-86

10 % ASTM D-86

50 % ASTM D-86

90 % ASTM D-86

EP ASTM D-86

COLD FILTER PLUG POINT ASTM D-4539

FLASH POINT ASTM D-93 CORROSION ASTM D-130

HEAT of COMBUSTION ASTM D-3338

CETANE NUMBER ASTM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFTN CONTENT PARAFFIN CONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR

ASH NEUTRALIZATION NUMElER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 64.1 ASTM D-13 19 1.6 ASTM D-1319 34.3 CARLO ERBA 81.59

CARLO ERBA 12.62

CARLO ERBA 6.49 ASTM D-4294 0.022 ASTM D-432 0.01 ASTM D-664 0.25 ASTM D-2075 61.8

ASTM D- 189 0.03

201 243 312

339 343 +I0 180 IA 18:368 49.1

NIL STRAW TRACE

DEG C. DEG C. DEG C. DEG C. DEG C. DEG F. DEG F.

E3TU / lb

VOL % ‘JOL % VOL % ‘w-r % ‘WI- % WT % ‘w-r %

‘WT % rng KOH / g

‘w-r %

CLEVELAND, OH l KANSAS CITY, KS - PHOENIX. AZ l LINDEN, NJ. GOLDEN VALLEY, MN * SPOKANE. WA l ATLANTA. GA. PORTLAND. OR - : _ _ : Expert Lubrication and Fuel Analysis Services

Page 71: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DIVISION OF CONAM INSPECTION INC. 936 Sunshine Road Kansas City, KS 66115-1 IZ (913) 281-9861 (800) 332-8055 FAX: (913) 281-9885

BATCH #l SmpLE 5 (CAN#502-503) 70% BIODIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM D-86 IBP ASTM D-86 10% ASTM D-86 50 % ASTM D-86 90 % ASTM D-86 EP ASTM D-86

COLD FILTER PLUG POINT ASTM D-4539 FLASH POINT ASTM D-93 CORROSION ASTM D-130 HEAT of COMBUSTION ASTlM D-3338 CETANE NUMBER ASTM D-613

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFIN CONTENT CA.RESON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTR4LIZATION NUMBER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 80.5 ASTM D-13 19 1.2 ASTM D-1319 18.3 CARLO ERBA SO.05 CARLO ERBA 12.29 CARLO ERBA 9.29 ASTM D-4294 0.020 ASTM D-482 0.02 ASTM D-664 0.39 ASTM D-2075 81.3 ASTM D- 1 S9 0.02

206 256 323 338 350 +12 190 1 A 17,850 50.9

NIL STRAW TRACE

DEG C. DEG C. DEG C. DEG C. DEG C. DEG F. DEG F.

BTU I lb

VOL % VOL % VOL % w-r% w-r% PVT% w-r % WT % mgKOH/g

wr %

CLEVELAND. OH l KANSAS CITY, KS : PHOENIX, AZ. LINDEN. NJ . . GOLDEN VALLEY, MN. SPOKANE. WA l ATLANTA, GA. PORTLAND, OR

Expert Lubrication and Fuel Analysis Services

Page 72: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DlVlSiON OF CONAM INSPECTION INC. 935 Sunshine Road

Kansas City. KS 66115-11~

(913) 281-9881 (800) 332-8055

FAX: (913) 281-9885

BATCH #l SAMPLE 6 (CAN#602-603) REFERENCE DIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM D-86 IBP ASTM D-86 10 % ASTM D-86 50 % ASTM D-86 90 % ASTM D-86 EP ASTM D-86

COLD FILTER PLUG POINT ASTM D-4539

FLASH POINT ASTM D-93

CORROSION ASTM D-130 HEAT of COMBUSTION ASTM D-3338 CETANE NUMBER ASTiM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFIN CONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODJNE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR

SEDIMENT

ASTM D-1319 ASTM D-1319 ASTM D-1319 CARLO ERBA CARLO ERBA CARLO ERBA ASTM D-4294 ASTM D-482 ASTM D-664 ASTM D-2075 ASTM D-l 89

159 333 ---

259

309

336 3 --

165

IA 19,672

47.1

28.3

2.6 69.1

86.60

13 7’ .--

co.15 0.034

co.01 0.01 18.4 0.02

NIL STRAW

NIL

DEG C. DEG C. DEG C. DEG C. DEG C. DEG F. DEG F.

:BTU I lb

VOL % VOL % VOL % w-r % WT. % WT% W-I-% WT% mgKOH/g

WT%

CLEVELAND, OH l KANSAS CITY, KS. PHOENIX. AZ. LINDEN, NJ. GOLDEN VALLEY, MN. SPOKANE, WA. ATLANTA. GA. PORTLAND, OR

. , _; Expert Lubrication and Fuel Analysis Services

Page 73: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DIVISION OF CONAM INSPECTfON INC. 935 Sunshine Road Kansas City, KS 66115-1122 (913) 281-9881 (800) 3324055 FAX: (913) 281-9885

BATCH #2 SAMPLE 7 (CAN#ll-12) 100% SOYDIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM D-86 IBP ASTM D-86 10 % ASTM D-86 50 % ASTM D-86 90 % ASTM D-86 EP ASTM D-86

DENSITY @ 15 DEG C. ASTM D-1298 SPECIFIC GRAVITY ASTM D-1298 CLOUD POrNT ASTM D-2500 POUR POINT ASTM D-97 COLD FILTER PLUG POINT ASTM D-4539 FLASH POl-NT ASTM D-93 CORROSION ASTM D- 130 VISCOSITY @ 40 DEG C. ASTM D-445 HEAT of COMBUSTION ASTM D-3338 CETANE NUMBER ASTM D-6 13

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFJNCONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODINE VALUE CAREION RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 99.4 ASTM D-1319 4.0 ASTM D-1319 Cl.0 CARLO ERBA 76.48 CARLO ERBA 11.78 CAR-LO ERBA 12.83 ASTM D-4294 0.012 ASTM D-482 co.01 ASTM D-664 0.48 ASTM D-2075 140.9 ASTM D-l 89 co.0 1

311 329 334 351 356 0.8850 0.8855 +26 +20 +24 310 IA 4.03 17,372 51.1

ML

DEG C. DEG C. DEG C. DEG C. DEG C.

DEG F. DEG F. DEG F. DEG F.

c:St EtTU / lb

VOL % VOL % VOL % WT% WT % w-r % WT % w-r % mg KOH / g

w-r %

PALE STRAW NIL

CLEVE,+ND. OH * KANSAS CITY. KS. PHOENIX. Ai! l LINDEN. NJ l GOLDEN VALLEY. MN l SPOKANE, WA l ATLANTA, GA. PORTLAND. OR 2 L

Expert Lubrication and Fuel Analysis Services

Page 74: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNiCAL CENTER A lYlVlSiON OF CONAM INSPECTION INC. 935 Sunshine Road Kansas City, KS 661151iz.z (913) 281-9881 (800) 33243055 FAX: (913) 291-9885

BATCH #2 SAMPLE 8 (CAN#21-22) 20% BIODIESEL

PHYSICAL PROPERTIES

DtSTILLATION ASTM D-86 IBP ASTM D-86 10 % ASTM D-S6 50 % ASTM D-86 90 % ASTM D-86 EP ASTM D-86

DENSITY @ 15 DEG C. ASTM D-1298 SPECIFIC GRAVITY AS”l-bf D-1298 CLOUD POrNT ASTM D-2500 POUR POINT ASTM D-97 COLD FILTER PLUG POINT ASTM D-4539 FLASH POINT ASTM D-93 CORROSION ASTM D-130 VISCOSITY @ 40 DEG C. ASTM D-445 HEAT of COMBUSTION ASTM D-333 8 CETANE NUMBER ASTM D-613

CHEMICAL COMPOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFIN CONTENT CARBON CONTENT HYDROGEN CONTENT OXYGEN CONTENT SULFUR ASH NEUTRALIZATION NUMBER IODINE VALUE CARBON RESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTM D-1319 37.8

ASTM D-1319 3.1

ASTM D-1319 59.1 CARLO ERBA 84.04

CARLO ERBA 12.97

CARLO ERBA 3.41

ASTM D-4294 0.033

ASTM D-482 co.01 ASTM D-664 0.10 ASTMD-2075 43.9 ASTM D-l 89 co.01

177 214

280

332

344 0.8545

0.8550

+I8

-15 +4

140 1A 2.77

19,156 47.3

NIL STRAW N-IL

DEG C. DEG C. DEG C. DEG C. DEG C.

DEG F. DEG F. DEG F. DEG F.

cst BTU I lb

VOL % VOL % VOL % w-r % w-r % WT% w-r % WI-% mgKOH/g

WT %

CLEVELAND. OH l KANSAS CITY, KS . PHOENIX. AZ. LINDEN, NJ l GOLDEN VALLEY, MN. SPOKANE, WA *a ATLANTA. GA. PORTLAND. OR .

Expert Lubrication and Fuel Analysis Services

Page 75: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

DISTILLATION ASTM D-86 IBP ASTM D-86 10 % ASTM D-86 50 % ASTM D-86 90 % ASTM D-86 EP ASTM D-86

DENSXTY @. 15 DEG C. ASTM D-1298 SPECIFIC GRAVITY ASTM D-1298 CLOUD POrNT ASTM D-2500 POUR POINT ASTM D-97 COLD FILTER PLUG POINT ASTM D-4539 FLASH POINT ASTM D-93 CORROSION ASTM D-130 VISCOSITY @ 40 DEG C. ASTM D-445 HEAT of COMBUSTION ASTM D-3338 CETANE NUMBER ASTM D-61 3

CHEMICAL COMPOSITION

AROMATIC CONTENT ASTM D-1319 44.1 VOL % OLEFIN CONTENT ASTM D-13 19 3.2 VOL % PARAFFIN CONTENT ASTM D-1319 52.7 VOL % CARBON CONTENT CARLO ERBA 83.69 wT% HYDROGEN CONTENT CARLO ERBA 12.66 w-r % OXYGEN CONTENT CARLO ERJ3A 2.69 W-I-% SULFUR ASTM D-4294 0.03 1 WI- % ASH ASTM D-482 KO.01 w-r % NEUTRALIZATION NUMBER ASTM D-664 0.11 mg KOH / @ IODINE VALUE ASTM D-2075 53.6 CARBON RESIDUE ASTM D-189 co.01 w-r % APPEARANCE, 24 HOUR

SEPARATION NIL COLOR STRAW SEDIMENT NIL

:

180 219 291 334 344 0.8577 0.858 1 +20 +5 +10 145 1A 2.87 18,957 48.9

CLEVELAND TECHNICAL CENTER A DlVlSION OF CONAM INSPECTION INC.

935 Sunshine Road Kansas City, KS 6611511~ (913) 281-9881 (800) 332-8055 FAX: (913) 281-988s

BATCH #2 SAMPLE 9 (CAN#31-32) 30% BIODIESEL

PHYSICAL PROPERTIES

DEG C. DEG C. DEG C. DEG C. DEG C.

DEG F. DEG F. DEG F. DEG F.

cst B,TU / lb

CLEVELAND, OH. KANSAS CITY, KS - PHOENIX. AZ l LINDEN, NJ. GOLDEN VALLEY. MN. S?OKANE, WA l ATLANTA, GA l PORTLAND. OR

Expert Lubrication and Fuel Analysis Services

Page 76: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

(913) ZBl-SW (800) 392-6(355 FAX (913) 281~em5

BATCH #2 SAMPLE 10 (CAN#41-42) 50% BIODIESEL

PHYSICAL PROPERTIES

DISTlLLAnON ASTM D-86 ASTMD-86

10 % ASTAJD-86 50 % Ash4 D-86 90 % ASTM D-36 EP ASTM D-86

DENSITY @ 15 DEG 12. ASTM D-1298 SPECIFIC GRAVITY ASTM D-1298 CLOUD POINT ASTM D-2500 POUR PcmT ASTMB97 COLD FILTER PLUG I’CNNT ASTM D-4539 FLASH POW ASTM D-93 CORROSION ASTM D-130 VISCOSITY @ 40 DEO C. ASTM D-445 HEAT of COMBUSTION ASTM D-3338 CETAW NUMBER ASTM D-613

CHEMICAL COtiOSITION

AROMATIC corn OLEFIN CONTENT PAFtAFmNComT CARBON CONTENT HYDROGEN CONTENT OXYGENCONTENT SULFUR

LHEUTR~LIZATION NUMBER IODINE VALUE CARBON RESIDUE AFPEAR4NCE, 24 HOUR

SEPARATION COLOR SEDIMENT

ASTiM D-1319 61.6 ASTMD-1319 2.2 ASTM D-1319 36.2 CARLOERBA 81.24 CARL-OERBA 12.45 CARLOERBA 5.74 ASTM D-4294 0.025 ASTM D-482 <o.Ol ASTM D-664 0.20 ASTM D-2075 79.1 ASTM D- 189 co.01

197 236 302 339 342 0.8660 0.8665 +18 +10 +14 160 IA 3,18 18,466 453

h?L STRAW ML

D’EG C, DlEG C. DlEG C. DlEG C. DlEG C.

DlEC) F. DlEG P. DEG F. DlEG F.

cst BTU/lb

VOL % VQL % VOL % WT % W-T% WT% MT% WT% nngKOH/g

W-l-%

CLEVWNO. OH l KiUQM CTTy, KS - PHOENIX, AZ. LINDEN, NJ l QCLOEN VALLEY, YN l S?OKANE. WA l ATLANTA. CIA l PORTLAMI, Of?

Expert Lubricatbn and Fuel Analysis Services -

Page 77: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

PHYSICAL PROPERTIES

IXSIKLATION

10 % SO% 90 % EP

DENSITY@ 15 DEG C. SPECIFTC GRAvxTY cmuD POINT POUR POINT COLD FILTER PLUG POINT FLASH POINT CORROSION VTSCOSI’IY @ 40 DEG C. HEAT of C0MEWSTKIN CETANE NUMBER

ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-86 ASTM D-1298 AS7Xf D-1298 AS’lX D-2500 ASTM D-97 ASTM D453 9 ASTM D-93 ASTM D-130 AsTMD-445 ASTM D-3338 ASTM 13613

AROMAIPIC CUNTENT OLEFm CONTENT PAR4FFINcoNTENT CARBON COlTENT HYDROGEN CONTENT OXYGEN CON’TENT SULr;-LiR ASH NEulRAL1zATTmNLTMBER IODME VALUE CARBONRESENJE APPEARANCE, 24 HOUR

SEPARA-ITON C0U)R SE.DmT

AXMD-1319 75.8 ASTM D-13 19 2.2 ASTM D-1319 22.0 cARLoExBA 80.35 CARLOERBA 12.41 CARLOE;RBA 8.25 ASTM D-4294 0.016 ASTM D-482 a.01 ASTM D-664 0.30 ASTM D-2075 102.9 ASTM D-189 KO.01

CLEVELAND, OH * &‘&ISA9 CITY, YS . PHOENIX, AZ l UNDEN, NJ l wXDEN VALLEY, MN. SPOKANE, WA. ATLMA, QA . PC)RfLMJD, CR

Expert Lubrfcatlcm and Fuel Analysis Services

204 260 316 339 344 0.8703 0.8708 +18 +15 +I6 135 IA 3.53 17,9!w 49.7

DEG C. DEG C. DEQ C. DEG C. DEG C.

DEG F. DEG F. DEG F. DEG F.

‘czt :BTU / lb

‘VOL % ‘VOL % ‘VOL % ‘WI- % ‘wr % ‘WT % ‘iv-r % ‘wr % fng KOH / g

w-r %

Page 78: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

KanoaociIy, KS 8811~1122 (Ql3) 281-8881 (WO) 3?2.aos5 FAX@xi)z8l-Qms

BATCH #2 SAMPLE: 12 (CAN#61-62) LS REFERENCE DIESEL

PHYSICAL PROPERTIES

DISTILLATION ASTM. a-86 ASTM D-8-6

10 % ASTM D-86 50 % ASTM1186 90 % AS’l-hJD-86 EP ASTMD-86

DENSITY @ 15 DEG C. ASTM D-1298 SPECIFIC GR.4VIl-Y ASTMD-1298 CLOUD POINT ASTM D-2500 PouRPoINT ASTM D-97 COLD FILTER PLUG POINT ASTM D-4539 FLASH POINT ASTM D-93 CORROSION ASTM D-130 VISCOSITY @ 40 DEG C. ASTM D-445 HEAT of CCMWSTION ASTM D-3338 CETANJZIVUMBER ASTM D-61 3

CHEMICAL COMiOSITION

AROMATIC CONTENT OLEFIN CONTENT PARAFFmcONrEm CARBON CONTENT HYDROGEN CCWTEXT OXYGEN CONTENT !txJLFLTR

NJWTRALlZA-I-ION~ER 10DrNE VALUE CAFtBONFtESIDUE APPEARANCE, 24 HOUR

SEPARATION COLOR SEDIMENT

AS-l-M D-1319 25.9 ASTM D-1319 4.2 ASTM D-1319 69.9 CARLO ERBA 8621 CARLOERBA 13.40 CARLOERBA a.15 ASTM D-4294 0.036 AS-i-M D-482 a.01 AsTMD-664 0.01 ASTM D-2075 20.5 ASTM D-189 a.01

170 209 259 317 343 0.8469 0.8473 +10 -2O +6 130 IA 2.55 19,682 435

:DEG C, lDEG C. lDEG C. :DEG C. :DEG C.

:DEG F. :DEG F. :DEG F.. :DEG F.

cst :BTU/B

‘VOL % ‘VOL a/ ‘VOL Yo ‘w-r% ‘w-r% ‘WI-% ‘RT % ‘WT % mgKOH/g

‘wT%

CLEVELANO. OH - KWSAS CITY, KS - WCENIX, AZ . -INDEN, NJ l QOLDEN VALLEY. h!N l PCKANE. WA. ATMA, GA- PORTLMJD, OR Expert Lubrication and Fuel Analysle Swvlces

Page 79: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

Appendix F

Cleveland Technical Center Quality Assurance Report

Page 80: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

-- F - CLEVELAND TECHNICAL CENTER

A DMSION OF CONAM 1NSPECTlON /NC , 935 Sunshine Road

Kansas City. KS 66115-1122 (913) 281-9881 (800) 332-8055 FAX: (913) 281-9885

Dr. Leon Shumaeher University of Missouri

Department of Agricultural Engineering 2 3 5 Agriculture Eqjneering Buildi%

Wnbia, MO 6 52 i 1

Reference Purchase Order No. WI6938

QUALrrY ASSURANCE REPORT

Biodiesel Fuel Project

Cleveland Technical Center 935 Sunshine Road

Kansas City, KS 66 115

.

CLEVELAND, OH * KANSAS CITY, KS. PHOENIX, AZ l LINDEN. NJ l GOLDEN VALLEY. MN l SPOKANE. WA l ATLANTA, GA l PORTLAND, OR Expert Lubrication and Fuel Analysis Services

Page 81: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A DlVlSlON OF CONAM 1NSPECTlON INC. 935 Sunshine Road Kansas City, KS 661151122 (913) 281-9881 (800) 332~8GS5 FAX: (913) 281-9885

ASTM D-86 Distillation

Sample No. 1 Sample No. 1 Origjrtd Value, Deg C. Replicate Value. De:? C.

IBP 293 IBP 259 loo/ 326 10% 324 50% 334 50% 333 90% 350 90% 351 EP 356 El? 356

Sample No. 7 Sample No. 7 Ori.ginal Value, Dee C. Replicate Value. Deg C.

IBP 311 IBP 305 10% 329 10% 327 50% 334 50% 334 90% 351 90% 335 EP 356 EP 344

ASTM D-93 Flash Point

p-Xylene Standard True Value = 81 Deg C Actual = 60 Dleg C

ASTM Round Robin LU-9509 Robust Mean = 184 Deg C Actual = 182 Deg C

ASTM D-130 Copper Strip Corrosion

Laboratory Control Sample - Mobil DTE 797 True Value = IA Actual = 1A (l.b/19/95) True Value = IA Actual = IA (1.0/25/95)

. CLEVELAND, OH. KANSAS CITY, KS l PHOENIX. AZ l LINDEN, NJ l GOLDEN VALLEY. MN l SPOKANE. WA l ATLANTA, GA. PORTLAND, OR _ . Expert Lubrication and Fuel Analysis Services

Page 82: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

--

- CLEVELAND TECHNlCAL CENTER - A DIVISION OF CONAM INSPECTlON /NC

935 Sunshine Road -- Kansas City, KS 651151122

(913) 281-988~ (800) 332-8055 FAX: (913) 287-9885

ASTM D-3338 Heat of Combustion

Standard - Benzoic Acid True Value = 11373 BTU/lb Actual = 11433 13TU/lb

Sample No. 2 Original Value, BTU/lb

Sample No. 2 Replicate Value. BTU ,/A

18981 18863

Sample No. 12 Original Value. BTU/lb

Sample No. 12 Replicate Value, BTU/&

19682 19637

ASTM D-613 Cetane Number

Reference Fuel Cetane Number

T-21 30% / U-14 70% 34.9 T-2 1 40% / U-14 60% 40.4 T-21 50% / U-14 50% 46.0 :. _ ”

T-2 1 60% / U-14 40% 51.5 T-2 1 70% / U-14 30% 57.1

Sample No. 2 0ripj.na.l Value

Sample No. 2 Replicate Value

51.9 : ‘. -- -- - .

Sample No. 8 Original Vdlue ..

.- ._ _ y47.3 Y : : .:;I

51.3 :. _, . ” . Sample No.” 8. . ‘- ‘. Replicate Value

47.9

CLEVELAND, OH l KANSAS CITY, KS l PHOENIX. AZ. LINDEN, NJ l GOLDEN VALLEY. MN l SPOKANE, WA l ATLANTA. GA l PORTLAND. OR - , -. -, - ..:: .>_ ~.. Expert Lubrication and Fuel Analysis Services

Page 83: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

--

- CLEVELAND TECHNICAL CENTER - A DIVISION OF CONAM INSPECTION INC.

936 Sunshine Road -- Kansas City, KS 661151122

(913) 281-9881 (800) 3324055 FAX: (913) 281-9885

Sample No. 9 Origird Value

Sample No. 9 Replicate Value

48.9 46.4

ASTM D-613 Cetane Number

Sample No. 10 Original Value

48.3

Sample No. 10 Replicate Value

48.3

Sample No. 11 Original Value

49.7

Sample No. 11 Replicate Value

47.2

ASTM D-1319 FIA

Sample No. 10 Sample No. 10 Original Value Replicate Value

Aromatics 61.6 Vol % Olefms 2.2 Vol % Saturates 36.2 Vol %

ASTM D-4294 Sulfur

61.8 Vol% 1.5 Vol Yo

36.7 Vol %

Standard = 0.000 Wt % Actual = 0.005 ‘% Standard = 0.052 Wt % Actual = 0.055 ‘%

Sample No. 1 Sample No. 1 Ori,ginal Value Replicate Value

0.014 Wt % 0.011 Wt %

CLEVELAIJD, OH l KANSAS CITY, KS - PHOENIX, AZ. LINDEN, NJ l GOLDEN VALLEY, MN. SPOKANE, WA ’ ATLANTA, GA. PORTLAND, OR .,- Expert Lubrication and Fuel Analysis Services.

Page 84: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

CLEVELAND TECHNICAL CENTER A D/V/S/ON OF CONAM INSPECT/ON INC. 935 Sunshine Road Kansas City, KS 66115-l 122 (913) 281-9881 (800) 3324055 FAX: (913) 281-9685

Sample No. 7 Sample No. 7 Original Value Replicate Value

0.012 Wt % 0.007 Wt %

ASTM D-482 Ash

Sample No. 2 Original Value

Sample No. 2 Replicate Value

0.02 Wt % 0.03 Wt %

Sample No. 3 0ricr;inal Value

Sample No. 3 Replicate Value

0.01 Wt % < 0.01 Wt %

ASTM D-664 Total Acid Number

Standard = Mobil DTE 797 + Oleic Acid True Value = 0.51 mg KOH /g Actual = 0.49 mg KOH / g

Sample No. 7 Sample No. 7 Original Value Replicate Value

0.48 mg KOH / g 0.48 mg KOH / g

ASTM D-2075 Iodine Value

Sample No. 7 Original Value

Sample No. 7 Replicate Value

140.9 140.8 -- - . . . IL-.

CLEVELAI0. OH l KANSAS CITY, KS l PHOENIX. AZ l LINDEN, NJ l GOLDEN VALLEY. MN l SPOKANE:WA * ATLANTA, GA l PORTLAND. OR

. .; : I ;, : .: ..1 Expert Lubrication and Fuel Analysis Services _. ._

Page 85: The Physical & Chemical Characterization of Biodiesel Low Sulfur ...

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; CLEVELAND TECHNICAL CENTER - A DlVlSlON OF CONAM INSPECTION INC.

935 Sunshine Road -- Kansas CiIy, KS 661157122

(913) za1:9aa1 (800) 332-8055 FAX: (913) 28 l-9885

ASTM D-189 Conradson Carbon Residue

Sample No. 1 Sample No. 1 Original Value Replicate Value

-=O.Ol Wt % < 0.01 wt %

CLEVELAND. OH. KANSAS CITY, K.&I l PHOENIX, AZ. LINDEN, NJ l GOLDEN VALLEY. MN l SPOKANE, WA l ATLANTA, GA l PORTLAND. OR

Expert Lubrication and Fuel Analysis Services