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Cloud and Pour Points in Fuel Blendsq Fuel 81A2002) 963±967 www.fuel®rst.com Short Communication Cloud and pour points in fuel blendsq J.A.P. Coutinhoa,*, F. Mirantea, J.C. Ribeirob, J.M. Sansotc, J.L. Daridonc aDepartamento de QuõÂmica da Universidade de Aveiro, 3810 Aveiro, Portugal bPetrogal, Re®naria do Porto, Apartado 3015, 4451-852 LecËa da Palmeira, Portugal cGroupe Haute Pression, Laboratoire des Fluides Compexes, Universite de Pau et des Pays de l'Adour, 64000 Pau, France Received 13 August 2001; revised 19 November 2001; accepted 29 November 2001; available online 4 January 2002 Abstract Cloud and pour points are part of the speci®cations for diesel fuel oils. This work studies the dilution of a diesel with a jet fuel of very low cloud point to produce fuel blends with lower cold characteristics. It is shown that the cloud point of the blend is a highly non-linear combination of the cloud points of the original fuels and is mainly dependent on the cloud point of the heavier ¯uid. Using a thermodynamic model previously proposed, an accurate description of the cloud point for the fuel blends is achieved. This model also allows an estimation of the amount of solid at the pour point showing that as little as 0.5±1wt% of solids are enough to gel the fuel. q 2002 Elsevier Science Ltd. All rights reserved. Keywords: Wax; Cloud point; Modelling 1. Introduction 2. Experimental At low temperatures crystals of paraf®ns form in fuels Both the diesel and the jet fuel used on this work are non- imposing restrictions to its use. A few degrees below the additive samples. The n-alkane distribution on the diesel temperature at which these crystals ®rst appear, the cloud was measured by g.c. equipped with f.i.d. using a protocol point, a crystal network develops in the ¯uid preventing it established in previous studio that proved to be ef®cient from ¯owing and leading to the pour point. The presence of for the analysis of this sort of ¯uids [7,8]. The column solids plugs pipes and fuel ®lters causing the engines to used consisted of a composed by a pre-column of 1m stall. For this reason among the standard speci®cations for Ai.d. 530 mm), one 60 m Ohio Valley column OV-5 fuels [1] there are the cloud [2] and pour points [3] that are Ai.d. 320 mm and ®lm thickness 0.5 mm) and a ®nal related to the low temperature characteristics of the fuel. empty column of about 30 cm. The pre- and post-columns The de®nition of a maximum value for these properties are used for protection of the main column. The post- depends on the fuel purpose, the time of the year and the column protects the main column from the high tempera- region [1]. To achieve a given value of these properties for a tures of the detector and reduce the noise in the detector due distillate two approaches are followed. The ®rst blends [4] to phase destruction. The pre-column `concentrates' the the high cloud or pour point fuel with fuels of lower cloud sample heavy and light components before the main point. The other uses additives such as cloud and pour point column. It is larger than the main column to reduce the depressants to achieve the desired goal [5,6]. The planning length of the sample before the partition in the main column. followed in the re®neries aims at producing a fuel at the It also acts as protection against the heavy compounds that lowest cost but is often quite empirical due to the dif®culty accumulate here. The injection is performed on-column. to predict the low temperature behaviour for fuel blends. Both the temperature and the carrier gas ¯ow rate are This communication reports the effect of diluting a diesel, programmable. To obtain a better separation of the heavy with a jet fuel produced by the same re®nery, on the fuel paraf®ns the gas ¯ow rate is kept at 2 ml/min during the ®rst cloud and pour points. 100 min and then increased to 3 ml/min. The heating starts at 40 8C, is heated at 2.5 8C/min to 305 8C, and then at 2 8C/ min up to 320 8C. Under these conditions paraf®ns between * Corresponding author. Tel.: 1351-234-401507; fax: 1351-234- heptane An-C7) and dotriacontane An-C30) can be quanti®ed. 370084. E-mail address: [email protected] AJ.A.P. Coutinho). Hexane An-C6) [Aldrich 99.5 1 %] was used as reference q Published ®rst on the web via Fuel®rst.comÐhttp://www.fuel®rst.com and CS2 as solvent. The integration is done base to base 0016-2361/02/$ - see front matter q 2002 Elsevier Science Ltd. All rights reserved. PII: S0016-2361A01) 00213-7 964 J.A.P. Coutinho et al. / Fuel 81 :2002) 963±967 Table 1 Nomenclature Properties and composition of the studied fuels g Gibbs free energy Diesel Awt%) Jet h enthalpy q UNIQUAC structural parameter n-C7 0.102 n-C8 0.508 r UNIQUAC structural parameter n-C9 2.126 R universal gas constant n-C10 6.804 T temperature n-C11 8.765 V molar volume n-C12 10.450 V van der Waals volume n-C13 11.513 w n-C14 11.421 x liquid molar fraction n-C15 8.949 s solid molar fraction n-C16 6.901 Z coordination number n-C17 6.934 Greek letters n-C18 5.671 g activity coef®cient n-C19 4.690 n-C20 4.191 l pair interaction energy n-C213.385 Subscripts n-C22 2.541 i component i n-C23 1.668 j component j n-C24 1.133 m fusion n-C25 0.825 n-C26 0.601 sblm sublimation n-C27 0.376 tr solid phase transition n-C28 0.230 Superscripts n-C29 0.148 E excess property n-C30 0.068 l liquid phase Total n-alkane content 16.45 Average Mw Ag/mol) 193.8 149.9 s solid phase Density A20 8C) 0.8352 0.8070 whenever possible. The n-alkane content above heptane was equilibrium equation relating the composition in both found to be negligible for the jet fuel. The analysis for the phases with the non-ideality of the phases and the pure diesel is reported in Table 1along with the total n-alkane component thermophysical properties is used content and other fuel properties. The concentrations of sgs Dh T Dh T heptane or larger n-alkane in the jet fuel were negligible. ln m m 2 1 1 tr tr 2 1 1 l The average molecular weight was measured by freezing xg RTm T RTtr T i point depression and the densities at 20 8C were determined using an Anton Paar DMA 58 densimeter. where s is the molar fraction of compound i in the solid Blends with compositions of 20, 40, 60 and 80 vol% of phase, and x in the liquid phase, Tm and Ttr are the melting the diesel were prepared by mixing measured volumes of and solid±solid transition temperatures, respectively, and hm diesel and jet fuels to achieve the desired concentration. The and htr the heats of these phase transitions. The correlations cloud, freezing and pour points were measured using the for these thermophysical properties used in this work are ASTM standard methods: D 2500 for the cloud point [2], based on the data presented by Broadhurst [12]. D 2386 for the freezing point [9] and D 97 for the pour point [3]. Results are reported in Table 2. Duplicates for each essay were run to check for consistency. Composition for 2.1.1. The liquid phase non-ideality the different blends prepared was obtained by mass balance The activity coef®cient model used for the liquid phase is using the reported densities since the jet fuel acts only as the Flory-free volume model [13]: diluents for the diesel n-alkanes. The average molecular f f weight is used to calculate the mass fractions, the molar ln gcomb-fv ln i 1 1 2 i ; with i x x fractions used by the thermodynamic model. i i 3:3 x V1=3 2 V1=3 2 i i wi 2.1. Cloud point modelling fi X 1=3 1=3 3:3 xj Vj 2 Vwj The cloud point is de®ned as the temperature at which the j ®rst crystals appears in the fuel. The crystal formation is treated as a solid liquid equilibrium of paraf®ns between a where Vi is the molar volume and Vwi is the van der Waals solution and a solid phase [10,11]. The general solid±liquid volume of component i. J.A.P. Coutinho et al. / Fuel 81 :2002) 963±967 965 Table 2 Experimental values of cloud, freezing and pour points Diesel Avol%) Freezing point A8C) Cloud point A8C) Solids at cloud Pour point A8C) Solids at pour point Awt%) point Awt%) 0 262 20 216 0.013 40 211 0.027 233 1.38 60 27 0.024 218 0.71 80 25 0.051 212 0.57 100 23 0.068 212 1.14 2.1.2. The solid phase non-idealityÐpredictive UNIQUAC good knowledge of the paraf®ns composition to describe The solid phase non-ideality will be described by the the phase behaviour of a ¯uid at low temperature. No predictive UNIQUAC model [10,11]. This is a version of pseudo-components are used in the paraf®ns description.
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