Physical and Chemical Properties of 1-ButanolâDiesel Fuel Blends

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Biofuels and Biomass

Physical and chemical properties of n-butanol–diesel fuel blends Hubert Kuszewski Energy Fuels, Just Accepted Manuscript • DOI: 10.1021/acs.energyfuels.8b02912 • Publication Date (Web): 23 Oct 2018 Downloaded from http://pubs.acs.org on October 24, 2018

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Physical and chemical properties of n-butanol–diesel fuel blends Hubert Kuszewski* Faculty of Mechanical Engineering and Aeronautics, Rzeszow University of Technology, 8 Powstancow Warszawy Ave., 35-959 Rzeszow, Poland ABSTRACT: One of the methods to improve the emission parameters of diesel engines is the use of fuels containing an increased fraction of oxygen compounds. This can be achieved by adding oxygen compounds, in the form of alcohols (e.g. ethanol, methanol and n-butanol), to a standard diesel fuel. Due to a number of advantages over ethanol and methanol, n-butanol is of particular interest. It is important to determine the physical and chemical properties of the diesel fuel to which alcohol has been added, in order to study the engine efficiency. From a legislative point of view, it is also necessary to compare these parameters with those of a typical diesel fuel. In this study, the physical and chemical properties of blends of standard diesel fuel and n-butanol were tested, with n-butanol volume fractions of up to 25%. Density, kinematic viscosity, distillation characteristics, heating values, water content, flash point, cold filter plugging point, lubricity, autoignition properties and corrosiveness to copper were tested. The obtained results were compared with the standard requirements specified in the EN 590 standard. Studies have shown that for fuel blends with an increasing volume fraction of n-butanol, autoignition properties deteriorate and lower and higher heating values decrease significantly. The distillation

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curves also change and the mass fraction of water increases. For a higher fraction of n-butanol, deterioration of lubricity was observed, while for the smaller fractions, an improvement in lubricity was noted. Even when using higher volume fractions of n-butanol, the values of some tested parameters were within the limits specified in the standard requirements for typical diesel fuel. 1. INTRODUCTION The widespread use of diesel engines in the transportation industry has resulted in the search for alternative fuels for these types of engines. Due to the beneficial ecological effects associated with the reduction of nitrogen oxide and smoke opacity emissions, there is significant interest in the use of organic oxygen compounds in diesel engines; in particular alcohols. Previous studies have mainly focused on the use of ethanol [1–7], methanol [8–12] and n-butanol [13–23]. Alcohols in general have a low propensity for autoignition and have poor lubrication properties, which is a significant limitation for use in diesel engines [1–4,24–29]. The use of these fuels in a pure form would require significant engine modifications or the use of special additives to improve lubricity and autoignition properties. Due to these poor properties, blends of oxygen compounds with standard diesel fuel are of more practical importance [1–5,30]. N-butanol is a particularly noteworthy oxygen additive for diesel fuel. This alcohol is produced during the fermentation process of biomass derived from lignocellulose, and thus can be considered a fully renewable fuel [13,31,32]. The physicochemical properties of n-butanol, compared to ethanol and methanol, are closer to those of typical diesel fuel [13,33,34], but nbutanol has more favourable autoignition properties [13,26,34–36] and very good miscibility with diesel fuel [13,26,36]. N-butanol also has a higher Lower Heating Value (LHV) and Higher Heating Value (HHV) value [27,34–38], in particular compared to methanol. N-butanol has a


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higher kinematic viscosity (KV), better lubricity, higher flash point (FP), lower evaporation heat, higher density and a much lower autoignition temperature [13,26,27,34–38] than methanol or ethanol. The lower autoignition temperature of n-butanol results in a higher cetane number (CN) [13,34–36]. Another very advantageous feature of n-butanol is its significantly lower hygroscopicity. The issues related to the impact of n-butanol on the performance parameters of a diesel engine have been reported in [13,16–18,20–22,33,34,39–58]. The cited references focus mainly on engine performance and the harmful exhaust gas emissions, showcasing the benefits of adding nbutanol to diesel fuel by reducing the concentration of nitrogen oxides (NOX) and particulate matter. However, the parameters of engine operation depend to a large extent on the fuel injection conditions, which in turn depend on fuel properties. Therefore, when considering the use of a blend of diesel fuel and n-butanol, it is important to determine the physical and chemical properties of the same, in order to determine the efficiency of the fuel under various conditions. Density is a characteristic feature of each group of fuels, including diesel fuels. The amount of fuel injected into the combustion chamber is controlled by volume or time within electronically controlled injectors. A decrease in fuel density (and also viscosity) can result in a reduction of the engine brake power, an increase in (volumetric) specific fuel consumption and an increase in the emission of toxic compounds in the exhaust gas [3,30,59,60]. Knowledge of the density of fuel at a given temperature is necessary for the fuel storage and distribution processes. For material settlements with the fuel turnover conducted, for example, between the refinery and the fuel base, or between the fuel base and the petrol station, mass units are used. Settlements between a petrol station and a user of the fuel (as a vehicle is refuelled) are carried out in units of volume [30].


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The viscosity of the fuel determines the fuel flow resistance through the elements of the injection system and has a direct impact on the atomisation process [30,61–63]. When fuel viscosity increases, losses of the energy for fuel circulation in the fuel supply system increase [30,61,64]. The viscosity increases flow resistance in fuel pipes, through filtration elements, and in the injection system, in the holes of the pumping elements and in the fuel ducts and spray holes of the injector nozzle. In addition, when the viscosity increases, the cylinder within the high-pressure pump deteriorates and the pressure relief effect of the shut-off valve in the highpressure pipe becomes weaker [30]. With a higher viscosity fuel, however, there is less leakage in injection pump, which increases the precision of fuel delivery. The viscosity also determines the shape of the fuel spray characterized by the spray tip penetration and the spray cone angle. When viscosity increases, the spray tip penetration increases and the spray cone angle decreases, as the conditions of droplet secondary break-up deteriorate [30,61,65,66]. With a lower fuel viscosity, the spraying quality is better, which means that the fraction of droplets with smaller diameters in the spray increases [30,65,67]. Smaller fuel droplets of low mass have less ability to penetrate the combustion chamber, being intensively braked in a medium of compressed air at the end of the compression stroke. Low spray tip penetration may cause an incomplete burn of the fuel [30]. If the spray tip penetration is too high, the fuel can settle on the cylinder walls removing a lubricating layer, which accelerates wear of the piston-rings-cylinder assembly. The distillation curve plots temperature versus the amount of distillate collected. The distillation characteristic is determined by normal distillation, during which the fuel is separated into fractions of different boiling point. The initial boiling point (IBP) along with the distillation temperature of 10% of the fuel volume determines the starting characteristic of the engine and the warm up procedure [61]. This measure is also vital for engines with external formation of the


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combustible mixture. Lower values of these temperatures contribute to easier starting and warmup. Too much light fraction in the fuel can cause intensification of the premixed combustion process and can result in high pressure rise rates in the cylinder, which in turn negatively effects the engine durability and its noise [30,61]. The IBP also indicates the volatility of the fuel, which ensures the use of appropriate operations for safe distribution and storage conditions [3,68]. The distillation temperature of 50% of the fuel volume determines the quality and homogeneity of the spray. A lower temperature shortens the time to form the fuel-air mixture by facilitating the process of fuel evaporation [30, 68], which has a beneficial effect on warm-up of the engine. The fuel components with high boiling temperature tend to burn incompletely, contributing to the formation of carbon deposits in the combustion chamber and thermal decomposition of nonvaporized fuel droplets into high levels of soot. In addition, fuel that has not burned can settle on the cylinder walls, disrupting the process of forming a lubricating layer, which accelerates wear of the cylinder bearing surfaces. The heating value is the amount of heat produced by complete combustion in a unit of fuel mass. It is especially important to know the LHV, which does not include the amount of heat produced from the condensation of water vapour. The higher the LHV, the lower the fuel mass consumption by the engine [30,61]. In general, the heating value of fuel is determined by the ratio of the mass fraction of hydrogen to the mass fraction of carbon in the fuel. The higher this ratio, the higher the heating value of the fuel [30]. Although the heating value of diesel fuel is not a standardized parameter, it allows for prediction of fuel consumption. The LHV is necessary to calculate the brake thermal efficiency of the engine, which is an important performance parameter for comparing design and output. At volumetric measurement of the injected fuel amount, which is typical in injection systems of diesel engines, assuming a specific fuel density,


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knowledge of The LHV allows for the precise determination of the amount of fuel delivered in terms of the energy it contains. Water in diesel fuel can exist as dissolved, emulsified or free water (as a separate phase) [30,69]. Emulsified or separate phase water in the fuel intensifies the corrosion processes in the injection system. Water in the fuel deteriorates fuel atomization, reduces the life of fuel filters, degrades lubricity and low temperature properties and may be why microorganisms develop. For these reasons, the presence of emulsified and suspended water is not permitted in the fuel, whereas the content of dissolved water in diesel fuel, is limited to 200 ppm [70]. It should also be noted that water in alcohol hinders the blending process of alcohol and diesel fuel. The blend becomes less stable and tends to delaminate, especially at lower temperatures [3–5,36]. The flash point of the fuel has no direct effect on the combustion process in a diesel engine. The FP is defined as the lowest temperature at which fuel heated under strictly defined conditions gives off enough vapour to create an air mixture that ignites when approaching the flame source. The FP determines the safety precautions for handling the fuel and qualifies the fuel to the appropriate fire hazard class [3,4,30]. The cold filter plugging point (CFPP) is the basic and most important parameter for assessing the low temperature properties of diesel fuels used in Europe. In particular, this parameter determines the lowest temperature for diesel fuel use. The CFPP forms the basis for the division of diesel fuels into seasonal species depending on climatic conditions [70]. The CFPP quantifies the solidification of paraffin hydrocarbons. Excessive amounts of formed paraffin hydrocarbon crystals makes the flow of fuel through the fuelling system impossible. [3,30,71–73]. The CFPP refers to the highest temperature for which the flow time is greater than 60 seconds for a specified volume of test fuel through a standardized filter at a certain negative pressure.


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Fuel lubricity is an important parameter through the lens of durability for the precision pairing of the fuelling system and diesel engine [2,29,30,61,74]. To prevent the seizing of friction connections in the injection system, the friction surfaces must be separated by a durable layer of lubricant. In the vast majority of design solutions for injection systems, fuel is the only lubricant. Due to the relatively low viscosity diesel fuel, the conditions generally present in the friction connections allow for boundary lubrication, rather than hydrodynamic lubrication [29,30]. The durability of boundary layers in the friction connections limiting the wear processes is determined by the fuel lubricity. Fuels with better lubricating properties have a greater ability to create permanent boundary layers. In turn, this ability depends, inter alia, on adsorptive properties of the fuel; i.e. the presence of fuel substances of a polar nature. Such substances include, among others, sulphur and its compounds. Several methods are used to assess the lubricity of fuels [29,30]. The most frequently used approach is the high frequency reciprocating rig (HFRR) method in which a loaded steel ball is the end-effector. The lubricity measure of fuel is the diameter of the wear scar on the ball. The results of the research on fuel lubricity determined by the HFRR method can be found in [3,29,75–81]. The autoignition properties of fuels are determined based on the CN, or the derived cetane number (DCN), in compliance with the appropriate standards requirements [70,82]. For this purpose, a test engine can be used, in accordance with the procedures contained in [83,84], which, are both complicated and expensive. An alternative is the constant volume combustion chamber (CVCC) method. When measurements are made using the CVCC method, the DCN is used [85]. In the DCN determination, the correlation between the ignition delay period (ID) and the CN [85–89] is used. A description of the standard method for DCN determination can be found in [90–95]. In the procedures described in [91–94], the DCN is calculated based on the


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measured ID. In the procedure included in [94,95], additionally the combustion delay period (CD) is used for determination of the DCN, as described in detail in [28,96–99]. Low CN values of fuels are unfavourable, because it indicates a longer ID. A long ID has a negative effect on the operation of the diesel engine, because during this period, a large amount of fuel accumulates in the combustion chamber, which in turn causes an increase in the peak combustion pressures [30,61,85]. Operation of the engine becomes noisy and the load on the elements of the crank piston mechanism increase, which accelerates engine wear and increases NOX emissions. The impact of the CN on the performance parameters of diesel engines were presented in [86,100– 109]. The corrosive effect may cause chemical and electrochemical corrosion of metal elements that contact with the fuel. Intense corroding effects can therefore have a destructive effect on metal components in the fuel system, both in the high and low pressure regions [3,5]. In general, the hydrocarbons that make up the fuel do not have a corrosive effect on metals. However, metal corrosion is caused by other chemical compounds found in the fuel; e.g. sulphur compounds, organic and inorganic acids and bases soluble in water [30]. The most aggressively corrosive are active sulphur compounds (e.g. free sulphur, hydrogen sulphide), especially in the presence of water. According to the standard [70], the corrosive effect of fuels on copper is determined. A properly prepared copper plate is immersed in a fuel at a constant temperature. After a specified time period, the colour of the plate is evaluated by comparing it with the corrosion patterns. The issues concerning this type of study in relation to various fuels can be found in [110]. The present study focused on the basic physical and chemical properties of n-butanol–diesel fuel blends (nBDB) with n-butanol volume fractions of up to 25%. The obtained results for individual blends were compared with the parameters of neat diesel fuel (NDF) and with the


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standard requirements for such a fuel. Density, kinematic viscosity, distillation characteristic, lower and higher heating values, water content, flash point, cold filter plugging point, lubricity, derived cetane number and the corrosive effect on copper were analysed. It should be noted that some of the above parameters can be estimated based on the mass fractions of n-butanol and diesel fuel in the blend. In this way, the heating value, density or water content can be determined. However, it was assumed that all parameters for the blends are determined by measurement and using methods that are normally used for diesel fuel. It should be expected that if the n-butanol–diesel fuel blends are approved for use in diesel engines, they will be prepared by volume, and the parameters of these blends will be determined by measurement. The objective of the study was to show the trend of changes in the analysed parameters of diesel fuel and n-butanol blends with respect to the n-butanol fraction. The presented data complemented previous research, as detailed in [28,29,96,97,99] related to the properties of diesel fuel and oxygen compound blends. The collected data may also be helpful for optimizing the combustion systems used in diesel engines. 2. EXPERIMENTAL METHODOLOGY 2.1. Samples characterization The study of the physical and chemical properties was carried out for six fuel samples. One of the samples was a standard, commercially available, grade-F diesel fuel that meets the requirements of [70]. Subsequently, n-butanol with a purity of more than 99.0% was added to the diesel fuel, with the n-butanol volume fraction varying from 5% to 25%. A number of publications concerning engine tests focus on nBDBs containing a maximum of about 20–30% of n-butanol [16–18,20,22,33,34,39,41–46,48,49,51,53–57]. Because the author’s research aimed to complement these other studies, the maximum fraction of n-butanol in the study was 25%.


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The use of higher fractions of n-butanol results in a significant deterioration of the autoignition properties of blends, which excludes such fuels from applications in typical diesel engines. The basic parameters of the diesel fuel and the n-butanol used to prepare the blends are given in Table 1. Additionally, Fig. 1 shows the distillation curve of the NDF. The details of the individual fuel samples are presented in Table 2. Table 1. Parameters of Diesel Fuel and n-Butanol Used in the Study

Property

Method

Derived cetane number (DCN)

EN 16715 Infrared analysis (instrument TD PPA – PetroSpec by PAC) PN-C-04375-3 PN-C-04375-3 EN ISO 3104 EN ISO 12185 EN ISO 2719 A EN ISO 12937 EN 116 EN ISO 12156 (1) Infrared analysis (instrument TD PPA – PetroSpec by PAC) Infrared analysis (instrument TD PPA – PetroSpec by PAC) Infrared analysis (instrument TD PPA – PetroSpec by PAC)

Cetane improver (2-EHN), ppm Higher heating value, kJ/kg Lower heating value, kJ/kg Viscosity at 40C, mm2/s Density at 15C, g/cm3 Flash point, C Water content, mg/kg Cold filter plugging point, C Lubricity (WSD), m HPLC total aromatics, % m/m HPLC PNA aromatics, % m/m FAME content, % v/v

Value Diesel fuel 56.5

n-butanol 16.6

78.0

-

46,248 43,221 2.1161 0.822 58.5 24 –27 408

36,067 33,116 2.2614 0.813 37.0 335 –69 614

16.3

-

1.4

-

0.6

-

Figure 1. Distillation curve for diesel fuel (method EN ISO 3405).


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Table 2. Symbols of Fuel Samples

Fuel description DF-B-0 (NDF) DF-B-5 DF-B-10 DF-B-15 DF-B-20 DF-B-25

Volume fraction, % Diesel fuel 100 95 90 85 80 75

n-butanol 0 5 10 15 20 25

The nBDBs, diesel fuel and alcohol were prepared and stored in sealed glass vessels at a temperature of 22°C  1°C. The procedures implemented in the preparation, storage and the entire test cycle of the physical and chemical properties ensured the homogeneity and stability of the prepared blends. Because n-butanol is hydrophobic, no signs of turbidity or delamination were observed for any of the samples. Confirmation of the good inter-solubility of higher alcohol content, including n-butanol, in diesel fuel without phase separation (as result of the low polarity of n-butanol) was also given in the study conducted by Lapuerta et al. [36]. 2.2. Experimental setup and data acquisition 2.2.1. Density Density measurements were made in accordance with the procedure contained in EN ISO 12185. The Accurate Density Meter of type DMA 4500 was used. The measurement consisted of introducing a small amount (1 ml) of the tested fuel sample into a temperature controlled U-tube. During the measurement, the vibration frequency of the U-tube was determined, and the density was then calculated using the measurement constant [111]. For each sample, density measurements were made at three temperatures (15, 40 and 60C), though according to [70] the measurement should be carried out at 15C. For each sample and each temperature, the measurement was performed twice. The results were presented as the mean value of two measurements. The figure with density results (in discussion part) shows the absolute value of


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the expanded uncertainty with a confidence level of 95% and an expansion factor of 2. This uncertainty was determined by the supplier of the test device and was confirmed by a calibration certificate of the measuring device. 2.2.2. Kinematic viscosity Measurements of KV were carried out in accordance with the procedure contained in EN ISO 3104. For this purpose, the automatic viscometer of type HVU 482 was used, as designed based on the Ubbelohde viscometer. The measurement consisted of measuring the flow time for a given sample volume under the influence of gravitational forces, through a calibrated glass capillary device. The value of KV was calculated from the measured flow time using the equation: KV = t  Cc

(1)

where: KV – kinematic viscosity, mm2/s, T

– average time for the free flow of the sample through the capillary (meniscus transition time from first to second mark of the measuring chamber), s,

Cc

– capillary constant, mm2/s2.

Measurements of the flow time through the capillary were measured at least twice, after which time values were averaged. The obtained KVs were corrected, taking into account the gravitational and Hagenbach constants. The tests were carried out at temperatures of 40 and 60C, though [70] specified that the KV measurement be carried out at 40C. The results were presented as the mean value of two measurements. For individual fuel samples, the values of the absolute measurement uncertainty of type A were calculated.


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2.2.3. Distillation characteristics Distillation curves for individual fuel samples were prepared in accordance with the methodology included in the EN ISO 3405. The automated distillation analyser of type Optidist was used. The measurement consisted of subjecting the 100 mL sample to distillation, during which the functional dependence of the boiling point and the volume of distilled fuel on the volume percentage were determined. The distillation process for NDF and the individual blends was conducted adequately to the group of the products to which typical diesel fuel belongs. According to the guidelines contained in [70], on the basis of the distillation curves, the percentage volume of the fuel distilled to 250°C and 350°C, as well as the temperature to which it distils 95% of the fuel volume, were verified. The dependence given in the discussion part allows for the calculation of the absolute measurement uncertainty of temperature. 2.2.4. Lower and higher heating values A study of the HHV was carried out in accordance with the procedure included in the PN-C04375-3. The automated bomb calorimeter of type IKA C5000 was used. To measure the mass of fuel samples, the analytical balance of type WAA 40/160/X/1 was used. The tests were conducted using the adiabatic method, filling the calorimetric bomb with oxygen at a pressure of 30 bar. The calorimetric measurement consisted of measuring the temperature increase of the liquid surrounding the calorimetric bomb. Within the bomb a specified, precisely measured mass of the test sample was burned. The HHV value was calculated using the calibration constant of the bomb and the measured temperature increase. The LHV values were calculated from the equation below [112]: LHV = HHV – 24.42 · (8.94 · H)

(2)


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where: LHV – lower heating value, kJ/kg, HHV – higher heating value, kJ/kg, H

– mass fraction of hydrogen in fuel sample, %, For NDF, the mass fraction of hydrogen in the fuel was calculated based on [113]: H = 0.001195 · HHV – 41.4

(3)

where: H

– mass fraction of hydrogen in fuel sample, %,

HHV – higher heating value, kJ/kg, The mass fraction of hydrogen in the blends was calculated based on the mass fractions of diesel fuel and n-butanol in the blends. The results of HHV and LHV were presented as the mean value of two measurements. For individual fuel samples, the values of the absolute measurement uncertainty of type A were calculated. 2.2.5. Water content The WC in the fuel was tested in accordance with the methodology included in EN ISO 12937. For this purpose, the coulometric Karl Fischer titrator of type AquaMAX KF was used. Determination of the mass fraction of water in the fuel sample was performed by coulometric titration to the set end point, when free iodine appeared in the system. Stoichiometrically, 1 mole of water reacts with 1 mole of iodine, which means that 1 milligram of water is equivalent to 10.71 electric coulombs generating 1 milligram of iodine. The results of the WC were presented as the mean of two measurements. For individual fuel samples, the absolute measurement uncertainty of type A was calculated.


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2.2.6. Flash point The FP measurement was carried out in accordance with the methodology included in EN ISO 2719 A. For this purpose, the Pensky-Martens flash point analyser of type HFP 339 was used. When measuring the FP, the fuel sample was placed in a test crucible with a special lid and was heated at a constant rate while mixing. At regular intervals, a small test flame was introduced into the test crucible. The FP was taken as the lowest temperature at which the flash of the flammable mixture with air occurred. The value of the uncertainty in the temperature measurement was determined by the manufacturer during calibration. 2.2.7. Cold filter plugging point The measurement of the CFPP was conducted in accordance with the methodology included in the EN 116. The automated cold filter plugging point analyser of type FPP 5Gs was used for this purpose. Before starting the measurement, a 45 mL sample was placed in the refrigeration chamber of the test device and was subjected to gradual cooling. After reaching a certain temperature, the vacuum pump was started and the sample flow was passed through a strainer into a 20 mL measuring pipette. The suction vacuum of the sample was 200 mmH2O. During the measurement, the flow time of the sample through the measuring pipette was measured. The lowest temperature at which the flow time of the sample through the measuring pipette greater than or equal to 60 s was the CFPP. The value of the uncertainty in the temperature measurement was determined by the manufacturer of the test analyser during calibration. 2.2.8. Lubricity The lubricity tests were conducted using the HFRR apparatus produced by PCS Instruments. The test procedure was conducted in accordance with the standard EN ISO 12156 (1). The main elements of the apparatus include a container for the tested fuel, a friction pair consisting of a ball and a test plate, a loading system to provide appropriate pressure on the ball, a heating block


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and the system forcing the reciprocating motion of a certain frequency and established stroke. The entire station also included humidity and temperature sensors, as well as a control system connected to a computer with the appropriate software, enabling the measurement parameters to be entered and the results to be archived. The test conditions appropriate for the standard are shown in Table 3. Table 3. Lubricity Test Conditions Parameter Volume of fuel sample Stroke length Frequency Fuel sample temperature Test mass Test duration

Unit cm3 mm Hz C g min

Value 2  0.2 1  0.02 50  1 60  2 200  1 75  0.1

After measuring, the ball, together with its holder, were placed under the measuring microscope ML7000/SP produced by MEIJI Techno Co., Ltd. and equipped with a PCS Instruments camera. After calibration, the wear scar was displayed and measured three times on the computer monitor. In the discussion below, photographs of the wear scars are presented for each sample. After measuring the length of the wear scar, the WSD was automatically calculated, as an assessment criterion for lubricity. In accordance to the standard method, the WSD was calculated by using the formula: WSD = (X + Y)/2

(4)

where: X

– scar dimensions perpendicular to oscillation direction, m,

Y

– scar dimensions parallel to oscillation direction, m. The results of the WSD were presented as the mean of three measurements. For individual fuel

samples, the values of the absolute measurement uncertainty of type A were calculated.


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2.2.9. Derived cetane number The DCN was determined in accordance with the procedure contained in EN 16715. For this purpose, the instrument of type CID510 with a CVCC was used. Before performing a series of tests, a calibration of the device was conducted according to the procedure specified in the standard. The required reference fuel consisting of a mass blend of hexadecane (40%, with a minimum purity of 99.0 vol%) and 2,2,4,4,6,8,8-heptamethylnonane (60%, with a minimum purity of 98.0 vol%) was used for calibration. The calibration parameters are summarized in Table 4. Table 4. Testing Device Calibration Settings Parameter Injection pressure Injection period, (injection pulse width) Chamber static pressure Wall temperature of the combustion chamber Injector nozzle coolant jacket temperature

Calibration settings 100 MPa 2.5 ms 2 MPa 600.5°C 50°C

Tolerance limit  1.5 MPa not defined  0.02 MPa  0.2°C  2°C

The single measurement step for each of the analysed fuel samples consisted of five preliminary combustion cycles and 15 fundamental cycles. The DCN was calculated based on ID and CD. The beginning of the ID period was the moment the injector solenoid control impulse was triggered. The end of the ID period was when the pressure in the combustion chamber reached a value that was 0.02 MPa greater than the initial pressure in the chamber. The CD is the time between triggering the injector coil control signal and the corresponding half increase in pressure in the combustion chamber, relative to the initial pressure. An accurate scheme for identifying ID and CD periods was presented in [28,94–96]. DCN measurement results were presented as an average value based on 15 essential combustion cycles. For individual fuel samples, the values of the absolute measurement uncertainty of type A were calculated.


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2.2.10. Corrosiveness to copper The assessment of the corrosive effect of fuel on copper was carried out in accordance with the procedure contained in EN ISO 2160. Instead of a liquid heating bath, a climatic chamber of type CTC 256 was used in the tests. Properly prepared copper strips were placed in glass vessels filled with tested fuel samples. The vessels were placed into climatic chamber set to 50C. After three hours, the vessels were removed from the chamber and the copper strips were rinsed and dried. The copper strips were then evaluated and compared to the corrosion description (according to EN ISO 2160) to determine the corrosion class. In this case, the copper strip corrosion standards were also used, in accordance with ASTM method D 130. 3. RESULTS AND DISCUSSION 3.1. Density Fig. 2 shows the effect of the n-butanol volume fraction on the density of the nBDB. Because the density of NDF is slightly higher than n-butanol at 15°C, as shown in Table 1, the density of nBDB only slightly decreases with the increased n-butanol fraction. The obvious consequence of the measurements being carried out at higher temperatures is the density reduction, whereas, as at 15C, the increase in the n-butanol fraction results in a slight decrease in density. According to the standard [70], the density of diesel fuel (grade A to F) at 15C should be 0.820 g/cm3 to 0.845 g/cm3. Since the density of the NDF used was only slightly higher than the required minimum value, the 15% higher n-butanol fractions resulted in the nBDB not meeting the requirements of the standard [70]. However, all fuel samples met the requirements of all five classes of arctic diesel fuel, for which the minimum density value is 0.800 g/cm3.


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Figure 2. The effect of n-butanol volume fraction on density of nBDBs. Considering the method of controlling the fuel delivery in modern diesel engines, a slight decrease in the density of nBDB with the increase in the n-butanol fraction is a marginal problem. The mass fuel delivery at lower fuel density can easily be increased by modifying the control system. The injection period (injection pulse width) or the fuel injection pressure could be increased [61,114]. Considering the standard requirements, to keep the density of all tested nBDBs within the required range, a NDF with a higher density should be used. 3.2. Kinematic viscosity As seen in Fig. 3, a slight decrease in the KV of nBDBs was noted with an increase in the nbutanol volume fraction, both for 40C and 60C. The natural consequence of the higher temperature is lower KV values at 60C. This confirms the results obtained by Lapuerta et al. [36,115] and data contained in the study by Kumar and Savaranan [26]. Comparing the KV for NDF and neat n-butanol (NnB) (Table 1) with the data in Fig. 3, a synergetic effect can be seen, because the KV of nBDBs was lower than the KV for NDF and NnB. The synergistic effect in the case of viscosity for nBDBs is characteristic for blends of diesel fuel and select alcohols (including n-butanol), where viscosity is similar to the viscosity of diesel fuel. The interaction between diesel fuel and n-butanol, creating the synergistic effect with respect to KV was highlighted in [36,115].


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Figure 3. The effect of n-butanol volume fraction on the KV of nBDBs. Comparing the results shown in Fig. 3 with the requirements in [70], it can be seen that even for an n-butanol fraction of 10%, the nBDB does not meet the requirements of the standard, where the minimum value of KV at 40C must be 2 mm2/s. The use of higher viscosity diesel fuel in the nBDB (e.g. with a higher FAME content) will change these relations and due to standard requirements, it will then be possible to use a higher n-butanol volume fraction. Fig. 3 indicates that due to the lower viscosity of the nBDB compared to NDF, the atomisation process of the fuel will be improved [61,115] and the power consumption to transfer fuel will be reduced. At the same time, however, leaks in the fuel system may increase and, as a result, non-uniformity in fuel delivery may occur. 3.3. Distillation characteristics As shown in Fig. 4, the IBP for blends reaches a value close to the boiling point of n-butanol. The change in slope of distillation curves for nBDBs occurred at the volume fraction of nbutanol. After distilling 35% of the sample, the distillation curves became more similar to the distillation curve of NDF.


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Figure 4. The effect of n-butanol volume fraction on distillation curves of nBDBs. The high volatility of nBDBs in the diesel engine, where the formation of a combustible mixture takes place in the cylinder after high-pressure fuel injection is less important than the external formation of a combustible mixture [61]. As can be seen from the distillation curves, there was a clear increase in the fraction of low boiling components for the nBDBs. The fraction of these components increases with the increase in the n-butanol volume fraction. This may result in improving the starting ability of the engine, but may also disturb the fuel distribution in the combustion chamber, due to the intense evaporation of the fuel directly at the injector nozzle [61]. According to the standard [70], distillation recovery at 250°C amounts to a maximum of 65% (v/v), and distillation recovery at 350°C amounts to a minimum of 85% (v/v), while 95% (v/v) is the maximum at 360°C. Fig. 4 shows that NDF and all nBDBs met these requirements. 3.4. Lower and higher heating values The results of studying HHV and LHV for nBDBs were already presented in a previous paper [99]. Figure 5 shows that along with the increase in the n-butanol volume fraction, the HHV, and consequently the LHV, for nBDBs were reduced proportionally. For example, with the n-butanol


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volume fraction of 25%, the HHV and LHV were lowered by 6% compared to the same values for NDF.

Figure 5. The effect of n-butanol volume fraction on the HHV and LHV of nBDBs. The decrease in HHV and LHV values for nBDBs, along with the increase in the n-butanol volume fraction was an obvious consequence of the lower HHV and LHV for NnB, as it can be seen from the Table 1. Using an n-butanol volume fraction of 25% in nBDB, reduced the energy value of the fuel and in relation to NDF should be considered acceptable. Bearing in mind the lower density of such a blend (Fig. 2), in order to provide an energy equivalent weight of the fuel with respect to NDF, the injector opening time or the fuel injection pressure may need to increase. The consequence of the increase in the n-butanol volume fraction when powering the engine with the nBDB will be an increase in both mass and volume fuel consumption. 3.5. Water content Figure 6 shows that as n-butanol is added to diesel fuel, the mass WC in nBDB increases. Because diesel fuel with a low WC was used in the tests, even at the n-butanol volume fraction of 25% in nBDB, the maximum WC allowable by standard [70], which is 200 mg/kg, was not exceeded.


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Figure 6. The effect of n-butanol volume fraction on WC in nBDBs. Considering the standard requirements and the fact that the mass WC in nBDBs was naturally determined by the mass WC of the input components, it is advisable to use diesel fuel with the lowest mass WC possible when preparing nBDBs. 3.6. Flash point According to the standard [70], the minimum FP for diesel fuel is 55°C. As it can be seen from Fig. 7, except for NDF, none of the tested fuel sample met this requirement. The low FP of nBDBs was the result of a relatively volatile component in the blend; i.e. n-butanol.

Figure 7. The effect of n-butanol volume fraction on FP of nBDBs. Figure 7 also shows that the FP of nBDBs depends slightly on the n-butanol volume fraction. As it can be seen, the FP is related to the presence of n-butanol in the blend and is slightly lower


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than for the higher volatility component, i.e. n-butanol (Table 1). The obtained results show that due to the FP, all safety measures when using any nBDBs should be the same as in the case of NnB and much stricter than for NDF. 3.7. Cold filter plugging point Figure 8 shows that the addition of n-butanol to diesel fuel results in a reduction of CFPP for nBDBs, as compared to NDF. However, from an n-butanol volume fraction of 15% and up, the CFPP stabilizes to a constant level. The reduction of CFPP for the analysed blends was the result of the addition of n-butanol, for which CFPP, as it can be seen from Table 1, amounted to –69°C.

Figure 8. The effect of n-butanol volume fraction on CFPP of nBDBs. Similar results regarding CFPP for nBDBs at smaller fractions of n-butanol were obtained by Lapuerta et al. [36,73]. The authors examined, among others, the CFPP parameter for nBDBs, where NDF was characterized by a CFPP of –17C. The measurements showed that for up to 80% n-butanol volume fraction, there was a slight influence on the reduction of CFPP [36]. In [73], the NDF was used, for which the CFPP was –20°C. A slight decrease in CFPP for nBDBs was obtained for n-butanol volume fractions of 10, 15 and 50%, but for fractions of 2.5, 5, 30 and 40% ,the CFPP parameter for nBDBs had a higher value than for NDF. Analysing the data


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contained in [36,73] and in this study, it can be concluded that CFPP for nBDBs are determined by the low-temperature parameters of the NDF used. Comparing CFPP results (Fig. 8) with standard requirements [70], it can be seen that using NDF, for which the CFPP value met requirements for arctic diesel fuels of Class 1, all nBDBs met the requirements for arctic diesel fuel of Class 1 and Class 2. 3.8. Lubricity As it can be seen from Fig. 9, wear scars on the test ball were similar in shape. For each tested sample, the length of the scar dimension in the Y direction was smaller than in the X direction. The recorded images of wear scars were characterized by clear edges, which allowed for the precise determination of individual lengths. From the data presented in Figs. 9 and 10, it can be seen that for NDF the WSD parameter was 408 m. For n-butanol volume fractions of 5% (sample DF-B-5), 10% (sample DF-B-10) and 15% (sample DF-B-15), the WSD parameter for nBDBs had lower values. This was despite the fact that for NnB the WSD parameter was 614 m. For subsequent samples with a higher nbutanol volume fractions (samples DF-B-20 and DF-B-25), the WSD had a higher value than the NDF.

Figure 9. Wear scars on the balls for analysed fuel samples.


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The synergistic effect of the WSD parameter for smaller n-butanol volume fractions (up to 15%) may be the result of the formation of anti-adhesive layers and the successive evaporation of the higher volatility component; i.e. n-butanol. As a result, the lubricity of nBDBs was improved in relation to NDF. However, for higher n-butanol volume fractions, the formation of anti-adhesive layers did not compensate for the negative effect associated with the presence of nbutanol in nBDBs. It should also be noted that for the higher n-butanol volume fractions, as it can be seen from Fig. 3, the lowest viscosity values were also observed. The lower viscosity may additionally weaken the formation of the lubricating film.

Figure 10. The effect of n-butanol volume fraction on WSD for nBDBs. Tribochemical reactions of oxygen with the friction surface, depending on the conditions present in the friction contact, impact wear [29]. At low concentrations of oxygen in the sample (lower fraction of n-butanol), the wear was decreased, due to the formation of anti-adhesive layers. It should also be noted that higher fractions led to excessive oxidation of the friction surface, which intensified the wear. More phenomena related to the formation of oxide coatings with anti-wear properties can be found in [116–119]. The data presented in Fig. 10 only partially correlated to the results contained in [36], where a higher value of the corrected WSD parameter was obtained for the nBDBs compared to the NDF.


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For the standard requirements [70], the permissible value of the WSD parameter is 460 m. Therefore, each n-butanol volume fraction met the standard lubricity requirements. 3.9. Derived cetane number Autoignition properties of nBDBs, including the DCN results, can be found in [99]. Figure 11 shows that increasing the n-butanol volume fraction in nBDBs caused a linear decrease in DCN, whereas in the studied fraction range of n-butanol, the DCN decreased by 2.9 units per 5% volume fraction increase. This is an obvious consequence of the increasing ID and CD values.

Figure 11. The effect of n-butanol volume fraction on DCN of nBDBs. Literature on DCN confirm that the autoignition properties of nBDBs deteriorate with the increase n-butanol volume fraction, which is a consequence of the lower propensity of n-butanol for autoignition, as compared to diesel [13,26,34–36,99]. This was reflected in the decreasing CN value as the n-butanol volume fraction increased [16,39–41,120]. The lower propensity for autoignition with nBDBs versus NDF causes more fuel to accumulate in the combustion chamber. As a consequence, the heat release in the premixed combustion phase will be intensified, which increases the NOX emissions. The average and maximum pressure rise rates in the combustion chamber also increase, which in turn increases the noise of the engine and the load on the crank piston mechanism, impacting durability of the engine.


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From studies [121–127], the length of the ID in pure n-butanol was determined by the pressure and temperature of the medium to which the fuel was injected. In order to improve the autoignition conditions of nBDBs, a higher compression ratio and fuel injection should be considered. The use or increase of the mass fraction of cetane improver additives may also be pursued. The effectiveness of such an additive in the form of 2-EHN with respect to an nbutanol–biodiesel–diesel fuel blend was confirmed in [128], where authors used, among others, an n-butanol–coconut biodiesel–diesel fuel blend (10%, 10% and 80% by volume, respectively) with addition of 2-EHN (2000 ppm). Considering the standard requirements [70], Fig. 11 shows that only the 5% n-butanol volume fraction results met the requirement for a minimum CN value of 51. Diesel fuels available in Poland most often have a cetane number in the range of approx. 52–55. The diesel fuel used in the tests had an above-average derived cetane number, resulting from, among other things, the fact that a low FAME content was used in that diesel fuel (Table 1). Therefore, it should be noted that the presented DCN values for the analysed blends will differ slightly, depending on the DCN value for the base fuel; i.e. diesel. The data presented in Fig. 11, allows for the prediction of changes to the DCN parameter, and consequently the CN, for nBDBs containing a specific volume fraction of n-butanol, up to 25%. 3.10. Corrosiveness to copper Fig. 12 shows the copper strips after conducting the corrosiveness to copper tests. Comparing the strip for the DF-B-0 sample with the others, it can be seen that for all nBDBs, the strips have slightly darker, irregular areas. These slight tarnishes qualified all samples to meet Class 1, as described in EN ISO 2160, and Class 1a according to ASTM D130. Therefore, all samples as complied with the standard [70], where the diesel fuel was characterized as Class 1 for corrosion.


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Figure 12. Copper strips after corrosiveness test for individual fuel samples. The issue of the corrosiveness of n-butanol as a biocomponent in diesel fuel was discussed in [13,26]. In these studies it was concluded that in spite of its corrosiveness, n-butanol could be successfully used in typical diesel engines. This statement was confirmed by the obtained results in this study. 4. CONCLUSIONS This paper presented experimental results of the physical and chemical properties of nBDBs. The tests were carried out for a typical diesel fuel and for several blends of this fuel with nbutanol. These physical and chemical parameters have been taken into account, which have a significant impact on the combustion process and the operation of the diesel engine, as well as safety considerations during storage, transport and distribution. The following conclusions were obtained: - As a result of blending diesel fuel with n-butanol, assuming a higher density for NDF than for n-butanol, the density of nBDBs linearly decreased in relation to the density of NDF, as the nbutanol volume fraction increased. - As the n-butanol volume fraction increased, a slight decrease in the KV of nBDBs was noted. A synergetic effect was observed, as the KV for each of tested nBDBs was lower than the KV for NDF and pure n-butanol.


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- The increase in the n-butanol volume fraction in nBDB resulted in a clear decrease in IBP and a clear increase in the fraction of low boiling components. The volumetric fractions of nbutanol (up to 25%) did not change the characteristic points on the distillation curve relative to NDF, from which standard requirements were formulated. - As the n-butanol volume fraction increased, the HHV, and consequently the LHV, for nBDBs reduced linearly. - The increase in the n-butanol volume fraction in nBDBs caused a linear increase in the WC in nBDBs. - The FP of nBDBs was lower than for NDF and depended slightly on the n-butanol volume fraction in nBDBs. Above a 15% volume fraction of n-butanol, the FP was constant. - As n-butanol was added to diesel fuel characterized by low CFPP, the value of this parameter for nBDBs was further reduced, but only to a certain value, where it stabilized. - In general, an increase in the n-butanol volume fraction resulted in an increase in the WSD parameter. However, for the lower n-butanol fractions (up to 15%), a synergistic effect was noted and as a result, nBDBs containing 5, 10 and 15% n-butanol were characterized by better lubricity than NDF and NnB. For higher n-butanol volume fractions (20 and 25%), nBDBs had poorer lubricity properties than NDF. - The increasing n-butanol volume fraction in nBDB caused a linear decrease in DCN. Under the test conditions, for each 5% increase in the volume fraction, the DCN decreased by of 2.9 units. - An increasing n-butanol volume fraction did not increase the corrosiveness to copper of nBDBs in relation to NDF.


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The tests confirmed that due to its physicochemical parameters, n-butanol can be considered as a biocomponent in diesel fuel. The trends in physicochemical parameters of nBDBs with an increase in n-butanol volume fraction were also noted. The tests further confirmed the applicability of the standards used for diesel fuel to be applied to nBDBs parameters. The data collected as a result of the study supplemented the literature related to the properties of n-butanol–diesel fuel blends. These data may also be helpful in optimizing the combustion systems of diesel engines for which n-butanol–diesel fuel blends will be allowed. The study show that the tested n-butanol–diesel fuel blends, from the technical point of view of the engine operation, can be used in a diesel engine. However, in the case of higher fractions of n-butanol (above 10%), one should bear in mind the deteriorated autoignition properties of the blend and low kinematic viscosity, which may negatively affect the durability of the crank-piston mechanism elements (due to knocking combustion) and disrupt the injection system (increased leaks in the precision pairs). AUTHOR INFORMATION Corresponding Author *E-mail: [email protected]. Phone: +48 17 865 15 82 Funding Sources The study was financed by the subsidy for statutory activity from the Ministry of Science and Higher Education of the Republic of Poland for the Faculty of Mechanical Engineering and Aeronautics at Rzeszow University of Technology. Notes The author declares no competing financial interest.


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ACKNOWLEDGMENT This work was supported by the Ministry of Infrastructure and Development under the Eastern Poland Development Operational Programme, including the European Regional Development Fund – Belgium, which financed the research instruments. The author wish to acknowledge the Polish Ministry of Science and Higher Education and the Rzeszow University of Technology for supporting this research. NOMENCLATURE LHV, lower heating value, kJ/kg HHV, higher heating value, kJ/kg KV, kinematic viscosity, mm2/s FP, flash point, C CN, cetane number NOX, nitrogen oxides IBP, initial boiling point, C CFPP, cold filter plugging point, C HFRR, high frequency reciprocating rig DCN, derived cetane number CVCC, constant volume combustion chamber ID, ignition delay period CD, combustion delay period nBDB, n-butanol–diesel fuel blend (prepared by volume) NDF, neat diesel fuel (standard diesel fuel without the addition of n-butanol) 2-EHN, 2-ethylhexyl nitrate


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WSD, wear scar diameter HPLC, high performance liquid chromatography PNA, polynuclear aromatic hydrocarbons FAME, fatty acid methyl esters FBP, final boiling point, C t, average time for the free flow of sample through the capillary, s Cc, capillary constant, mm2/s2 H, mass fraction of hydrogen in fuel sample, % X, scar dimensions perpendicular to oscillation direction, m Y, scar dimensions parallel to oscillation direction, m NnB, neat n-butanol (pure n-butanol without the addition of diesel fuel) T, temperature measurement uncertainty, C REFERENCES [1]

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