EP1756252B1 - Use of crude oil derived and gas-to-liquids diesel fuel blends - Google Patents

Use of crude oil derived and gas-to-liquids diesel fuel blends Download PDF

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EP1756252B1
EP1756252B1 EP05752458.9A EP05752458A EP1756252B1 EP 1756252 B1 EP1756252 B1 EP 1756252B1 EP 05752458 A EP05752458 A EP 05752458A EP 1756252 B1 EP1756252 B1 EP 1756252B1
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diesel fuel
gtl
diesel
ratio
nox
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French (fr)
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EP1756252A1 (en
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Paul Werner Schaberg
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Sasol Technology Pty Ltd
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Sasol Technology Pty Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/04—Liquid carbonaceous fuels essentially based on blends of hydrocarbons
    • C10L1/08—Liquid carbonaceous fuels essentially based on blends of hydrocarbons for compression ignition

Definitions

  • the invention relates to the use of Gas-To-Liquids (GTL) diesel fuel as a blend component for at least a crude oil derived diesel fuel for reducing the NOx and soot emissions of the resulting diesel composition.
  • GTL Gas-To-Liquids
  • Synthetic fuels such as GTL (Gas To Liquids) diesel fuel have seen a significant rise in interest in recent years. They are considered to be extremely clean fuels, with negligible sulfur and aromatics, and are odor-free and have a cetane number of > 70.
  • GTL diesel fuel used in the examples in this patent specification was manufactured by means of the Sasol Slurry Phase Distillate (Sasol SPDTM) process, which consists of three process steps, as depicted schematically in Fig. 1 .
  • an auto-thermal reforming process is used to convert the natural gas into the synthesis gas, a mixture of CO and H 2 .
  • the synthesis gas is converted into a so-called syncrude containing predominantly paraffinic hydrocarbons, by a Fischer-Tropsch process.
  • This syncrude is primarily in the form of waxes and distillates, which are further refined in a third, product upgrading step by means of mild hydro-processing, in order to produce products that meet commercial fuel specifications, such as diesel fuel and kerosene.
  • GB 2 387 175 A discloses a possible reduction of the soot emission of a diesel fuel by oxidizing the fuel to a certain point and then mixing it with certain oxygen-containing organic compounds. It does not address the problem of NOx reduction.
  • WO 03/087273 A1 discloses a method of increasing the cetane number of a gas oil product based on a petroleum derived gas oil by the addition of a Fischer Tropsch derived gas oil having a higher cetane number than the petroleum derived gas oil. NOx reduction is not mentioned.
  • WO 01/83848 A discloses a method of achieving emissions level of cracked stocks that are equivalent to or superior to base fuels while containing greater levels of aromatics and poylaromatics, where the base fuels are conventional, petroleum derived base fuels.
  • the invention provides the use of a Gas-to-Liquids (GTL) diesel fuel, which GTL diesel has a density at 15 deg C of below 0.78 kg/l, a sulphur content of less than 1 mg/kg, polyaromatics below 0.1 mass%, and a cetane number above 65, as a blend component for at least a crude oil derived diesel fuel for reducing the NOx and soot emissions of the resulting diesel fuel composition, characterized in that the crude oil derived diesel fuel has a density at 15 deg C below 0.85 kg/l, a sulphur content of less than 10 mg/kg, a polyaromatics content of below 5 mass%, and a cetane number from 51 to 60 whereby the NOx and soot emissions of the resulting diesel fuel composition, when combusted in an engine, are non-linearly reduced to a higher degree than would be expected when considering the blending ratio of the GTL diesel to the crude oil derived diesel fuel.
  • GTL Gas-to-
  • the resulting diesel fuel composition may have less than 10 mg/kg sulphur.
  • the resulting diesel fuel composition may have less than 5 mass% polycyclic aromatics.
  • the crude oil derived diesel fuel may be a fuel meeting the EN590 specification.
  • the volumetric ratio range of the GTL: Crude derived diesel may be from 1:9 to 9:1.
  • the volumetric ratio range of the GTL: Crude derived diesel may be from 1:5 to 5:1.
  • the molar H:C ratio of the resulting diesel fuel composition may be from 1.85:1 and 2.05:1.
  • the molar H:C ratio of the resulting diesel fuel composition may be from 1.9:1 and 2.00:1.
  • the resulting diesel fuel composition may have an ASTM D86 10% distillation temperature of from 180°C to 220°C.
  • GB 2 387 175 A discloses a possible reduction of the soot emission of a diesel fuel by oxidizing the fuel to a certain point and then mixing it with certain oxygen-containing organic compounds (see abstract and page 25, lines 22 to 25).
  • the diesel fuels may be derived form various sources including petroleum or Fischer Tropsch synthesis.
  • WO 03/087273 A1 discloses a method for increasing the cetane number of a gas oil product based on a petroleum derived gas oil by the addition of a Fischer Tropsch derived gas oil having a higher cetane number than the petroleum derived gas oil.
  • the amount of added Fischer Tropsch derived gas oil for reaching a target cetane number is less than the amount which would be added if the increase of the cetane number of the blend were linear.
  • the ASTM D86 10% distillation temperature of the resulting diesel fuel composition may be from 200°C to 215°C.
  • the resulting diesel fuel composition may have a flash point of between 60°C and 80°C, typically from 65°C to 78°C.
  • the resulting diesel fuel composition may have a density at 15°C of from 0.77 kg/l to 0.84 kg/l.
  • the resulting diesel fuel composition may have a density at 15°C of from about 0.8 kg/l to about 0.82 kg/l.
  • the resulting diesel fuel composition may have a lower heating value of from 42 500 kJ/kg to 43 800kJ/kg, usually from 43 100 kJ/kg to 43 600 kJ/kg, typically from 43 200 kJ/kg to 43 500 kJ/kg.
  • Gas-to-Liquid diesel fuel as a blend component for a diesel fuel composition, which, when combusted in an engine, has reduced NOx and soot emissions, yields a composition comprising both crude oil derived diesel fuel meeting the European EN590 specification for sulphur-free diesel fuel (designated EU diesel), and the Gas-to-Liquids (GTL) diesel fuel, wherein the crude oil derived diesel fuel to Gas-to-Liquid diesel volumetric blend ratio may range from 1:99 to 99:1 and the composition may have a molar H:C ratio of between 1.8:1 and 2.1:1.
  • the reduction in NOx emissions may be less than the reduction in soot emissions, and vice versa.
  • the reduction in NOx may be minimal, however, the NOx will be reduced by the use of GTL diesel in accordance with the invention.
  • compositions are as described above for the composition.
  • Table 2 Test vehicle and engine data Vehicle designation Mercedes E 220 CDI Limousine Model year 2003 Transmission 6-speed manual gearbox Gross vehicle mass 2 145 kg Engine designation MB OM646, EU3 emission level Displacement, configuration 2,2 L, in-line 4 cylinder, 4 valves per cylinder Compression ratio 18 : 1 Fuel management Common rail fuel injection (peak pressure 1 600 bar) Air management Turbocharged (VNT), intercooled Emission control Cooled EGR, inlet swirl control, close coupled and underfloor oxidation catalysts Rated torque 340 Nm at 2 000 rev/min Rated power 110 kW at 4 200 rev/min
  • Fig. 2 The results of the unadapted vehicle emission tests are depicted in Fig. 2 for the EU diesel, EU50, and GTL diesel fuel. The averaged results for the test runs are presented as the percentages relative to the EU diesel reference fuel. FC indicates the volumetric fuel consumption.
  • ECU Engine Control Unit
  • Fig. 3 shows two examples of results obtained from the steady state test bench work.
  • the figure depicts representative data for the effect of GTL diesel fuel and its blends on the soot - NOx trade-off characterisitc at two operating points, namely 1 600 rev/min and 3,3 bar bmep (brake mean effective pressure), and 2 000 rev/min and 5 bar bmep.
  • the EGR rate was varied, while the SOPI and SOMI were kept constant and equal to the reference values.
  • Soot emission levels were calculated from exhaust smoke levels determined by FSN (Filter Smoke Number) measurements.
  • GTL diesel offers a significant reduction in terms of both soot emissions and NOx for all the EGR rates tested.
  • the soot emission increase for decreasing NOx values follows the expected pattern, and enables a wide range of possible alternative software calibrations.
  • the strong non-linear behavior of the EU50 blend is again evident - this fuel exhibits almost the same benefits as neat GTL diesel fuel.
  • DOE design of experiments
  • the measured data at the five steady-state test points was used to predict the emissions over the NEDC test cycle. Empirical factors were used to account for the differences between the steady-state and transient engine operation. All results from the selected operating points have been normalized and combined into one universal plot, shown in Fig. 5 , to mimic the behavior in a NEDC test with an optimized calibration for each fuel. A surprisingly large reduction in soot and NOx appears to be possible for the GTL diesel fuel and the EU50 and EU80 blends. These reductions are possible without hardware changes to the engine.
  • the neat GTL would allow for a simultaneous soot and NOx reduction of at least 35% compared to the EU diesel calibration. For constant engine-out soot emission, a NOx reduction of 45% seems possible. Due to the non-linear response with the GTL blends, reductions in soot and NOx that are greater than expected when considering the blending ratio, could be obtained with the EU80 and EU50 fuels. This non-linear response is depicted graphically in Fig. 6 .

Description

    Field of the Invention
  • The invention relates to the use of Gas-To-Liquids (GTL) diesel fuel as a blend component for at least a crude oil derived diesel fuel for reducing the NOx and soot emissions of the resulting diesel composition.
    • Background of the Invention
  • Synthetic fuels such as GTL (Gas To Liquids) diesel fuel have seen a significant rise in interest in recent years. They are considered to be extremely clean fuels, with negligible sulfur and aromatics, and are odor-free and have a cetane number of > 70. The GTL diesel fuel used in the examples in this patent specification was manufactured by means of the Sasol Slurry Phase Distillate (Sasol SPD™) process, which consists of three process steps, as depicted schematically in Fig. 1.
  • In the first step an auto-thermal reforming process is used to convert the natural gas into the synthesis gas, a mixture of CO and H2. In a second step the synthesis gas is converted into a so-called syncrude containing predominantly paraffinic hydrocarbons, by a Fischer-Tropsch process. This syncrude is primarily in the form of waxes and distillates, which are further refined in a third, product upgrading step by means of mild hydro-processing, in order to produce products that meet commercial fuel specifications, such as diesel fuel and kerosene.
  • GB 2 387 175 A discloses a possible reduction of the soot emission of a diesel fuel by oxidizing the fuel to a certain point and then mixing it with certain oxygen-containing organic compounds. It does not address the problem of NOx reduction.
  • WO 03/087273 A1 discloses a method of increasing the cetane number of a gas oil product based on a petroleum derived gas oil by the addition of a Fischer Tropsch derived gas oil having a higher cetane number than the petroleum derived gas oil. NOx reduction is not mentioned.
  • WO 01/83848 A discloses a method of achieving emissions level of cracked stocks that are equivalent to or superior to base fuels while containing greater levels of aromatics and poylaromatics, where the base fuels are conventional, petroleum derived base fuels.
    • Summary of the Invention
  • The invention provides the use of a Gas-to-Liquids (GTL) diesel fuel, which GTL diesel has a density at 15 deg C of below 0.78 kg/l, a sulphur content of less than 1 mg/kg, polyaromatics below 0.1 mass%, and a cetane number above 65, as a blend component for at least a crude oil derived diesel fuel for reducing the NOx and soot emissions of the resulting diesel fuel composition, characterized in that the crude oil derived diesel fuel has a density at 15 deg C below 0.85 kg/l, a sulphur content of less than 10 mg/kg, a polyaromatics content of below 5 mass%, and a cetane number from 51 to 60 whereby the NOx and soot emissions of the resulting diesel fuel composition, when combusted in an engine, are non-linearly reduced to a higher degree than would be expected when considering the blending ratio of the GTL diesel to the crude oil derived diesel fuel.
  • The resulting diesel fuel composition may have less than 10 mg/kg sulphur.
  • The resulting diesel fuel composition may have less than 5 mass% polycyclic aromatics.
  • The crude oil derived diesel fuel may be a fuel meeting the EN590 specification.
  • The volumetric ratio range of the GTL: Crude derived diesel may be from 1:9 to 9:1.
  • The volumetric ratio range of the GTL: Crude derived diesel may be from 1:5 to 5:1.
  • The molar H:C ratio of the resulting diesel fuel composition the may be from 1.85:1 and 2.05:1.
  • The molar H:C ratio of the resulting diesel fuel composition may be from 1.9:1 and 2.00:1.
  • The resulting diesel fuel composition may have an ASTM D86 10% distillation temperature of from 180°C to 220°C.
  • GB 2 387 175 A discloses a possible reduction of the soot emission of a diesel fuel by oxidizing the fuel to a certain point and then mixing it with certain oxygen-containing organic compounds (see abstract and page 25, lines 22 to 25). The diesel fuels may be derived form various sources including petroleum or Fischer Tropsch synthesis.
  • WO 03/087273 A1 discloses a method for increasing the cetane number of a gas oil product based on a petroleum derived gas oil by the addition of a Fischer Tropsch derived gas oil having a higher cetane number than the petroleum derived gas oil. The amount of added Fischer Tropsch derived gas oil for reaching a target cetane number is less than the amount which would be added if the increase of the cetane number of the blend were linear.
  • The ASTM D86 10% distillation temperature of the resulting diesel fuel composition may be from 200°C to 215°C.
  • The resulting diesel fuel composition may have a flash point of between 60°C and 80°C, typically from 65°C to 78°C.
  • The resulting diesel fuel composition may have a density at 15°C of from 0.77 kg/l to 0.84 kg/l.
  • The resulting diesel fuel composition may have a density at 15°C of from about 0.8 kg/l to about 0.82 kg/l.
  • The resulting diesel fuel composition may have a lower heating value of from 42 500 kJ/kg to 43 800kJ/kg, usually from 43 100 kJ/kg to 43 600 kJ/kg, typically from 43 200 kJ/kg to 43 500 kJ/kg.
  • The use of Gas-to-Liquid diesel fuel as a blend component for a diesel fuel composition, which, when combusted in an engine, has reduced NOx and soot emissions, yields a composition comprising both crude oil derived diesel fuel meeting the European EN590 specification for sulphur-free diesel fuel (designated EU diesel), and the Gas-to-Liquids (GTL) diesel fuel, wherein the crude oil derived diesel fuel to Gas-to-Liquid diesel volumetric blend ratio may range from 1:99 to 99:1 and the composition may have a molar H:C ratio of between 1.8:1 and 2.1:1.
  • Reductions in both NOx and soot emissions are obtained which are greater than indicated by the blending ratio of the GTL diesel in the crude oil derived diesel fuel.
  • Thus, more than 70% of the reduction in both NOx and soot emissions which may be obtained with neat GTL diesel fuel, may be obtained with a 1:1 GTL:Crude derived diesel ratio.
  • More than 40% of the reduction in both NOx and soot emissions which may be obtained with neat GTL diesel, may be obtained with a 1:4 GTL:Crude derived diesel ratio.
  • However, in some embodiments the reduction in NOx emissions may be less than the reduction in soot emissions, and vice versa.
  • In some embodiments, the reduction in NOx may be minimal, however, the NOx will be reduced by the use of GTL diesel in accordance with the invention.
  • The properties of the composition and the blending ratios of the components are as described above for the composition.
    • Examples Involving the Invention
  • The effect of GTL diesel fuel blends on exhaust emissions and engine performance has been studied. EU diesel fuel was used as a reference fuel, in addition to being the base stock for the blends. The properties of test fuels used in the investigation are shown in Table 1. Table 1 Properties of the fuels investigated in this study.
    Property Units GTL EU50 EU80 EU
    100% GTL diesel fuel 50:50 Blend EU:GTL 80:20 Blend EU:GTL 2005 European sulphur-free diesel fuel
    Density @ 15HC kg/l 0.768 0.802 0.821 0.836
    Density @ 20°C kg/l 0.765 0.798 0.817 0.832
    Cetane Number 71 62 58 54
    Total Sulphur mg/kg < 1 4 6 7
    D86 Distillation IBP °C 169 157 174 193
    5% °C 180 193 204 214
    10% °C 187 201 212 221
    20% °C 200 215 225 233
    30% °C 219 231 240 248
    40% °C 235 248 256 264
    50% °C 251 264 270 277
    60% °C 267 277 282 287
    70% °C 283 291 294 299
    80% °C 297 305 307 313
    90% °C 312 322 324 332
    95% °C 321 337 339 354
    FBP °C 329 346 350 360
    Flash Point °C 59 66 76 82
    Kinematic Viscosity @ 40°C mm2/s 1.97 2.54 2.79 2.95
    CFPP °C -19 -18 -17 -17
    Cloud Point °C -18 -17 -15 -14
    Total Aromatics* % m/m 0.1 13.5 21.5 26.8
    Bi- and Polycyclic aromatics* % m/m 0.0 2.3 3.7 4.6
    Hydrogen Content* % m/m 15.0 14.3 13.8 13.5
    H/C ratio (molar)* - 2.10 1.98 1.91 1.86
    Lower Heating Value* MJ/kg 43.8 43.5 43.2 43.1
    HFRR Wear Scar Diameter µm 370 < 400 < 400 394
    * Values for blends calculated according to blending ratio
  • Dynamometer tests were conducted with a Mercedes Benz™ E220 CDI vehicle, using the New European Driving Cycle (NEDC) emission test, and without any changes to the basic EU3 emission level engine calibration or engine hardware. The vehicle was tested with its standard calibration without any adaptation, with EU diesel, the 1:1 blend and for the neat GTL fuel. The relevant test vehicle data are shown in Table 2. Table 2 Test vehicle and engine data
    Vehicle designation Mercedes E 220 CDI Limousine
    Model year 2003
    Transmission 6-speed manual gearbox
    Gross vehicle mass 2 145 kg
    Engine designation MB OM646, EU3 emission level
    Displacement, configuration 2,2 L, in-line 4 cylinder, 4 valves per cylinder
    Compression ratio 18 : 1
    Fuel management Common rail fuel injection (peak pressure 1 600 bar)
    Air management Turbocharged (VNT), intercooled
    Emission control Cooled EGR, inlet swirl control, close coupled and underfloor oxidation catalysts
    Rated torque 340 Nm at 2 000 rev/min
    Rated power 110 kW at 4 200 rev/min
  • The results of the unadapted vehicle emission tests are depicted in Fig. 2 for the EU diesel, EU50, and GTL diesel fuel. The averaged results for the test runs are presented as the percentages relative to the EU diesel reference fuel. FC indicates the volumetric fuel consumption.
  • For neat GTL diesel fuel, an unexpectedly high reduction of >90% for HC and CO emissions was observed. The CO and HC reductions for the 50% blend scale roughly with the blending ratio. The NOx emissions were reduced marginally, with the 50% blend again showing about half the reduction of the neat GTL diesel fuel. The same applies for the HC+NOx data.
  • PM emissions were reduced by up to 30% with the GTL diesel. Surprisingly, a strong non-linear characteristic was evident with the 50% blend (EU50), which showed a reduction of approximately 22%.
  • The potential for further emission reductions with the test fuels, and including the optimisation of a limited number of software parameters in the Engine Control Unit (ECU) of the engine was then investigated. For this purpose, an engine mounted on a test bench was used. Steady state test runs were carried out at five operating points characteristic for NEDC emission test cycle. The software parameters investigated were the Exhaust Gas Recirculation (EGR) rate, the start of pilot injection (SOPI) and the start of main injection (SOMI). The five operating points are shown in Table 3 Table 3 Steady state engine test points chosen to reflect NEDC characteristics.
    Engine Test Point Engine Speed (rev/min) bmep (bar) Power (kW) Description
    1 1000 0 0 Pseudo Idle
    2 1 600 3.3 9 Characteristic operating points for the NEDC emission test
    3 2000 2 7
    4 2000 5 18
    5 2800 4 20
  • Fig. 3 shows two examples of results obtained from the steady state test bench work. The figure depicts representative data for the effect of GTL diesel fuel and its blends on the soot - NOx trade-off characterisitc at two operating points, namely 1 600 rev/min and 3,3 bar bmep (brake mean effective pressure), and 2 000 rev/min and 5 bar bmep. In this case, the EGR rate was varied, while the SOPI and SOMI were kept constant and equal to the reference values. Soot emission levels were calculated from exhaust smoke levels determined by FSN (Filter Smoke Number) measurements.
  • It is evident that GTL diesel offers a significant reduction in terms of both soot emissions and NOx for all the EGR rates tested. The soot emission increase for decreasing NOx values follows the expected pattern, and enables a wide range of possible alternative software calibrations. Surprisingly, the strong non-linear behavior of the EU50 blend is again evident - this fuel exhibits almost the same benefits as neat GTL diesel fuel.
  • A design of experiments (DOE) method was used to numerically optimize the three software parameters simultaneously. The DOE predictions were verified by actual experiments, and an example of the results of the simultaneous optimisation of all three calibration parameters at each of the engine operating points is shown in Fig. 4. In this case the optimisation has been performed to minimise NOx emissions with the GTL diesel fuel. Reductions of between 30% and 75% were obtained, without compromising the other emissions, when compared to the EU diesel.
  • The measured data at the five steady-state test points was used to predict the emissions over the NEDC test cycle. Empirical factors were used to account for the differences between the steady-state and transient engine operation. All results from the selected operating points have been normalized and combined into one universal plot, shown in Fig. 5, to mimic the behavior in a NEDC test with an optimized calibration for each fuel. A surprisingly large reduction in soot and NOx appears to be possible for the GTL diesel fuel and the EU50 and EU80 blends. These reductions are possible without hardware changes to the engine.
  • The neat GTL would allow for a simultaneous soot and NOx reduction of at least 35% compared to the EU diesel calibration. For constant engine-out soot emission, a NOx reduction of 45% seems possible. Due to the non-linear response with the GTL blends, reductions in soot and NOx that are greater than expected when considering the blending ratio, could be obtained with the EU80 and EU50 fuels. This non-linear response is depicted graphically in Fig. 6.
  • A 50% GTL blend would recover approximately 85% of the soot/NOx benefits of neat GTL, while a 20% GTL blend would recover approximately 48% of the benefit. It should be noted that the results shown so far have been facilitated by a simple and cost-efficient software adaptation only. It is to be expected that further improvements will be possible if additionally hardware changes, e.g. in the injection system and/or the combustion chamber design are taken into account.

Claims (5)

  1. Use of Gas-to-Liquid (GTL) diesel fuel which has a density at 15 deg C of below 0.78 kg/l, a sulphur content of less than 1 mg/kg, polyaromatics below 0.1 mass%, and a cetane number above 65, as a blend component for at least a crude oil derived diesel fuel for reducing the NOx and soot emissions of the resulting diesel fuel composition,
    characterized in that the crude oil derived diesel fuel has a density at 15 deg C below 0.85 kg/l, a sulphur content of less than 10 mg/kg, a polyaromatics content of below 5 mass%, and a cetane number from 51 to 60, whereby the NOx and soot emissions of the resulting diesel fuel composition, when combusted in an engine, are non-linearly reduced to a higher degree than would be expected when considering the blending ratio of the GTL diesel to the crude oil derived diesel fuel.
  2. Use as claimed in claim 1, wherein a 1:1 GTL:Crude derived diesel ratio is used, the reductions in both NOx and soot emissions for said ratio being greater than 70% of the reduction obtained with a 100% GTL diesel fuel.
  3. Use as claimed in claim 1, wherein a 1: 4 GTL: Crude derived diesel ratio is used, the reductions in both NOx and soot emissions for said ratio being greater than 40% of the reduction obtained with a 100% GTL diesel fuel.
  4. Use as claimed in claim 1, wherein the GTL to crude oil derived diesel ratio is from 99: 1 to 1:99 and the diesel fuel composition produced has a molar H: C ratio of between 1.8: 1 and 2.1:1.
  5. Use as claimed in claim 4, wherein the molar H: C ratio is from 1.9: 1 and 2.00: 1.
EP05752458.9A 2004-04-28 2005-04-22 Use of crude oil derived and gas-to-liquids diesel fuel blends Active EP1756252B1 (en)

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WO2005105961A1 (en) 2005-11-10
ZA200608904B (en) 2008-07-30
EP1756252A1 (en) 2007-02-28
CA2564339A1 (en) 2005-11-10
JP5184881B2 (en) 2013-04-17
NL1028880C2 (en) 2006-02-27
SG152256A1 (en) 2009-05-29
NL1028880A1 (en) 2005-10-31
ES2574652T3 (en) 2016-06-21
US20050279669A1 (en) 2005-12-22
NO20064930L (en) 2007-01-26
CN1950487A (en) 2007-04-18
JP2007535614A (en) 2007-12-06
AU2005238539B2 (en) 2010-07-01
CA2564339C (en) 2011-12-06

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