Wax Test Methods

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Summary of wax appearance and deposition test methods

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Flow AssuranceWAT Testing MethodsCross Polar Microscopy (CPM) most sensitiveUses polarized light and temperature controlled stage to visually determine both wax appearance and disappearance temperatures.Disadvantages: Loss of light end componentsRequires careful temperature calibrationDependent on cooling rate and pre-treatment methodImagingLight ScatteringPrecipitationFiltrationCold Finger Deposition TestIndirectDifferential Scanning Calorimetry (DSC)Compositional Model#2Source: Flow Assurance Course - PETRONAS 2009 + Cranfield UniversityWAT Testing MethodsTest MethodAdvantagesDisadvantagesRecommendationEstimated Accuracy (C)Cross-Polarized Microscopy (CPM)Detection of first wax crystal and subsequent detection of growth rates and morphology via microscopeSmall sample size requiredDifficult to use at high pressure.Can be compromised for highly contaminated samplesRecommended method for WAT measurement.Widely used reliable method with high sensitivity.Requires low cooling rates and high quality samples.1 - 3Differential Scanning Calorimetry (DSC)Detects phase change, relying on exothermic and endothermic phase transition (i.e. melting/solidification) Quick, easy, reliableCan infer solid phase contentFast, unrealistic cooling rates required for good sensitivity.Can give low values (typically ~5C lower than CPM measurements)Less used in industryRepeatable method.Requires good sample quality.Sensitivity can be poor for low wax contents.3 - 5Filter pluggingCan be used for high-pressure testsSimple equipmentVery fine filters required for accurate determination of WATSomewhat subjective method that shouldnt be used as primary WAT measurement.May be confused by precipitation of other solids.8 - 10Near-Infrared (NIR)Simple, visual methodRely on light transmittance, which can be impacted by types of paraffinCan be misleading when asphaltenes are presentCan be used as back-up/confirmation for CPM test2-4ViscosityLarge sample size adds to representativeness. Can use high-pressure viscometer.Subjective interpretationDoes not work for low wax content fluids.Possibly recommended for live crudes with marked WAT, but should be used with caution.10 - 15Cold FingerSample sizeRelatively quick/simple test methodLimited control over cooling rateLimited ability to monitor crystal growthCan be used as screening-level analysis to determine bulk WAT or CWDT5 - 10#3Source: Flow Assurance Course - PETRONAS 2009 + Cranfield UniversityCross Polarization Microscopy (CPM)

34C28C27C25C20C#4Source: Flow Assurance Course - PETRONAS 2009

Wax Appearance vs. DissolutionWax deposits melt at significantly higher temperature than the form- ~10-20C above WAT- Could be as high as 64C (hard deposit)

Wax will re-dissolve into oil at temperature higher than WAT but less than melting point- form slurry flow of wax particles in bulk liquid- impact on fluid rheology

#5Source: Flow Assurance Course - PETRONAS 2009

Wax Content Precipitation MethodPrecipitation Method (BP237/75)Asphaltenes removed from the sampleCrude is dissolved in DCMChilled at -32CPrecipitated wax filtered offWeight of wax collected expressed as % of the amount of starting material

In comparison to an HTGC analyses, wax content measurements from precipitation methods provide a quick screening method to determine the amount of wax in the sample, but they should be used with caution, as they do not provide any information regarding the n-paraffin distribution of the sample.

#6Source: Flow Assurance Course - PETRONAS 2009

Wax Content HTGC Method(Extended n-Paraffin Analysis)High Temperature Gas Chromatography: Compositional method. Determines n-paraffin composition of all n-paraffin components between C15 and C100Required to identify content of higher number of n-paraffin chains. A simple lumped C30+ composition is not sufficientImportance in system design / wax deposition modeling:

Wax content heavily influenced by n-paraffin components at relatively low carbon numbers (C15 to C30) BUT WAT is heavily influenced by n-paraffin distribution at much higher carbon numbers#7Source: Flow Assurance Course - PETRONAS 2009

Similar wax content Similar WAT

Similar wax content. Different WAT Different wax content. Similar WAT#Crude Oil ViscosityViscosities should be measured by shearing the samples at a constant rate and by cooling the sample at a constant rate from above the WAT to the minimum ambient temperature expected in the field. Care should be taken to ensure the fluids are properly handled prior to starting the measurements, A reasonable cooling rate should be used. It is recommended that a cooling rate of 0.5C/minute be used to obtain the most accurate viscosity dataA sealed viscometer should be used to minimize light-ends loss in the sample.

#9Source: Flow Assurance Course - PETRONAS 2009