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Background
Scope (1.1)
• This test method addresses the procedure for determining the ash content from
petroleum products.
o in a range of 0.001 - 0.180 mass %
o applicable to distillate and residual fuels, gas turbine fuels, crude oils, lubricating
oils, waxes, and other petroleum products
Scope (1.1)
• Any ash-forming materials present in the petroleum products are normally considered
to be undesirable impurities or contaminants.
• This test method is limited to petroleum products having no added ash-forming
additives such as phosphorus compounds.
Summary of Test Method (3.1)
• Determining the ash content helps to decide whether or not the product is suitable for
use in a specified application.
o ash can result from oil or water-soluble metallic compounds or extraneous solids
such as dirt and rust
Apparatus
Apparatus (5)
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• Made of platinum, silica, or porcelain,
• Capacity of 90 -120 mL.
Electric Muffle Furnace (5.2)
• Propan-2-ol
• Toluene
Quality Control (QC) Samples (6.3)
• Are portions of one or more stable and representative liquid petroleum materials.
Sampling (7)
Procedure (8.1)
• Mix the sample thoroughly before weighing, when the sample is sufficiently mobile.
o satisfactory mixing can be achieved in 10 minutes by manual shaking or using a
mechanical shaker
• Examine the sample for homogeneity.
• Continue mixing the sample, if it is not homogeneous.
Procedure (8.2.1, 8.2.2)
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• When the sample is viscous or solid at room temperature,
o heat the sample until the sample is entirely liquid and mix carefully
o an oven at an appropriate temperature can be used for heating
• Mix the sample carefully by stirring rather than shaking.
Procedure (8.3)
• Select the quantity of the test specimen based on the expected ash content, as
described in Table 1.
• Select the weighing procedure based on whether the sample requires heating or not,
and whether more than one portion has to be weighed.
Note 3
0.18 11 20
0.10 20 20
0.05 40 20
0.04 50 20
0.02 100 20
0.01 100 10
0.001 100 1
Procedure (8.4)
• Use a top loading balance to weigh the sufficient test specimen to the nearest 0.1 g
into the crucible.
o to yield no more than 20 mg of ash
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• Determine the mass of the test specimen at ambient temperature which is the
difference between the initial and final masses of the sample container weighed at
ambient temperatures.
Procedure (8.6)
• If one weighing is sufficient, carefully heat the crucible with the Meeker burner until
the contents are ignited by the flame.
• Maintain the crucible at the temperature sufficient to burn the sample at a uniform
and moderate rate.
o only the carbonaceous residue is left when the burning ceases
o use a hot plate for burning the sample
Procedure (8.6.1)
• Remove and transfer any test specimen adhering to the glass rod to the crucible
using a strip made of ashless filter paper.
• Continue burning the sample strictly under operator vigilance.
Procedure (8.8)
• Some test specimens will require extra heating after the burning has ceased.
o heavy samples such as marine fuels forming crusts over the unburned material
• The crust can be broken with the glass rod.
o remove and transfer the crust adhering on the glass rod to the crucible using the
strip
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• Burn the remaining test specimen.
Procedure (8.9)
• Heat the residue in the muffle furnace at 775 ± 25 °C until all carbonaceous material
has disappeared.
• Cool the dish to room temperature in the container and weigh to the nearest 0.1 mg.
• Reheat the dish for 20 min, cool and reweigh.
• Repeat the heating, cooling and weighing processes until consecutive weighings
differ by not more than 0.5 mg.
Note
• If more than one addition of test specimen is required, cool the dish to ambient
temperature before adding more samples.
Calculation
Calculation (9.1)
Calculate the mass of the ash as a percentage of the original samples using the formula,
mass % = (w/W)x100
Where,
Report (10)
• Record the value as the ash content, stating the mass of the sample taken.
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Quality Control (QC)
• Confirm the performance of the instrument or the test procedure by analyzing the QC
sample.
• When QC/Quality Assurance (QA) protocols are already established in the testing
facility, confirm the reliability of the test result using the protocols.
• When there is no QC/QA protocol established in the testing facility, use Appendix X1
as described in the standard as the QC/QA system.
The End
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