ASTM D 482 Standard Test Method for Ash from Petroleum

Products
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)

The sample contained in a suitable vessel is ignited.

The ignited sample is allowed to burn until only ash and carbon remain.
The carbonaceous residue is heated in a muffle furnace at 775 C, and reduced to
ash.
The ash is cooled and weighed.
Significance and Use (4.1)

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)

Evaporating Dish or Crucible

Electric Muffle Furnace
Meeker Gas Burner
Mechanical Shaker
Evaporating Dish or Crucible (5.1)

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 Made of platinum, silica, or porcelain,
Capacity of 90 -120 mL.
Electric Muffle Furnace (5.2)

Capable of maintaining temperature of 775 25 C.

Has apertures at front and rear to allow slow natural draught of air to pass through.
Reagents (6)

Propan-2-ol
Toluene
Quality Control (QC) Samples (6.3)

Are portions of one or more stable and representative liquid petroleum materials.
Sampling (7)

Obtain samples in accordance with ASTM Practice D 4057 or ASTM D 4177.

Transfer the portion of the sample to the crucible,
o after ensuring that the portion taken is representative of the larger portion
Shake the sample vigorously.
Procedure

Procedure (8.1)

Heat the crucible at 700-800 C for a minimum of 10 minutes.

Cool the crucible to room temperature in a container.
Weigh the crucible to the nearest 0.1 mg.
Procedure (8.2)

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)

When the sample is not homogenized after repeated mixings,

o use a non-aerating, high-speed shear mixer as per ASTM D 4928
When the sample cannot be satisfactorily homogenized,
o reject the sample and acquire a new sample
Procedure (8.2.3)

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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

The container can be a desiccator not containing a desiccating agent.

All weighings of the crucible should be performed immediately after cooling the
crucible.
Table 1- Test Specimen Mass versus Ash Content

Test Specimen Ash Mass

Expected Ash (mass %)
Mass (g) (mg)

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)

The sample may contain water causing spattering effect.

o it is advisable for an operator to heat the sample cautiously by wearing personnel
protective equipment such as safety goggles and gloves
o discard the test portion when the sample escapes the confines of the crucible
due to severe spattering
Procedure (8.6.1)

If the first test portion is discarded, add 2 1 mL of flammable propan-2-ol to a

second test portion,
o while stirring the second test portion with a glass rod and warming it gently to
liquefy, if it is solid
If this is unsuccessful, repeat the process on a third test portion using a 10 1 mL
mixture of toluene and the propan-2-ol,
o each weighing 50 5 % by volume
o take care since toluene is flammable and its vapor harmful
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)

Avoid foaming of heavier material with considerable care.

Avoid overheating to prevent a red hot appearance of the test specimen or the dish,
and loss of ash.
Maintain the flame ignition level to be below the rim of the dish to avoid superheating
of the crust and sparks.
Procedure (8.10, 8.11)

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,

w - mass of ash (in g)

W - mass of sample (in g)

Report (10)

Record the value as the ash content, stating the mass of the sample taken.

Test Specimen Mass, g Report to

9.00 - 39.99 3 decimal places

40.00 3 - 4 decimal places

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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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