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Recently, an engine oil sample was tested to determine the root cause of a failure that resulted in an engine seizing. Initial observation of the oil sample showed it was thick and almost gel-like.
Common causes of engine oil thickening include highly oxidized oil, glycol contamination, thermal degradation and severe soot contamination. Initial analysis of the oil sample revealed that the oil was relatively new additive elements were similar to the reference oilit did not appear to be oxidized reasonable acid numberand there was no sign of glycol contamination or wrong oil added no unusual additive elements were present in the used oil that did not show up in the reference oil.
To sample for soot load, a pentane and toluene coagulated insolubles test ASTM D was run on the sample and results indicated less than 1 percent solids in the sample.
Generally, results of these tests should correlate, but in this case they seemed to disagree with each other. To 8d93 further, two additional pentane insolubles tests by membrane filtration ASTM D were run.
The first test was conducted using a 0. It appeared that a high soot asttm caused the samples to become thick, but it was strange that the pentane insolubles test utilizing centrifugal solids separation did not report similar results. After d8933 investigation, the reason why one test was more successful than the other was discovered. To understand why the results of the pentane and toluene coagulated insolubles test did not coincide with D93 and membrane filtration tests, it is important to know how each test is performed and understand the underlying theories.
Basically, this test separates insolubles from the oil after it has been mixed with solvents. First, a pentane solvent is mixed in with the oil to separate solids and oxidation products from the oil by lowering the viscosity. The mixture is then centrifuged to separate the insoluble material and the insoluble material is measured to determine the percentage of insolubles present.
The test c893 then repeated using toluene instead of pentane. The toluene dissolves organic oxides, but not soot. The mixture is centrifuged again and the insoluble material is weighed.
The difference between the two weights pentane and toluene is the estimated soot content ashm the sample. The TGA method d8893 placing the sample in an oven, where it is weighed continuously as the temperature is increased at specific increments.
An inert nitrogen purge gas is used over asrm sample to enable the oil to evaporate without other reactions oxidation taking place. When the weight stabilizes and remains stable for a certain duration, this signifies that all the oil has evaporated and only insolubles remain.
At this point, oxygen, rather than nitrogen, is introduced, which allows all the carbonaceous material mainly soot to combust and leaves the other metal insolubles in the sample. The soot percentage is calculated by measuring the difference between the weight of the sample before oxygen was introduced to the weight of the sample after it stabilized and all the soot is removed.
However, instead of centrifuging to separate the solid particles from the oil, the oil is passed through a submicron membrane. As the sample passes wstm the fine mesh patch, the insoluble material remains on the upstream surface of the patch while the remaining sample passes through.
The insolubles are then dried and weighed, and the insolubles percentage is calculated.
ASTM D – 14() Standard Test Method for Insolubles in Used Lubricating Oils
Upon speaking to the laboratory personnel, it was discovered that when the pentane insolubles test was run, the additives dispersants in the oil appeared to have kept the soot suspended in the sample. When the sample was centrifuged, the soot d8893 moved along the side of the test tube instead of being forced to the bottom with the other insolubles. Therefore, test results asmt a low insolubles reading. This is further supported by the fact that the soot passed through a 0.
Dispersant additives keep soot from agglomerating.
Two lessons were learned from this discovery. First, had the TGA test or the ASTM D pentane insolubles test using a membrane not also been conducted, the oil analysis results would have shown that soot was not above critical levels usually about 2 percent or 3 percent.
Although more expensive in certain cases, these tests are more appropriate for measuring soot than pentane and toluene insolubles by centrifuge. The customer can oftentimes help when decisions are being made about what tests are most appropriate in a particular application. In addition, if questionable test results are obtained, the laboratory can serve as a good second opinion and troubleshooter.
Toggle navigation Toggle search. Current Issue Archive Advertise. Conclusion Upon speaking to the laboratory personnel, it was discovered that when the pentane insolubles test was run, the additives dispersants in the oil appeared to have kept the soot suspended in the sample.
Standard Test Method for Insolubles in Used Lubricating Oils
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