COLD SOAK

FILTRATION TEST

ASTM D6751-08 Mandatory Annex

ASTM D6751-08 Mandatory Annex

• Cold Soak Filtration became part of the Biodiesel

Fuel Blend Stock (B100) specifications effective
October 13,2008.
 History of the Method

• Cloud point (CP) has been determined to be an

accurate if not conservative indicator of a fuels
Estimated Minimum Operating Temperature (EMOT)

• During winter months in cold climates, Diesel fuel is

formulated to have a lower cloud point.
 History of the Method

• Biodiesel typically has cloud points ranging from

-5C to 20C depending on feedstock
• The blending of B100 into Diesel fuel will typically
raise the CP.
• Final blend CP should still be an indicator of the
Estimated Minimum Operating Temperature.
 History of the Method

• During the winter of 2005/2006 there were a

significant amount of fuel filter plugging issues for
consumers using Biodiesel blends.
• During the winter of 2006/2007, a version of the
Cold Soak Filtration test was implemented in
Minnesota, which seemed to identify B100 that
can affect low temperature operability.
 Why was the Method Developed?

• Some B100 can form precipitate at temperatures

above CP

• The search was on for a test that could identify

B100, that in blends up to B20, shows
precipitation and fuel filter plugging above the CP
Why was the Method Developed?
Watch Video
 What Are Industry Concerns?
• What were the impurities that were the cause of the filter
plugging?
• Potential culprits:
– Monoglycerides
– Soap
– Water
– Sterol Glucosides (plant sterols)
ADM study seems to show a combination effect
• Both the National Biodiesel Board (NBB) and
National Renewable Energy Laboratory (NREL)
have indicated that the, “typical sample will either
pass, or fail miserably.”
• They have further indicated that this largely
depends on the manufacturing processes.
 Method Concerns

• Published interim precision:

200s 360s
– Repeatability 34.0 61.0
– Reproducibility 115.9 208.1
• Lab-to-lab reproducibility will become the focus of
critical attention.

• The following points refer to sections of the

method and require consideration:
• A1.6.1.1
• Funnel and Filter Base with a stainless steel filter
support. The sintered glass support has been
shown to give much higher filtration times and
should not be used. USE ONLY THE SS FILTER
SUPPORT!
• A1.6.2.4
• Glass Fiber Filters, plain, 47mm diameter, nominal pore
size 0.7um.

Intertek uses a standardized filter in an attempt to reduce

variables:
Whatman GFF 47mm Circles,
Part No 1825-047, Fisher 09-874-71
• Sampling A1.9
• DO NOT skip over the "Sampling" section
assuming it contains nothing of importance from a
laboratory perspective! It does!
 Sample Container
A1.9.1 to A1.9.3
• Recommended sample container for this test is a 500ml bottle. Use of this
container might not be logistically possible, so other container sizes are
permissible.
• Sample size must be at least 300ml. An individual sample for CSFT should be
obtained. Samples must be protected from sunlight, amber bottles are preferred.
This test may require sample preparation prior to withdrawing any portion from
the bottle. Typically, other tests are performed on the product, so additional
samples should be available. For example, if a D6751 or EN14214 slate is
requested, typically four individual amber quart/litre boston round bottle samples
will be obtained. If U,M,L level samples are required to be composited, an
additional set should be taken for the cold soak sample preparation.
A1.9.3.1

• It should be known that performing the CSFT

preparation on the sample portion designated for
additional analysis may alter parameters such as
Oxidation Stability, Cetane Number, Methanol content,
Flash point and others.
• If the sample may have been <20C, “thermal memory
removal” must be performed before transfering any
portion of sample.
A1.9.4 through A1.9.5

These sections may be considered confusing and

possibly out of sequence.
• Only in warmer climates or the middle of summer
will it be safe to acknowledge that the sample has
never been exposed to temperatures below 20°C,
(assuming sample is of local origin.). It is also
unlikely that the lab will receive 300ml of sample in
a 500ml bottle.
A1.9.4.1 Sample Preparation

• Heat the designated CSFT sample to 40°C for at

least 3 hours under an inert atmosphere to erase
any thermal history and to dissolve any solids that
might have precipitated during transit. This
preparation is not necessary if it can be clearly
demonstrated that the sample has never been
exposed to temperatures below 20°C. If this is
verified then the test can proceed directly to
A1.9.5.
A1.9.4.2

• After heating for the required time, allow the

sample to sit for at least 24 hrs at a temperature
no lower than 20°C. The 24 hrs is a significant
change to this method. If using ambient air,
assure your lab temperature does not fall below
20°C during the cooling period.
A1.9.5

• Shake the sample vigorously for 1 minute, measure

300ml and transfer to a clean fresh 500ml bottle. A
clear bottle is recommended at this point so that the
sample can be easily inspected for the presence of
visual solids. It is mandatory to pour off 300ml to a
fresh 500ml bottle at this point, regardless of how
the sample was handled in previous steps. The
actual analysis is performed on this 300ml sample
portion in a 500ml bottle.
A1.11.2

• After the16hs cold soak is completed, allow the sample

to come back to room temperature (20-22°C) on its own
without external heating. Filter the sample within 1hr
after reaching 20-22°C.

• The NBB stated, "no external heating above room

temperature, can be interpreted to mean a room temp
water bath".
A1.11.4

• This section contains sequence errors. Applying

vacuum to a dry filter paper will not allow the
operator to set the pressure. Start the vacuum
and set target conditions to achieve 21-25 in. Hg
below atmospheric pressure when the sample is
introduced. The adjustment and recording of
vacuum pressure is handled in A1.11.6.
A1.11.6

• Immediately after swirling, pour the entire contents of the

sample container into the filtration funnel and simultaneously
start the timer. Start the timer immediately the B100 contacts
the filter under vacuum. The vacuum pressure shall be
between 21-25 in. Hg below atmospheric pressure, if not
make adjustments. After one minute, record the vacuum
pressure. 21-25 in. Hg below atmospheric pressure is a fairly
wide range. Higher vacuum pressure could decrease filtration
time. In order to provide process standardization, set the
vacuum pressure in the middle range, ~23 in. Hg below
atmospheric pressure, and maintain using a needle valve for
the duration of the timing.
 Results

• Record the Filtration Time (FT) from the point

where the sample hits the filter until the point that
the filter is visibly free of liquid sitting on top of it.
• If FT is >720s (12min), record final pressure, stop
the test, and record sample amount that had been
filtered.
Test Demonstration