Wall Wash Sample Water Miscibility-Hydrocarbon Procedure

L&I
7. Analysis – Water Miscibility / Hydrocarbon.
This test serves to determine water immiscible contaminants in wall wash or

cargo samples. The level of detection will vary widely dependent on the solvent
and the type of impurity. The test is qualitative, not quantitative and the results
can only ever be reported as either “Pass” or “Fail”.
The mechanism of this procedure for wall wash analysis is as follows. The wall
wash solvent for the hydrocarbon test is usually methanol or acetone and both
are completely soluble in water. As organic solvents, they also have the ability to
dissolve / extract hydrocarbon residues from the surface of the cargo tank,
(always bearing in mind the solubility of the hydrocarbon in the wall wash
solvent directly impacts how much of the hydrocarbon will be extracted).
When the wall wash sample is mixed with water, any hydrocarbon contaminant
that is soluble in the wall wash solvent, but insoluble in water, is forced out of
the wall wash solvent and shows up as a hazy / turbid emulsion in the solvent-
DI water solution. If the wall wash sample shows any sign of haziness, it is said
to contain water immiscible (hydrocarbon) contaminants and will fail the test.
The relevant test method for hydrocarbon/water miscibility is ASTM D1722,

which states that the wall wash sample must be diluted in a ratio of 1:9 with DI
water (10ml of wall wash sample to 90ml of DI water).
However, it is not uncommon for the hydrocarbon test to be run at dilutions of

1:3 (25ml of wall wash sample to 75ml of DI water) or 1:1 (50ml of wall wash
sample to 50ml of DI water), both of which will have a significant impact on the
final test result. If the hydrocarbon test is part of a wall wash inspection prior to
loading a sensitive chemical cargo, it is essential to know which dilution ratio
will be employed at the load port, otherwise there is an increased risk of failing
the test / inspection.
Equipment Required
1. 100ml graduated glass measuring cylinders with stoppers – (Avoid cylinders

with blue graduation markings where possible because these can interfere
with the interpretation of the results, particularly at low levels of
contamination)
2. Laboratory grade methanol
3. Laboratory grade DI water
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Procedure
1. For each cargo tank sampled, mix 10ml of wall wash / cargo sample with
90ml of lab grade DI Water in the 100ml measuring cylinder. Insert the
stopper and invert the cylinder two or three times, without shaking.
2. Simultaneously, prepare a “reference” sample by mixing 10ml of lab grade

solvent with 90ml lab grade DI water in a 100ml measuring cylinder in the
same way described above. This reference sample is used for comparison
purposes against individual wall wash / cargo samples. It also demonstrates
that the lab grade solvent is pure and free from water immiscible
contaminants.
If there is any haziness or turbidity in the reference sample and this

was the same source of solvent used for the wall wash samples, it may
be necessary to dispose of the wall wash samples and re-take the
samples with on specification solvent.
3. Leave the wall-wash / cargo and reference samples to stand for 20 minutes
before assessing the result.
Reporting
In order to pass the test, the wall wash / cargo samples must be free from any
haziness or turbidity after the 20 minutes standing time, compared to the
reference.
If any hydrocarbons are present, there will be a visual difference between the
test sample(s) and the reference sample. The presence of low levels of
hydrocarbons will typically be identified by the presence of a transparent blue
coloured tinge, compared to the presence of higher levels of hydrocarbons which
will be identified by the presence of an opaque white “milky” emulsion.
Some laboratories shine the beam of a pen-light / torch horizontally through the
measuring cylinder against a black background, which will show up trace levels
of hydrocarbons quite clearly. Strictly speaking, this is not in accordance with
ASTM D1722, but as the test can only be reported as “pass” or “fail” it is difficult
to argue against a rejection on the grounds of subjectivity.
Note. If there is any evidence of foam or bubbles on the top of the liquid
inside the measuring cylinder, this is generally an indication that tank
cleaning chemicals have not been completely rinsed away. This is far more
common in coated cargo tanks compared to stainless steel.
The results of ASTM D 1722 are given as either “Pass” or “Fail” only. There is no
allowance for the degree of failure.
L&I
1 2 3 4 5
. . . .
Pic 1. (Above)
Sample 1. Reference sample – 10/90 Lab methanol & DI water

Sample 2. Result is equal to 10 FTU on Spectrometer (see later) – “Fail” Result
Sample 5. Result is greater than 200 FTU on Spectrometer (see later) – “Fail”
Result
Pic 2 (Right)
Wall wash samples observed

under torch beam.
Sample 1. Reference of 10/90

Lab methanol & DI water
Sample 2. 20 FTU on
spectrometer.
Note that even in the reference

sample, a beam is highlighted
by torch-light.
1 2
. .

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L&I

7. Analysis – Water Miscibility / Hydrocarbon.

This test serves to determine water immiscible contaminants in wall wash or

The relevant test method for hydrocarbon/water miscibility is ASTM D1722,

However, it is not uncommon for the hydrocarbon test to be run at dilutions of

1. 100ml graduated glass measuring cylinders with stoppers – (Avoid cylinders

2. Simultaneously, prepare a “reference” sample by mixing 10ml of lab grade

If there is any haziness or turbidity in the reference sample and this

Sample 1. Reference sample – 10/90 Lab methanol & DI water

Wall wash samples observed

Sample 1. Reference of 10/90

Note that even in the reference

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