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Wall Wash Procedures Manual Watermarked
Wall Wash Procedures Manual Watermarked
Wall Wash Procedures Manual Watermarked
Contents.
1. Introduction.
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1. Introduction.
Whilst the chemical analysis on a wall wash sample, performed correctly (in
accordance with ASTM test methods) will accurately define a result which can be
both repeated and/or reproduced, the same can not be said for the process of
wall wash sampling.
Wall wash samples can and will differ between two separate samples taken
independently, from the same tank. Therefore, results can be different. One
sample may pass, the other fail.
The reason for this is more clearly understood when a surveyor/crew member,
takes samples from areas blind to the full effect of the tank cleaning machines
or perhaps from sloping bulkheads, as opposed to samples taken from areas
where the cleaning machines have direct action to the bulkheads.
At best, the process of wall wash sampling is random and only reflects the areas
where the samples are drawn from, normally the bottom 2.5meters of the tank
bulkheads. It is not representative of the condition of the whole tank.
For this reason, it is also important to follow the suggested ‘Wall Wash Sampling
Procedure (4) below, as this at least, standardizes the technique for all tanks.
2. Visual Inspection.
If previous cargo(es) were viscous, check machine blind areas, blind side of angle
brackets and under heating coils.
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Take a clean white rag and wipe surfaces, nothing should come off onto the rag.
No grease or any lose dust, rust spotting must be removed.
For Epoxy tanks, coatings should be sound. Lose or flaking surfaces should also
be made sound. In general, coating breakdown should not be greater than 2% of
the total tank surface area.
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Odour, during the visual inspection can also be a problem. Tanks should not
retain the smell of previous cargo(es) or from washing chemicals.
1. Clear Glass Sample Bottles. 500ml. Best to use new, chemically clean
bottles.
(If you are re-using bottles, make sure they have been carefully washed
with a final D.I. rinse followed by two flushes with Laboratory grade
Methanol).
2. Plastic Cut or Stainless Steel Funnel, Approx 10 - 14 cm Diameter.
3. Plastic Squeeze wash bottle with tube. 500ml.
4. Laboratory Grade Methanol. 500ml per tank.
5. Eye Protection glasses.
6. Latex / Nylex gloves.
7. Shoe covers.
8. Marker pen. (Preferably ‘paint marker’. Methanol will wash away labelling
from most permanent markers).
9. Portable Gas Detector. (Leave this at the bottom of the stairwell or in your
back pocket. It will give an alarm from the methanol vapours if you have it
on your top pocket).
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Don’t touch or lean against bulkheads – loadport surveyor may take a sample
from that area!
Do not wall wash tanks that are wet. Water or moisture will affect the ability of
the methanol solvent to absorb contaminants from the coating and may also give
misleading chloride values. It is also best not to wall wash tanks when too hot,
as the methanol will evaporate quickly.
The aim is to finish with a sample that represents the chemical condition of the
whole tank. However, in practice it is only (normally) taken from random spots
on the lower 2.5 meters of the bulkheads. This ‘random choice’ means that no
two samples will be exactly the same and it is quite possible for one sample to
pass the tests, whilst another can fail. And of course, upper tank levels are not
represented.
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Added together, these will give you an area of approximately 1 square meter
sampled. Chose areas that will help represent some good and some of the worst
(blind spots) of the bulkheads. It is better we know the worst, rather than the
inspectors.
If you know of any specific areas where you expect problems, take a separate
sample of just that spot, (machine blind area or upper tank level) to test
separately.
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Observe the methanol as it flows down the bulkhead surface. If oil is present or
perhaps a film of Veg Oil remains, you may observe small ripples. Watch the
area washed as the methanol evaporates. If you observe brown ‘burn marks’ to
the edges, it can indicate the presence of Non volatile matter (NVM), which can
lead to failure on Hydrocarbon and/or PFT.
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Rinse the sample bottle cap with clean methanol and close securely. Mark the
bottle with the relevant tank number. Good sample identification is important.
Be aware that most marker inks will dissolve in methanol.
Analysis Procedures.
Equipment Required
1. Sample bottle of pure methanol – for comparison as blank.
2. Tank wall wash samples.
Procedure.
Compare each tank wall wash sample with a blank sample of pure methanol.
The individual wall wash samples should have the same clear and bright
appearance as the pure methanol.
Note any sediment in the bottom of the bottle and report.
Note any matter still suspended in the sample (fibres etc) and report.
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1 2 3 4 5 6
. . . . . .
Sample 1. Blank Laboratory Grade Methanol. Will be ‘Clear & Bright’ and
without any ‘Suspended Matter’ or ‘Particles/Sediments’. Sample equivalent is
‘Pass’
Sample 2. ‘Clear & Bright’ with some very slight ‘Suspended Matter’ and
Particles that settle out to the bottom of the bottle. This sample should be
acceptable. Sample is ‘Borderline’.
Sample 3. ‘Clear & Bright’ with more obvious ‘Sediment’ which settles out to the
bottom of the bottle. This sample would fail the appearance test. Sample is ‘Fail’.
(Tank may need spot sweeping or flushing with D.I water to remove).
Sample 4. ‘Clear & Bright’ with heavy ‘Sediment’ settling out to the bottom of
the bottle. This sample fails the appearance test. Sample is ‘Fail’. (Tank will
likely need flushing with D.I. water to remove).
Sample 5. ‘Hazy’ appearance, with (or without) ‘Sediment’ and ‘Suspended
Matter’. Sample fails the appearance test. Sample is ‘Fail’. (Tank will likely need
re-washing).
Sample 6. Sample is coloured and will therefore fail the test. This comes into
appearance of sample based on the colour, which could be the effect of a dye
used in previous cargo(es). (APHA colour is based on a ‘yellow’ scale).
In section 2. Visual Inspection, it was noted that on entering the tank, any
noticeable odour should be reported. This can be particularly relevant where a
cargo like Styrene Monomer was the last cargo. Such odour should be removed.
For the wall wash samples, there is a test for ‘Odour of Volatile Solvents and
Diluents’ ASTM D 1296.
Any solvent used for wall wash sampling, normally methanol, is a hazardous,
toxic substance so it is inadvisable to inhale. The test method is based on
immersing strips of absorbent paper into the Laboratory Grade methanol and
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Most ships will have a box of ‘filter paper’ (circles) on board, which can be used.
(Make sure they are clean and odour free before use. These can be cut into
strips of around 25mm x 75mm.
If the odour is the same, Report the Odour result as ‘Characteristic’. (MCO –
Methanol Characteristic Odour). If you detect a difference in the odour, report
the result as Non-characteristic. (NC – Non-Characteristic).
For Non Residual or Residual’ odour, allow the absorbent paper to dry. The
Laboratory Grade Methanol should not have any residual odour, and would be
reported as Non-Residual. Compare this with the wall wash sample. If you detect
a lingering odour, this would be reported as ‘Residual’.
This test serves to determine water immiscible contaminants in the wall wash
sample. The level of detection will vary widely dependent on the solvent used for
wall wash and the type of impurity. However, the test is qualitative, not
quantitative. Results are either ‘Pass’ or ‘Fail’.
Methanol is soluble in water. When a wall wash sample is mixed with water, any
contaminant which is soluble in the methanol, but insoluble in water is forced
out of the methanol and shows up as haziness in the methanol-DI water
solution. The turbidity is actually composed of emulsified contaminants
scattered evenly throughout the solution and can be seen as a ‘blue-ish tinge’ or
opaque, milky turbidity.
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Equipment Required.
On board Procedure.
1. Using the Laboratory grade methanol, make up a 'blank' sample with 10ml
Laboratory grade methanol and 90ml Laboratory grade D.I. Water. (This
'blank' sample is used for comparison purposes against your individual tank
samples. It also proves your blank methanol is clear and free from
contaminants. If there is any haziness or turbidity in the blank sample –
same source methanol as used for wall wash, you will have to throw all away
and start again, as all samples will be contaminated!)
2. For individual tank samples, mix 10ml of wall wash sample with 90ml of
Laboratory grade D.I. Water.
Samples should be well mixed, invert the glass cylinders, mix with mild
agitation, leave for 20 minutes before reading the result.
Reporting.
Samples must be free of any haziness or turbidity. Compare with the blank
sample. If Hydrocarbon is present, you will see a blue-ish tinge if slight
Hydrocarbons to a milky haziness for heavier Hydrocarbons. The degree of
the haziness indicates the degree of contaminant that has been picked up
by the wall wash sampling. Some surveyors will use a torch beam to
‘highlight’ any turbidity in the sample. Place the tubes against a black
surface in a darkened room and pass a torch beam horizontally through the
sample tube. If the sample shows any cloudiness/turbidity compared to the
blank, the sample fails the test.
Also note if there is any foam on the surface. This can indicate that washing
chemicals have not been completely rinsed away.
Results are given as either 'Pass' or 'Fail'. There is no allowance for the degree of
failure.
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1 2 3 4 5
. . . .
Pic 1. (Above)
Sample 1. Blank of 10/90 Lab MeOH & D.I. – Pass Result.
Sample 2. Result is equivalent of 20 FAU on Spectrometer. – Fail Result.
Sample 3. Result is equivalent of 50 FAU. – Fail Result.
Sample 4. Result is equivalent of 200 FAU.- Fail Result.
Sample 5. Result is greater than 200 FAU. – Fail Result.
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The Platinum Cobalt Scale Test describes the visual determination of essentially
light coloured liquids (yellow scale). For most accurate visual determinations,
you will need ‘long stem’ clear glass tubes and Platinum Cobalt Colour
standards. As you will note from the below Colour examples, the colour
variations between 0, 5, 10 and 20 on the Pt-Co scale is minimal. For Methanol
standard wall wash, it is usually required that the wall wash sample is ‘less
than 10’. In some cases, ‘less than 5’. If you do not have long stem tubes, use
100ml tubes as substitute.
Equipment Required.
Procedure.
1. Use tubes of the same length. Decant 100ml fixed mark with Laboratory
Grade methanol.
2. Take the appropriate colour standard into a glass tube to 100ml, or same
fixed mark on the tube.
3. Decant the same quantity of each wall wash sample into similar tubes and
fill to same level as the blank and the standard.
Reporting.
Looking down the length of each tube against a clean white background,
compare the blank sample against the required colour standard to confirm
your Lab Methanol is clear.
If you are working to a colour standard of max 10 Pt-Co, use the Pt-Co 10
standard and compare this with your wall wash samples. If they are lighter
than the standard, you can report the result as ‘less than Pt-Co 10’. If they
are darker, they do not meet the specification required. (You can also report
‘greater than’ the particular standard – if you do not have the next required
colour standard).
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see a yellow tinge in your wall wash sample, this will likely not meet Pt-Co
10. Of course, any other noticeable colour will also fail the test.
Blank Pt-Co ‘0’ Pt-Co ‘5’ Pt-Co ‘10’ Pt-Co ‘15’ Pt-Co ‘20’
This test is a non quantitative, non specific analysis for oxidizable contaminants
found in the wall wash sample. These can be from previous cargoes or even
traces of detergents used in the tank washing process.
The chemical principle behind this test is the colour change permanganate
undergoes as it oxidizes contaminants. Permanganate is purple in solution and
as it is consumed in the oxidation process, it is transformed into brown
Manganese dioxide. Where the contaminant is acid, the purple permanganate is
converted to colourless Manganese ions. The rate of the reaction is dependent on
the amount of contaminants: the more contaminants in the sample, the faster
the colour change.
Prepare the Cool box with Ice to maintain a 15 deg C temperature. Water
level to equal level of liquid in the test tubes.
clear glass bottle with silver foil), Keep in cool dark place when not in use -
fridge if possible.
Procedure.
Reporting.
Check the samples every 10 minutes. For most Methanol loadings, the
samples should maintain their 'Purple/Pink' colour for 60 minutes. (Some
loadports allow 50 minutes and for MEG, 30 minutes is the normal
specification. You should know the 'test time' specification for the applicable
cargo and load port).
Pure Laboratory Grade Methanol should maintain its Pink colour for well
over 60 minutes.
Having noted the time the Potassium Permanganate was added and placed
the samples in the cooler/darkness, after 10 minutes, check the colour of
each tank sample. Check the ‘blank’ sample (which should not have lost any
of its Purple/Pink colour). When checking the samples, also make a
temperature check to see the 15C (+/- 1C), is maintained.
Compare the tank samples with the blank sample. Colour should maintain
its 'pink' hue. If this colour degrades to an orange/brown/yellow, no pink
hue remains to the colour, the time should be taken.
Reporting will be based on the ten minute intervals. So if a sample has lost
its pink colour when you check the results after say 30 minutes, then the
time is reported as 'less than 30 minutes' (< 30). If the colour is still similar
to the blank, with a pink/purple colour then continue the test to the next 10
minute check time.
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In cases where the samples fade to a clear colourless solution before the
specification time, this is still a failure and can indicate that the contamination
is acid based, as below image.
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This test determines the level of Chloride in the wall wash sample, which will
normally be present from earlier seawater washing. This can also come from
fresh water. Typically seawater may have a chloride content around 15,000
to 20,000 ppm. Normal freshwater, around 300 to 500 ppm. Technical grade
D.I water, used for tank spraying, should be below 0.5 ppm.
The chemical principle behind this test is the formation of insoluble silver
chloride, when any chloride from the wall wash sample reacts with the silver
from the silver nitrate reagent. This reaction can be seen as turbidity after
adding the reagent. The level of turbidity indicates the level of chloride in the
sample.
The reaction is a 1:1 ratio. So, 1 part of chloride will react with one part of
silver. Silver nitrate is sometimes supplied as 2% or 5% or in some cases
10% concentration. A 2% concentration is equivalent to 20,000 ppm of silver.
If we use 5 drops of 2% concentration, we have the ability to react with up to
approximately 200 ppm of chloride. If we used a 5% concentration, we would
have sufficient concentration from 5 drops, to react with up to 500 ppm
chloride.
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As we are looking for chloride levels of less than 10 ppm, typically 2 ppm or
less, we do not need to use more than a 2% concentration. (We could even
use 1% and it would be quite sufficient to precipitate the expected chlorides
in a methanol wall wash sample).
Equipment.
Laboratory grade Methanol.
Graduated 50ml glass cylinders, with 25ml graduation.
Silver Nitrate 2% or 5%.
Nitric Acid 20%
*Or, (Acidified Silver Nitrate 2% or 5%)
Dropper Bottle or pipette.
Standard Chloride Solution. 10ppm
‘* Laboratory prepared reagent based on Nitric Acid 20% and Silver Nitrate
2%
Procedure.
From tank wall wash samples, decant 25ml of sample to test tube.
Add 5 drops Nitric Acid 20% and 5 drops Silver Nitrate 2% (or 5%) to each of
the above samples. (If you have Acidified Silver Nitrate, you can just add 5
drops of this reagent.
Reporting Results.
In much the same way as you read the Hydrocarbon results, darken the
room and compare the blank sample against your Chloride Standard. The
blank should have no turbidity. Then compare your wall wash sample
against the Chloride standard.
Using a 10ppm standard, if your wall wash sample is less turbid, you will
report ‘less than 10ppm’. If more turbid, ‘greater than 10ppm’.
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0 0.2 1 2 5 10
ppm ppm ppm ppm ppm ppm
0 0.2 1 2 5 10
ppm ppm ppm ppm ppm ppm
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0 0.2
ppm ppm
Scope:
This method covers the determination of the acid wash color of benzene,
toluene, xylene, refined solvent naphtha and similar hydrocarbons. The test
is also used for detecting impurities in Methanol.
Definition:
Acid wash color: The color developed in the separated acid when a sample is
agitated with sulphuric acid under the conditions described in this method.
Apparatus:
Acid wash color standards, numbered 0 to 14.
Stoppered cylinders, 30 ml.
Sulphuric Acid 96%. (For High Flash solvent or Heavy Solvent Naphtha, use
Sulphuric Acid 78%. See below chart.)
Toluene (or Xylene) to be used as wall wash medium.
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Procedure:
Fill a dry and clean 30 ml glass stoppered cylinder up to the 7 ml mark with
acid of the strength specified in Table 1 for the type of sample to be tested.
Insert the stopper, hold a finger over the stopper and give vigorous shakes
with a stroke of 10 to 25 cm, shaking for a total of 150 cycles over a period of
40 to 50 seconds, that is at a rate of 3 to 3,75 cycles per second.
Allow the cylinder to stand, protected from direct sunlight, for the period of
time shown in Table 1.
Without further delay invert the cylinder gently once or twice to obtain a
uniform color in the acid layer and compare the color of the acid layer with
those of the standards. Make the comparison against a white background or
at daylight.
Designate the color of the acid layer by the number of the nearest matching
standard and add to the number a plus or minus sign if the sample is
respectively darker or lighter than the standard color.
Note: Concentrated sulphuric acid will cause severe burns on contact with
the skin. When spilled, remove with plenty of water.
When performing the test, use clean plastic disposable gloves. Ensure the
test tube and top make an effective seal.
Table 1
Acid strengths and standing times
Sample Acid strengths Standing time
Group 1 Benzene, all ASTM grades 96% l5min
Toluene, all ASTM grades
Xylene, nitration grades
Xylene 5º
Xylne l0º
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Good organization.
Safety.
Cleanliness.
Reliable results.
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Good organization is very important when working in any laboratory. Clear
operational practices help ensure equipment is in good condition and properly
clean for use. Correct recording of results is absolutely essential. (You don’t want
to be re-cleaning the wrong tank!)
When you have finished your analysis, it is a golden rule to clean all your
equipment before putting it away; and just as important to ensure it is cleaned
before using on the next occasion.
Glassware does stain over usage. You will see this particularly after tubes used
for PFT (Potassium Permanganate Fade Time) analysis. The tubes will show a
brown staining, which needs to be removed, as noted above.
Safe working practices come from good organization. Ensure the space is well
ventilated and cool.
Use latex gloves when handling chemicals and chemical resistant gloves when
handling acids. (Avoid the powdered type latex gloves).
Eye glasses should be worn and an eye wash bottle should be on hand.
Solvents and Reagents should be clearly labelled and securely stored in a cool,
dark and dry space. Ensure they are well sealed after use. Labels should
indicate an expiry date.
Make random tests on newly delivered stocks of Lab Grade Methanol and
D.I.Water, to ensure their integrity.
Record Results immediately and after each step. Keep a formatted results log so
you can compare results as the cleaning progresses.
Glassware.
100 ml tubes will be required for the Hydrocarbon analysis. Best to avoid blue
graduation markings as these can lead to mis-interpretation when reading
results visually. Detachable plastic bases are good as they can be removed and
the tubes used in a rack.
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50 ml tubes are best for use in both Chloride and PFT analysis. Glass or plastic
stoppers are best as they are easier to keep clean.
100 ml ‘Long stem’ Glass cylinders are used for Colour determinations.
Sufficient quantity should be available for testing all tanks, per test. Saves
considerable time, especially when checking PFT. The test needs to run for one
hour, so best to check all necessary tanks in one batch.
General Equipment.
Plastic 500 ml Squeeze bottles, with spray tube tops. (2 for wall washing,
2 for Lab use).
Plastic or Stainless Steel wall wash funnels
Dropper bottles – 30ml.
Glass Pipettes, 2ml & 10 ml.
Plastic Pipettes, 2ml disposable.
Plastic disposable shoe covers.
Latex disposable (unpowdered) gloves.
Cool (Igloo) Box. (sufficient size to take rack of 50 ml tubes).
Glass Cylinder racks. (Correct size for Glass 100 ml & 50 ml tubes).
500 ml clear glass sample bottles. (Sufficient stock for wall wash samples
from tanks.
500 ml amber glass sample bottles. (For mixing of Potassium
Permanganate solution.
Mag-light type torch.
Standard Solutions.
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New deliveries of Methanol and D.I. Water supplies should be randomly checked
for purity.
Supplies of reagents should be properly labelled and show an expiry date.
The above list is not exhaustive, but will allow you to perform all basic and
usual testing for Methanol Standard analysis.
Using the L&I Wave 11 Spectrometer, has distinct advantages for reporting of
your wall wash analysis results. For the normal wall wash analysis tests, the
scaled results given by the Spectrometer are definitive and allow you to see the
improvement (or lack of improvement), as your tank washing progresses.
Tank wall wash sampling and analysis is performed in the same way as
described above. However, the Spectrometer very accurately reads the sample
giving you a scaled result.
For wall wash analysis, this is extremely important. Load port surveyors will
normally take their samples to a shore lab where results are determined using
specialized equipment. The analysis is performed by a chemist in laboratory
conditions. They are ethically bound to report the result they find. Where you
have a Chloride maximum specification of 2 ppm, if they find 2.1 ppm, you
technically fail the test. Where a colour specification is maximum APHA 5 and
they find APHA 6, again you fail.
Visually you really can not tell the difference in either case. Most Masters, Chief
Officers, will clean to well below these standards to be sure of passing. This is
expensive and possibly un-necessary.
Using the Spectrometer also puts you in a better position to ‘know exactly’ the
condition of your tanks not only before tendering your NOR, but during the
washing process.
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Tank Coatings.
• Organic coatings are made from extenders, pigments, fillers all held
together in organic solvents (hence the name), typically higher alcohols
and aromatics.
• As such, there is an inherent attraction between the coatings and all
organic cargoes … a massive amount of cargoes.
• Experience tell us which cargoes are most absorbed (and retained) and
these are what create the greatest tank cleaning challenges, because
there are really only two ways of removing cargo residues once they have
been absorbed.
i.) Heat.
ii.) Transmission into another cargo.
• However - If the retained residues are transmitted into a cargo that is
sensitive, it may become contaminated.
Looking at Organic coatings, it is their ability to retain these lighter grades that
makes cleaning for later high grade or sensitive cargoes a significant problem.
The most common “nasties” that are absorbed into organic coatings are:
• Styrene Monomer
• Methanol / Ethanol
• EDC / MEC
• VAM
• Acrylates in general
Residues of these cargoes can be retained in the coating for months until they
are completely desorbed.
We also, can not rely on the pre-loading wall wash tests, to confirm the coatings
are free from trace contaminants that will cause a sensitive cargo to be found
‘off-Spec’ at the next disport.
Remember the contact time of the methanol during wall wash is minimal. The
contact time for the cargo will be days or weeks.
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UV Graph Display.
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The below graph, illustrates the ‘read-out’ on a series of Wall wash samples
taken during tank washing from last cargo ‘Styrene Monomer’
The smooth ‘blue’ curve is the UV read-out for Pure, Lab Grade Methanol. The
remaining read-outs illustrate ‘peaks’, consistent with levels of contamination of
the sample from Styrene Monomer.
The tanks had received initial pre-washes with the 1st wall wash taken
(18/09/11), prior to making a hot wash.
You will note that on the 2nd wall wash (20/09/11), the graph shows the sample
has picked up an increased level of contamination. This is likely due to the hot
wash opening the coatings, allowing the methanol to more easily penetrate and
absorb a higher level of the Styrene.
It is also important to note, that all parameters of the wall wash tests, including
PFT, passed on normal Ethylene Glycol load port requirements.
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We can see whether our tank cleaning plan is working and amend as necessary
to optimize efficiency.
You might have noted in the above graph, the line display is not the same as the
earlier graph examples given for Styrene Monomer, Phenol and Acrylonitrile.
The example graphs for Styrene Monomer, Phenol and Acrylonitrile are based on
a flat line graph.
The above graph showing the improvement over the cleaning time, is based on a
curve graph.
The curve graph is useful to us because we can use this procedure to show what
the pure methanol looks like. A smooth curve (Pure Methanol/Dark blue line).
This is our blank sample to compare with the wall wash samples. We actually
want our wall wash samples to look the same, just as we make a blank sample
for Chloride, Hydrocarbon and PFT testing. We use the bank as a reference ‘for
the perfect result’. If it doesn’t appear the same, we know there is some
contamination in the wall wash sample, just as in the Chloride sample being
more turbid than the blank, we know there is contamination. The UV helps us
to find out what this can be.
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L&I LIGHTWAVE 11 – Spectrophotometer.
The L&I menu offers the choice of programs for determination of results for;
The unit is supplied with full user manual and L&I instructions for test procedures. On
request, L&I can also provide accessories to the base unit. Hard carry case. Additional
crystal 40 mm cells and 10 mm UV quartz cell.
L&I also provide full training programs for ASTM wall wash analysis testing and use of
the Lightwave 11 Spectrometer.
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Dissolve 10 g of silver nitrate in 500 ml of 20% nitric acid. Store this solution in a dark bottle.
Alternatively, separate solutions of 2% silver nitrate and 20% nitric acid can also be used just as
successfully.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are accepted,
the instrument is calibrated and ready for use. A screen showing four files is shown.
2. Press the button relating to the LI Maritime Programs, file number 2.
3. Press the button relating to 950 Chloride in MeOH. The tests can now be performed.
4. Transfer 25 ml of test sample into an appropriate sample tube.
5. Add 5 drops of the acidified silver nitrate reagent, or 5 drops each of 2% silver nitrate and 20%
nitric acid.
6. Prepare a zero sample (reference sample) to run concurrently, by following steps 4 and 5
using reagent grade (pure) methanol. Leave to stand for 15 minutes.
7. After 15 minutes, follow these instructions.
8. Fill one Hach 25ml glass cell to the mark with the prepared reference sample and insert into
the square cell holder with the mark facing left, ensure the cell is seated fully in the cell
holder.
9. Press the 0A/100%T button to set the instrument to zero. Once the instrument is zeroed, it
does not display any result, 0.000 can be seen in the Absorbance box.
10. Remove the reference sample from the instrument and pour it back into the reference sample
tube.
11. Rinse the same glass cell with the test sample and then fill to the line before inserting into the
instrument, with the mark also facing left. Press the GREEN button and read the ppm of the
CHLORIDE directly from the Concentration box.
12. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by repeating steps 8 and 9.
Interpretation of Results
The chloride content of the test sample in ppm, is read directly from the instrument.
Interferences
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Procedure
1. Switch the L&I Wave II instrument on. After a few seconds, and if all self checks are accepted,
the instrument is calibrated and ready for use. A screen showing four files is shown.
2. Press the button relating to the L I Maritime programs, file number 2.
3. Press the button relating to 951 Permanganate Test, the test can now be performed.
4. Prepare a water bath at 15 C 1 C
o o
5. Fill a sample tube with 25 ml of the test sample and place it in the bath for at least 10 minutes
o
to allow it to cool down to 15 C
6. Now add 1 ml of the potassium permanganate reagent to the sample tube, mix the contents
well and replace in the bath. Note the time
7. Leave the sample tube in the bath for 50 minutes, or whatever length of time the potassium
permanganate time test specification is set at
8. Fill one Hach 25ml glass cell to the mark with pure methanol, with no potassium
permanganate solution added (reference sample) and insert into the square cell holder with
the mark facing left
9. Press the 0A/100%T button to set the instrument to zero. Once the instrument is zeroed, it
does not display any result, 0.000 can be seen in the Absorbance box.
10. Remove the reference sample from the instrument
11. Rinse the same glass cell with the test sample and then fill to the line inserting into the
instrument, with the mark also facing left. Press the GREEN button and read the % TRANS
PTT directly from the Concentration box.
12. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by following steps 8 and 9.
Interpretation of Results
Samples having a reading greater than 35.0 % by this procedure, will still show a pink
colour, and pass the test
Samples having a reading less than 35.0 % by this procedure will appear to be brown in
colour, and fail the test
Interferences
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Range APHA 5 – 500 in line with ASTM D 1209 on the Platinum - Cobalt scale.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds, and if all self checks are accepted,
the instrument is calibrated and ready for use. A screen showing four files is shown.
3. Press the button relating to 952 APHA Colour, the test can now be performed.
4. Fill one Hach 25ml glass cell to the mark with pure methanol (reference sample) and insert
into the square cell holder with the mark facing left
5. Press the 0A/100%T button to set the instrument to zero. Once the instrument is zeroed, it
does not display any result, 0.000 can be seen in the Absorbance box.
7. Rinse the same glass cell with the test sample and then fill to the line before inserting into the
instrument, with the mark also facing left. Press the GREEN button and read the COLOUR
reading directly from the Concentration box.
8. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by following steps 4 and 5.
Interpretation of Results
The colour of the test sample is read directly from the instrument
According to the ASTM reference the colour should be reported either as an exact multiple
of 5 or “lighter than” the next highest multiple of 5 whichever is the most appropriate
Interferences
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953 Hydrocarbons
Range Pass or Fail in line with ASTM D 1722.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds, and if all self checks are accepted,
the instrument is calibrated and ready for use. A screen showing four files is shown.
2. Press the button relating to the L I Maritime programs, file number 2.
3. Press the button relating to 953 Hydrocarbons, the test can now be performed.
4. Add 10ml of the methanol test sample to 90 ml of distilled water, in a suitable sample tube.
5. Invert the tube once or twice to mix the water and methanol.
6. Prepare a zero sample (reference sample) to run concurrently, by following steps 4 and 5
using reagent grade (pure) methanol instead of the test sample.
7. After 20 minutes follow these instructions.
NOTE: To avoid the formation of air bubbles in the sample cell, samples should be
transferred very carefully. Similarly, the sample tube should not be re-inverted after the
initial mixing. If air bubbles are present in the sample cell at the time of analysis,
inconsistent results may be observed.
9. Fill one Hach 25ml glass cell to the mark with the prepared reference sample and insert into
the square cell holder with the mark facing left
10. Press the 0A/100%T button to set the instrument to zero. Once the instrument is zeroed, it
does not display any result, 0.000 can be seen in the Absorbance box.
11. Remove the reference sample from the instrument and keep it for future reference (if required)
12. Rinse the same glass cell with the test sample and then fill to the line before inserting into the
instrument, with the mark also facing left. Press the GREEN button and read the Hydrocarbon
value (in FTU) directly from the Concentration box.
13. It is advisable to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by following steps 9 and 10.
Interpretation of Results
All results are relative to the reference sample. The results are quoted in formazine turbidity units
(ftu), they do not directly relate to hydrocarbon concentration (ppm).
Samples having a reading greater than 0 by this procedure fail the test
Known Interferences
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Dissolve 10 g of silver nitrate in 500 ml of 20% nitric acid. Store this solution in a dark bottle.
Alternatively, separate solutions of 2% silver nitrate and 20% nitric acid can also be used just as
successfully.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds, and if all self checks are
accepted, the instrument is calibrated and ready for use. A screen showing four files is
shown.
2. Press the button relating to the L I Maritime programs, file number 2.
3. Press the button relating to 954 Chloride in Water. The tests can now be performed.
4. Transfer 25 ml of sample water into an appropriate sample tube.
5. Add 5 drops of the acidified silver nitrate reagent, or 5 drops each of 2% silver nitrate and
20% nitric acid.
6. Prepare a zero sample (using laboratory DI Water) to run concurrently, by following steps
4 and 5. Leave to stand for 15 minutes.
7. After 15 minutes, follow these instructions.
8. Fill one Hach 25ml glass cell to the mark with the prepared reference sample and insert
into the square cell holder with the mark facing left, ensure the cell is seated fully in the
cell holder.
9. Press the 0A/100%T button to set the instrument to zero. Once the instrument is zeroed, it
does not display any result, 0.000 can be seen in the Absorbance box.
10. Remove the reference sample from the instrument and pour it back into the reference
sample tube.
11. Rinse the same glass cell with the test sample and then fill to the line before inserting into
the instrument, with the mark also facing left. Press the GREEN button and read the ppm
of the CHLORIDE directly from the Concentration box.
12. It is recommended to regularly check that the reference sample still reads zero. If the
reading shows any significant drift, reset the reference by repeating steps 8 and 9.
Interpretation of Results
The chloride content of the test sample in ppm, is read directly from the instrument.
Interferences
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The following guidelines are written to provide the user with a convenient reference document and
to familiarise the user with the sometimes unique responses that this spectrophotometer can
provide. This guide should not be used in place of the manufacturer’s instrument manual or in
place of the method cards provided to determine various Wall Wash Test parameters.
This instrument can be run on either 120 or 240V mains supply and is supplied with UK, US or EU
mains cables. The instrument should be sited on a dry, flat surface. Due to its mode of operation,
its readings are stable, even in relatively rough seas.
Instrument start-up
After switching this instrument on, a series of rapid self-calibration tests are performed. During
this switch on, the cell holder area should be free from cells. If there are any problems during the
switch on, the faults will be reported by the instrument and the user advised how to remedy the
problem. After successful switch on, the screen will show 4 optional files.
To allow the optical and electrical components to stabilise it is recommended to allow a minimum
of 15 minutes for the unit to warm up.
There are two sets of sample cells and sample cell holders supplied with this instrument.
For ‘visible’ spectra work, (e.g. Chloride, Hydrocarbon, Colour or Permanganate), the long (40
mm) crystal glass cells should be used.
For UV work, the Quartz glass cells (10 mm) should be used. Quartz glass cells are invisible to UV
light, but they are very delicate and should be handled with great care. When using these cells the
clear sides should be exposed to the light path, and the cell should be placed at the far right hand
side of the cell holder.
Due to the unique light path and optical arrangements of this instrument, it is not necessary to
have a cell cover on this instrument.
The operation of this instrument is by simple file driven menus. Navigation through the screens
and methods is performed by pressing appropriate numerical keys and by the GREEN ‘accept’ or
the RED ‘cancel’ key.
Pressing the RED key also takes the user back one step/page or aborts the current operation.
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Running a Method
Once selected, the method screen will display the Method number and name, the wavelength and
units.
Pressing 0A/100%T (with the appropriate blank reference sample installed in the instrument) will
zero the instrument and the ‘sample’ box will show reference. During the scanning, a rapid ticking
noise is heard, this is normal.
Pressing GREEN (with the appropriate working sample installed in the instrument) will take a
measurement; the value obtained will be shown in the ‘concentration’ box.
If the instrument shows a value of ‘-----’ in the concentration box, it is because it has detected less
absorbance in the test sample compared to the reference sample. This does happen in some
circumstances.
Connection to a PC
The spectrophotometer has a built in USB communications port that can be used to connect to a
dedicated manufacturers’ printer, manufacturers Bluetooth device or to a PC, but it is pre-set to
communicate with a PC via the enclosed USB cable and software.
The instrument can be used for more sophisticated analytical determinations (UV scanning) and
the connection to a PC enables operators to send spectral data via email for evaluation. It will also
enable software updates to be uploaded remotely.
Equipment.
1. UV/Vis Spectrometer.
2. Laptop computer. (PVC Program installed).
3. 10 mm UV Quartz Cell.
4. Laboratory Grade Methanol.
5. Laboratory Grade D.I. Water
6. Box of Tissues.
7. Latex Gloves.
8. Samples.
Set up Instructions.
1. With both Spectrometer and Laptop in ‘Power Off’ mode, connect the
Spectrometer to the computer using the supplied USB cable.
2. ‘Power ON’ the Spectrometer. Allow the unit to perform its self calibration
checks. Once this is done,
3. ‘Power ON’ the connected computer. Once both systems are stable;
4. Click on the ‘PVC’ icon on your computer. The program will search and
find the Spectrometer (You will get a box stating ‘looking to see if Excel is
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present’ and a box screen will pop up entitled ‘PVC Application’. This will
show the product name ‘Lightwave11’, Serial Number (of the Spectrometer
you are connected to,) and ‘Activity’ – Connected.
5. The unit is now waiting for input.
UV Scanning.
14. Take the 10 mm Quartz Sample Cell. Note on the open top of one of the
clear panels, there is a ‘Q’ printed. When placing the cell in the cell holder
bracket in the Spectrometer, always have the ‘Q’ facing to the left.
15. Rinse the cell with Lab Grade Methanol, then rinse again with Lab Grade
D.I. Water.
16. Fill the 10 mm cell with D.I. Water. Carefully wipe the clear panels with
soft tissue to ensure they are absolutely clean and the cell is dry. (No
finger marks).
17. Place the cell carefully into the ‘right hand side’ of the cell holder. (There is
a holding lug to hold the cell securely in place).
18. The D.I. Water is used to calibrate the Spectrometer. So we need to use
the ‘BLUE’ calibration reference button. On pressing the BLUE button, the
unit will take this as reference, you will not see a readout.
19. Remove the Quartz cell from the unit. Rinse with pure Lab Grade
Methanol. Fill the cell with pure Lab Grade Methanol and make sure you
wipe and dry it with soft tissue.
20. Replace the methanol filled cell in the cell holder.
21. To read the result, press the GREEN button. You will see a line graph. If
the methanol is pure, without any contamination, you will see a smooth
curve to the left of the read-out panel. On your computer, you will see a
read out screen, recording the data.
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22. Create a folder on the desktop where you want to store the data and work
on the files.
23. On the PVC Application Screen, open the options screen by clicking on
the Icon next to the Connected unit.
Selection Box
The screen should be set up as you see above. However, you will need to
specify the location of the folder you have created to save your data.
This will open up the ‘Browse for Folder’ Box. You can either create your
new ‘Folder’ here, or just select the folder you have created previously in
which to store your files.
Select the folder and click OK on the ‘Browse For Folder’ Box.
Click OK on the ‘PVC Instrument Calibration Box.
The UV data will be automatically exported to the specified folder.
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25. Open the specified folder. Each time you press the GREEN button to scan
a sample, the excel data will be sent to this folder.
26. Exported files are automatically named:
“WAVE SCAN (Date and time).”
Rename the files as it goes into the folder, so it is easily identified later,
e.g. Tk 1P (Date/time).
Within the Folder you select to store your UV data files, Save the Excel File
‘Nordic Ship WW & UV Report’. This Excel Workbook file contains a
Worksheet for report on your Wall Wash Analysis. It also contains
Worksheets for tank by tank cumulative data storage and graph display.
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Each Graph line name (appearing on the Graph) can be renamed by right
clicking on the Graph Box.
Choose option ‘Select Data’.
To allow you to make effective comparison of your data, you can proceed
as follows;
1. Run a UV Scan on your ‘Blank’ Pure Lab Grade Methanol. Copy and
Past the Data from this sample as your first entry ‘Pure Methanol’. So
you will not need to rename this.
2. For your first Wall Wash sample, Copy and Paste your data to Columns
No. 2.
3. Rename the Graph line description by ‘Right Clicking’ on the graph
area.
4. In the ‘Select Data Box’, Select the line data you wish to rename and
click on ‘Edit’.
5. Enter the Series Name only. (Do not change the series values – unless
you know what you are doing!)
6. In the Series Name, enter the description for that line. (ie. 1P
18/04/12). Click OK
7. Click OK in the Data Source Box. The line will be renamed as
appropriate.
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By adding the progressive Data in this way, you will develop a Graph of your
Scans which can show a development as in the below Graph. This Graph will
show the development of your cleaning. IE. Your methanol wall wash is picking
up reduced amounts of contamination from the tank coatings.
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