JAPAN P& I CLUBVol.44 February 2019

P&I Loss Prevention Bulletin
The Japan Ship Owners'Mutual Protection & Indemnity Association Loss Prevention and Ship Inspection Department

The Importance ofCargo Sampling

The Importance ofCargo Sampling
In virtually every dry and liquid bulk cargo, in many break bulk
and container cargoes, sampling is critical and it is becoming
increasingly important.

index
Why do we sample cargoes? ……………………1
Representative samples ……………………………1
Statistics ………………………………………………2
Sample preparation …………………………………10
Practical considerations …………………………12
Causation ……………………………………………15
Liquid cargoes ………………………………………15
Chain of Samples ……………………………………16
Dynamic sampling …………………………………16
Static sampling ………………………………………19
Independent petroleum inspectors
and retained samples ………………………………21
Sample handling ……………………………………22
Conclusions …………………………………………25
Case study 1 …………………………………………26
Case study 2 …………………………………………27
Case Study 3 …………………………………………28

JAPAN P& I CLUBWhy do we sample cargoes?
Cargoes, whether dry or liquid, are stored and transported in large quantities and it
is impractical and unrealistic to check every single portion of the cargo. Therefore, asmaller quantity is taken that has been shown to be statistically reliable estimate of theentire cargo. It is important to take a sample of a suﬃcient size, at a required frequency
and often at diﬀerent locations to properly represent the cargo quality. We will discuss
the basics of statistics later with some examples.
Sometimes but less often, samples are taken in order to determine the causation which
we will discuss brieﬂy later.

Representative samples
Representative sampling methods are used on a daily basis in the grain industry.
For example, the US Department of Agriculture has distinct grades for each of thecommodities commonly traded. Samples are taken “live” during the loading process andthe samples are usually taken from an automatic sampler prior to reaching loading bins.
Those samples are combined in various ways to assess such wide-ranging parameters
as odour, presence of insects and moisture content, but most critically they are used asa basis to assess the grade of the cargo. Grading parameters are commonly factors suchas broken kernels, foreign matter and test weight, and since the value of the cargo isdependent on the grade, it is critical that the sampling is conducted correctly.
Grading of agricultural commodities may or may not be involved during loading ofvessels, but almost certainly samples will be taken for contractual purposes between
buyer and seller. Depending on the commodity, this will be GAFTA (grain and feed)or FOSFA (seeds) sampling rules, which recently have aligned themselves. Both give
guidance on the sampling methods, frequencies and sample sizes. For example, GAFTA
no.124 stipulates a sliding scale of sampling frequency depending on the consignment
size. Please note this is the minimum frequency recommended:−1−

P&I Loss Prevention Bulletin
Table1: Increment sampling - size of lots, number and size of consignments

Consignment size
（Tonnes）

0-50005001 − 10,000

10001-25,000＞ 25,000

Lot size（Tonnes）

500

1,000

2,500

5,000

No.of increments perlot（number）

min 20min 30min 40min 50

Min bulk aggregate
sample per lot（Kilos）

20

30

40

50

Max weight ofincrements（Kilos）

1

1

1

1

From GAFTA Sampling Rules No.124 Rules for sampling, Analysis Instructions, Methods of Analysis andCertification.

Virtually all international bulk cargo shipments will be at least 25000 tonnes and thus
GAFTA stipulate the cargo is divided into lots of 5000 tonnes, each lot taking at least 50
individual samples and taking at least 50kg per lot but at most 1kg per sample.

Statistics
If only small quantities of samples are taken, then there is a higher margin of error.
For example, the allowable level of heat-damaged beans in soya from Brazil is 4%. If
we have a large quantity of, say, soya beans that deﬁnitely contains 4% heat damaged
beans and 100 beans are selected at random, the chances of ﬁnding exactly 4% damaged
beans are low. If, however, we take 1000 beans the probability of ﬁnding the actual level
increases:−2−

JAPAN P& I CLUBError margin

Error margin

1000 beans

Probability

100 beans

0

1

2

3

4

5

6

7

8

9 10... 0

1

2

3

4

5

6

7

8

9 10.

% of damaged beans found in the sample

The margin of error decreases dramatically the more beans we take. This is the reason
why as many samples as practically possible should be taken.
This example above is for a type of parameter that we call “non-continuous” variable.
It is non-continuous in the sense that a bean can be either heat-damaged or not heatdamaged. Other types of parameters are called “continuous” variables and will have arange of values. For example, the moisture content will differ in different parts of aniron ore ﬁnes stockpile, but it is unlikely that the cargo will be very wet and/or very dry.
Similarly, with parameters such as wet gluten in wheat samples - there will be a range ofvalues in diﬀerent parts of the cargo. Regardless of the type of variable, taking a higher
number of samples will reduce the margin of error.
These above examples envisage a relatively even distribution of the parameter in thecommodity but, in practical situations, there are factors at play by which cargoes canbecome heterogenous (i.e. uneven) with respect to a factor, and in these cases the
sampling method and sample handling are critical and need to be adjusted to suit their
purpose.
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P&I Loss Prevention Bulletin

Sampling methods
We mentioned earlier the GAFTA no.124 rules. In addition to
stipulating the sample frequency, they also specify the following
for bulk (for example) cargo samples:✔ Concurrently with loading✔ At the nearest practical point to the vessel✔ Throughout the consignment✔ Uniformly✔ Systematically✔ At loading or at discharge from a moving stream(if taken from a conveyor, vehicle or port storage)✔ At loading from quay or barge(if loaded by grab)✔ At discharge from various parts of the holdAll this is designed to create a reliable picture of the cargo condition throughout theconsignment. If sampling is conducted to this regime, it is usually a reliable regimen.
However, cargoes are not always homogeneous and certain factors are notorious for this,mycotoxins being the classic example. Mycotoxins are highly toxic chemicals producedby mould. They are not always produced by mould – they are a defence mechanismthat is intended to kill competing species. Some of these are also toxic to mammals andare strictly controlled nationally and internationally. For example, the most commonly
encountered family of mycotoxins, aﬂatoxins, have a maximum residue level of 15ppb
in some varieties of nuts intended for human consumption. The problem with aﬂatoxins−4−

JAPAN P& I CLUBis that they are only produced by moulds under specific circumstances and therefore
any aﬀected cargo tends to have a highly sporadic distribution of the toxin, but where
it is present, the levels will be very high. Such extreme unevenness has to be dealt withby adapting sampling methods (and sample handling, which we will discuss later). For
example, for a typical 60,000 tonne grain shipment, GAFTA would require the cargo be
split into 12 lots, each lot requiring 50 samples, so one sample every 100 tonnes:

Each lot = 250 trucks

60,000MT cargo = 12 lots●

60,000MT cargo = 12 lots●

5,000 MT lot with min.
50 incremental samples●

1 incremental samples
every 100 MT= about every 5 trucks

●

20 kg

A 20 kg sample representativeof 5,000 MT for each lot

1

2

3

4

5

6

7

8

9

10

11

12

1. Mixing
2. Splitting

3 kg

Aﬂatoxin sampling is typically more frequent and involves taking larger samples. For
example, Commission Regulation (EC) No 401/2006 of 23 February 2006 stipulates
500 tonne lots and taking 100g of sample every 5 tonnes to form 10kg samples. For a
60,000 tonne cargo that is a total of 12,000 incremental samples to form the 120 samples
for analysis. The whole point of this is to try to lower the margin of error as much as
possible.
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P&I Loss Prevention Bulletin

What is important for operatives in the marine industry is that the above examples
clearly demonstrate the importance of a sampling regime in cargo acceptance. We
have had cases in the past where entire shipments have been rejected for aflatoxin
contamination but on totally inappropriate sampling regimes. Some trivial sweat orwetting might result in mould growth and aﬂatoxin production in a small area, but theentirety of the lot must be taken into consideration.
Some cargoes are more predictably heterogeneous and sampling plans should take this
into consideration. For example, many Group A ❶ cargoes are typically formed into
conveniently-sized stockpiles and are stored outside sometimes for extended periods,
during which time the moisture will tend to drain. Samples taken from the upper surface
will tend to have a lower moisture content than the samples taken from the base of thestockpile, so it is essential that all levels are sampled and tested. A recent addition to the
IMSBC Code (section 4.4.8) states:“For unprocessed mineral ores, the sampling ofsection 4.4.8

stationary stockpiles shall be carried out only whenaccess to the full depth of the stockpile is available
and samples from the full depth can be extracted.”

We would recommend this is conducted on individual samples in any case from various
depths and regular points in nominated stockpiles to obtain a 3D map of each. This❶ Group A cargoes❶

Group A cargoes are those that are liable to liquefy. In order to be carried according to the
IMSBC Code, the lowest moisture content at which the cargo is considered to achieve a flow stateis measured on representative samples of the cargo in a laboratory. This is the Flow Moisture Point
or FMP from which the Transportable Moisture Limit (TML) is calculated (90% of FMP). The moisture
content of the cargo is also determined from samples – not necessarily the same samples. The
moisture content in each cargo space must be lower than the TML.

−6−

JAPAN P& I CLUBis important: if a stockpile is nominally acceptable in terms of moisture content on
average, the diﬀerence in moisture content can still be signiﬁcant from the upper part ofthe stockpile to the lower part. As such, there is potential for the wetter part to be loaded
in one cargo space which would be in contravention of section 4.3.5 of the IMSBC
Code:“When a concentrate or other cargo which may liquefy issection 4.3.5

to be loaded into more than one cargo space of a ship,
the certificate or the declaration of moisture content shallcertify the moisture content of each type of finely grainedmaterial loaded into each cargo space.”

If stockpiles have been properly mapped with respect to moisture content, this isstraightforward to calculate and load safe cargo. Shippers have been reluctant in the past
to go to these measures but it is often advantageous to them in that if the stockpile as awhole is not within the acceptable range, they might nominate not to load the wettest
part. IMSBC Code section 4.4.4 states:“Depending upon the results obtained in these tests, it may

section 4.4.8

be necessary to reject those particular portions as unsuitable
for shipment”.

Many stockyards use reclaimers which take layers from the surface of the stockpiles andit is straightforward to avoid any overmoist portions. The cargo is shipped and the Coderequirements are satisﬁed.

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P&I Loss Prevention Bulletin

Reclaimer loading iron ore from a stockpile

Following implementation of MSC.1/Circ.1454/Rev.1 of 15 June 2015 “Guidelines fordeveloping and approving procedures for sampling, testing and controlling the moisture
content for solid bulk cargoes which may liquefy” into IMSBC Code amendment 0315, which is now mandatory, shippers are required to establish sampling procedures
to ensure test samples are representative of the cargo to be shipped. The required
procedures need to incorporate provisions such as:−8−

JAPAN P& I CLUBSampling methods✔ Identifying the consignment to be sampled✔ Describing the method of sampling✔ Number of subsamples✔ Location of subsamples✔ Sampling equipment✔ Evidence of staﬀ training
This circular can be found in the 2016 Edition of the IMSBC Code on pages 561
to 566 and incorporates methods for analysis, guidelines for competent authority
implementation and moisture control in addition to the sampling. We would encourage
marine operatives from all involved parties to read and understand these sensible andcomprehensive requirements. All the above sampling information should be readily
available from shippers and we would recommend requesting it routinely in addition tothe other important documentation such as moisture content, FMP and the laboratory
worksheets.
We operate the same principles when sampling static grains because often quality and/or
condition will change in agricultural commodities with depth in a stockpile. We discuss
static sampling methods later.
One ﬁnal point in this section is regarding recent issues with partial sampling of cargoes.

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P&I Loss Prevention Bulletin
Occasionally, we encounter smaller but unusually high levels of bad quality cargo
portions incorporated into an otherwise normal bulk. When such cargo is loaded in ahold, it will naturally ﬂow into a layer shape on the stow surface. This is not easy to
distinguish during loading by looking at the cargo in a moving stream, especially withdust generated by loading. Also the layer of highly affected cargo might be coveredby a thin layer of normal cargo during a loading sequence which will totally obscure
it. During offloading, however, the grab or vacuvator cuts through the layers and thecontrast between the diﬀerent qualities is obvious. Often in these instances, receivers
will complain and segregate this darker layer as damaged cargo, sampling it duringoﬄoading and making a claim on any reduction in quality. However, the samples taken
at load port will have incorporated both relatively good and relatively bad portions
and the average is probably within speciﬁcation, so the heterogeneity in this instanceis not much of a problem in itself. Therefore, only sampling the “damaged” portionis ill-advised. While the “damaged” portion is more likely not to be in specification,
the remainder of the cargo is most likely to be well above specification and, if taken
as a whole – good and bad - is probably within speciﬁcation. Our advice is to sample
everything regardless of what segregation takes place. If the samples show that the cargo
is within speciﬁcation as a whole, it is disingenuous to claim for the worst part of it.
We have successfully pre-empted claims by not allowing consignees to sample only theworst portion of the cargo.

Sample preparation
Obtaining a sample is an important step but often the sample is enormous and toproperly prepare it for analysis is another critical and often overlooked step.
As highlighted earlier, there is a great deal of sample remaining following sampling
and it is usually impractical to post large quantities of samples to laboratories.
Typically samples have to be reduced in quantity in a sensible way that preserves the− 10 −JAPAN P& I CLUBcharacteristics of the material. For reasons
we will not go into in this article, following
typical transcontinental voyages we often see
the upper part of cargo stows more heavily
affected than lower parts. If sequential
samples have been taken during offloadingand placed in a large bag (as is the usual
Rifflermanner) this means the commodity in thelower part of the bag is probably worse than
the top part. If the sample is split, say, into 4
portions just by decanting the contents into
four separate bags then it is unlikely thatthese four samples will represent the samecargo.
Usually, therefore, methods are used toobviate any variations and the two techniques
commonly used are using a riﬄer or coning
and quartering. A riffler is a contraption,
typically metal, which has a series of chutesthat direct cargo to alternate sides. These
have been demonstrated to be effective inConing and quartering

splitting samples to a reasonable statisticalstandard. Other cargo splitters have diﬀerent designs but use the same principle, cutting
the sample stream in two and diverting it to split the sample.
If a riﬄer is not available, coning and quartering is another method shown to provide
satisfactorily even splits. The sample is poured from a height at the same location, so it
creates a cone, which is ﬂattened and split into quarters, each quarter forming a sample.
These can be further split if necessary.
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P&I Loss Prevention Bulletin

These methods are acceptable for the usual grading parameters in cargoes, but forfactors like mycotoxins, the sample preparation is even more critical. As discussed
previously, the sample sizes are large and need to be reduced, but given the extreme
heterogeneity of mycotoxin distribution, it is quite possible we obtain a situation where
one infected kernel is containing the entirety of the contamination. This might be within
speciﬁcation in the much larger sample but if that sample is split into 2 or 4 subsamples,the oﬀending kernel will only go into one of them and could render that sample oﬀ spec,
which is not a true reﬂection of the real situation. Because of this, the recommended
practice is to grind a large sample to make the particle sizes smaller and mix them. This
makes a sample split more representative of the actual concentration when the sample isanalysed.
Even if a cargo sample is taken correctly, if it is not processed correctly subsequently,
then spurious results can be obtained, and this has in the past resulted in mass rejections.
Marine operatives should ensure samples are being taken and processed properly
to obtain the true picture of the contamination level. We would recommend owners
and charterers pay special attention to this aspect because often local authorities will
reject cargo on sketchy evidence and it is worth requesting full disclosure of sample
preparation (in addition to the other sampling details and analysis).

Practical considerations
We hope the above gives some idea of the importance of sampling but also the sheer
effort involved in obtaining samples. Often, we are asked “take samples” half-way
through offloading or when offloading is nearing completion and there are many
obstacles to that.
Static cargoes, i.e. in warehouses, barges and silos are not straightforward to sample.

− 12 −JAPAN P& I CLUB
Spears are suitable for depths of up to 2m andwe also have a pneumatic sampler – basically apowerful armoured vacuum cleaner – capable ofsampling 6 m depths. Many sampling companies
worldwide will possess such apparatus.
If the stockpile is higher than 6m or stored in asilo, it is not sampleable by static methods andnormally we would suggest either stockpiles areconstructed to allow the normal methods to be
performed, or the silo contents are recirculated
or passed to an empty silo. This is timeconsuming and expensive in terms of manpower;
Sampling sorghum with Pneumac

it might also require the cargo custodian to rent
another warehouse/silo.

It is much easier to sample cargoes as they are moving and the GAFTA/USDA rules
envisage that system – it is relatively straightforward to sample from a moving stream.
Bagged cargoes are typically straightforward to sample if reasonable access is given inwarehouses to reach the required
stacks. Bags are typically stacked
on wooden pallets in warehouses
and pallets stacked atop each other,allowing access to a depth of cargo.
Samples are taken by a small spearthat can penetrate the bag weave
without damaging it too much.
Either way, people should be aware

Sampling soybeans with spear− 13 −

P&I Loss Prevention Bulletinof the physical reality of sampling.
The pneumac above weighs 24kg
and we typically double that when
taking a sample as the chamber
is filled. It is exhausting andrealistically is a 2-3 person task to
be done adequately. Most samplingneeds to be conducted aroundthe clock and for sampling to EU
Bag sampling

Mycotoxin requirements, this canonly be done by a team of people
taking shifts in order to keep up
with the speed of oﬄoading.
Sampling stockpiles of ore is
only possible if they are of areasonable size in accordance toCode stipulations as previously
discussed. Often, we are asked to250,000 tonne stockpile

sample enormous quantities whichis unreasonable and impossible. The
following was a 250000 tonne 12m
high cargo stockpile we were asked
to sample:
Sampling of ores can be conductedwith excavators and/or grabs but
if the cargo is not very cohesive,

Sampling nickel ore by excavatorthe “pits” need to be dug very
wide in order to get deep and this− 14 −JAPAN P& I CLUBtakes a great deal more time than is often
predicted.
Instructors of sampling companies need to
be aware of the time and the eﬀort required
to take samples and to ensure it is properly
funded with the appropriate manpower.
Sampling bauxite in ship’s hold by grab

Otherwise, these risk corners being cut.

Causation
Many operatives in the marine industry presume that the cause of damage of a given
commodity is determinable by sampling. In most spoilage cases this is a misconception.
In some instances, it can be useful to compare the properties of, say, an aﬀected sample
with the unaﬀected sample. The most commonly encountered instance of this is whenseawater ingress is suspected, and tests are conducted on samples to see if seawater ionsare present.

Liquid cargoes
Liquid cargoes are stored in tanks. Tanks can be static (i.e. shore tanks) or mobile (i.e.
ship tanks or other tanks associated with other modes of transport such as rail, road orair, when the liquid is to be conveyed). Liquid cargoes are transferred from one tankmedium to another via pipes and pumps. Pipes can be short, such as in a port when
the cargo is being transferred from a shore tank into a ship, or long, as when oil istransferred across countries or continents. Short pipes can be solid and ﬁxed or they
can be ﬂexible hoses. Pipes and tanks are often used to store or convey myriad typesof liquid; they are often not dedicated to any particular cargo. Ownership of the liquidcargo often changes at the point of transfer and sampling is necessary at the point at− 15 −

P&I Loss Prevention Bulletin
which custody handover takes eﬀect so that quality and conformance to speciﬁcation
can be veriﬁed.
Unlike solid bulk cargoes, there are more opportunities for liquid cargoes tobe contaminated and since liquid cargoes are typically much more sensitive tocontamination, the ramiﬁcations are more serious. Liquid cargoes can be contaminatedwhile in static storage or when being transferred from one storage tank to another via
pipes, by picking up contaminants from the pipelines or pumps. Contamination can be
due to pipes, pumps or tanks not being properly cleaned and prepared between diﬀering
cargo species. Cross contamination can also arise from pipes having valved branches toother adjacent pipes being improperly closed or secured.

Chain of Samples
In order to verify the condition of the cargo at any point in the transfer process, samples
need to be taken at all possible locations at each relevant point along the line: at theoriginating storage tank before; at suitable points in the pipeline during; and in thereceiving storage tank after the operation. This chain of samples from one location toanother will be necessary in order to pinpoint the location of contamination, if it occurs,
and, importantly, to help to apportion blame.

Dynamic sampling
Sampling can be static or dynamic. Static sampling is carried out from a body of liquidcontained within a tank either before the start or after the completion of the transfer
process. Dynamic sampling is carried out during the transfer process from the pipeline
between the two storage locations.
Automatic dynamic sampling is often carried out by in-line samplers during the transfer− 16 −JAPAN P& I CLUBprocess. Ideally they take ‘bites’ of sample at ﬂow proportioned intervals throughout theoperation. The stored sample is then mixed and divided to give a number of identical
portions. In-line sampling is usually used in bulk cargoes of crude oil when the static
liquid may not be homogeneous due to the presence of water and sediments. Automatic
in-line samplers usually oﬀer the best chance of getting properly representative samples
and they are therefore usually specified for this type of cargo. In-line samplers are
sophisticated and expensive items and they are usually owned by the exporting orimporting terminals and their operation is monitored by the independent petroleum
inspectors. Ship’s crews seldom have access to such equipment but should be aware of
it when in-line samples are presented to them as representing their cargoes.
The dynamic samples with which the crew should be more familiar are manifold
samples usually taken at the start of loading or of discharging. These can be from shoreor ship manifolds and are often used simply to verify the visual appearance of the cargoat that point in the line before valves are opened to allow it to flow on towards thereceiving tank, either ship on loading or shore on discharging.
Manifold samples at discharge, for example, are important to verify that the ship’s lines
and pumps are clean and free from water or other contaminants before cargo is released
to shore. In some trades, such as in chemical and parcel tankers, it may be considerednecessary to slop a small portion of cargo before it ﬂows clean. This is more often thecase with older ships which may have mild steel pipelines instead of stainless steel, or
when the last cargo may not have been completely removed from the ship’s lines.
Manifold samples at loading are similarly important to check that the cargo is as it is
supposed to be before it is allowed to ﬂow into the ship’s tanks. Manifold samples areusually taken unilaterally by the ship’s crew. They will be of limited evidential value,
however, unless they are properly registered, labelled and sealed, and preferably veriﬁedby an independent petroleum inspector.

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P&I Loss Prevention Bulletin

Manifold sampling

Manifold samples can be taken at the very start of loading or discharging, as suggested
above, or they can be taken at intervals as loading progresses. They might be taken,
for example, after the delivery tanks are changed over, in order to conﬁrm the ongoingcondition of the cargo. Ship’s manifolds, however, will often cause a “Venturi eﬀect” atthe sampling point such that there will be a suction into the sampling valve and no liquid
will be forthcoming. This eﬀect is most often caused during loading, when there is noback pressure at the manifold and a negative pressure is produced as the cargo drops
into the ship’s tanks. The eﬀect can also be produced by liquid ﬂow in the line passing
across the opening that is the sampling point. The eﬀect will cause outside air to be
drawn in to the opened sampling cock so that no liquid comes out and no sampling ispossible.
First foot sampling is often carried out with sensitive cargoes, as soon as the ﬁrst foot− 18 −JAPAN P& I CLUBor so (300mm) of cargo has arrived in the ship’s tanks. At that stage, loading may be
stopped while a sample is taken and analysed. A running ﬁrst foot may be taken without
stopping just to confirm visual appearance. First foots will confirm the cleanlinessand suitability of the ship’s pipelines and give the opportunity to stop loading and todischarge if contamination is found, before too much cargo is affected. First foots
taken in conjunction with manifold samples may help to identify where contamination
occurred. In the absence of a clean manifold sample, it may not be possible to knowwhether the cargo actually arrived on board clean.

Static sampling
Static samples are usually taken through the upper openings of a tank: through the roofof a shore tank or the deck openings of a ship’s tanks. They are usually comprisedof either running samples or zone samples. Since liquids are mobile, it is far morestraightforward to conduct reliable static sampling in them than in dry bulk cargoes.
Running samples are taken with the suitably weighed sampler, often a bottle with arestricted opening held in a cage, being lowered on a cord at a steady rate down throughthe liquid layer and then returned to the surface, again at a steady rate. The idea is to
get the sampler to be ﬁlling evenly all the way down and then all the way back up. The
sampler should not be full on completion, otherwise it cannot be known which portionof the liquid column has been represented and which has not. Running samples areusually used when it is thought that the liquid is reasonably homogeneous.
When the liquid cargo is not homogeneous, zone sampling may be considered more
appropriate. A zone sampler is capable of being lowered through the liquid column
to an appropriate height to capture a sample at that height. The captured sample fromthat zone is then recovered and transferred to a bottle. Zones can be at the top (near thesurface), upper (upper third), middle (central third), lower (lower third), bottom (dead− 19 −

P&I Loss Prevention Bulletinbottom) or at any increment in between. Intermediate increments may be tailored to suitspeciﬁc cargoes. For example, some fats and vegetable oils can become stratiﬁed withtemperature changes and may exist in quite diﬀerent forms at the various levels. They
can even be damaged at lower levels in contact with the heating elements if heated too
rapidly. Oil/water interfaces detected with water ﬁnding paste or electronic interface
detectors may be used in order to inform the levels at which zone samples are to betaken.
A dead bottom sampler (often called a thief) usually has a valve at the lower end which
is only opened when the device actually contacts the tank bottom, when it “steals” aliquid sample through the lower opening adjacent to the tank ﬂoor. Zone samplers havea device which allows them to be opened at any level or simple ﬂap valves which allow
ﬂow through them going down but close to hold a sample going up.

Zone samples will often be proportionally blended in order to make up a compositeof that tank. For example, a composite may be comprised of upper, middle and lower

Zone sampler− 20 −JAPAN P& I CLUBzones (U/M/L). However, bottom samples areusually kept out of a composite so as not todisproportionally represent the bottom (which
may contain a lot of water in less dense liquids)
in the finished sample. Bottom samples are
considered to be for information purposes: theycannot be proportionally representative of theliquid existing higher up in the tank.

Dead bottom sampler

Zone samples mixed from different incremental heights within a liquid column willneed to be proportioned according to the volume that they represent. For example, in a
vertical cylindrical or square tank the proportions will be the same at each vertical zone.
However, in a horizontally cylindrical or spherical tank, the central zones will represent
a larger proportion of the total volume than the upper and lower zones.

Independent petroleum inspectors and retained samples
Most custody transfers (ship loading and discharging operations) in the petroleum
industry are monitored and documented by accredited independent petroleum inspectors.
The inspectors are generally appointed jointly by buyers and sellers of the cargo, one
party is often the charterer. These inspectors will therefore act for cargo interests but
being independent ought to act in the best interests of all parties, including the ship.
A ship’s crew should be encouraged to cooperate with the independent inspectors but
should also recognise that, as they act for cargo interests: in the event of there being a
potential problem, a surveyor should also be appointed through the ship’s P&I Club.
The ship’s crew should ensure that the independent inspectors take proper and adequate− 21 −

P&I Loss Prevention Bulletinsamples, and that these are sealed, labelled, receipted and distributed in accordance withnormal procedures. The crew should ensure, for example, that duplicate sets of sealed
samples, properly receipted, are retained on board for future reference.
Retained samples should be logged into the ship’s own system and recorded inaccordance with the SMS procedures. Samples retained on board should be housed inapproved sample lockers where they can be kept dry, protected from sunlight, excessive
heat and mechanical damage. They should be retained as long as necessary, usually
until some months after the respective cargo has been discharged without comment, andthen destroyed. A ship should avoid retaining old and irrelevant samples in the lockers.
This just causes unnecessary clutter and confusion with current samples.

Sample handling
Regardless of whether the sample is a liquid or dry commodity, once the sample has
been taken and processed, it will be sent or retained for analysis and therefore it isimportant to identify it properly. Labels stuck to the outside of samples often will go
missing or become unreadable. We tend to double-bag all samples with clear polythenebags, with the label visible between inner and outer bag.
Sealing the sample with numbered seals is also recommended so there is less chanceof interference. Many seals are available, but a higher security is obtained from using
tamper-evident seals which show obvious signs of tampering if they are attempted to bereused.
Seals should be deployed properly and used to seal the actual sample. We have seen
seals used around the neck of bottles – it would be a simple matter for devious workers
to replace contents with that arrangement:− 22 −JAPAN P& I CLUBThe label information is also critical. We recommend as a minimum:

The label information
Ship/facility name
Date
Goods
(e.g. wheat)

Description(e.g. apparently sound)

Place (port/city)
Quantity
Whether bulk/bag
Sampler name and company
Sampling method
Identiﬁcation mark(usually seal number)

Origin of cargo
Location of sampling(e.g. holds, truck, conveyor)

Using good quality ink that lasts at least
several years is recommended.

The label information− 23 −

P&I Loss Prevention Bulletin

Seal around bottle neck

We also take close-up photographs of the samples including close-up photographs ofthe seals and sealing arrangements. We have heard of unscrupulous parties 3-D printing
new seals but when compared in detail with the originals, the structure is difficult toreplicate in the necessary detail so clear detailed photographs can be useful to address
such behaviour.
As part of the evidence trail we would also suggest taking time and date-stamped
photographs of the samples with the new custodian whether that is a courier, a lab or
surveyors so that evidence of sample location is retained.
Finally, samples should be stored in a clean, cool environment and checked on fromtime to time. Some samples need to be kept for 90 days or more as part of typicalcontractual agreements. We have in the past encountered samples totally destroyed byrats because the samples were stored in inadequate conditions.

− 24 −

Conclusions
1.

Sampling of cargoes appropriately and comprehensively can prevent
spurious claims or limit claims to realistic levels.

2.

In some instances, for example Group A cargoes, proper sampling is
critical for ship and crew safety.

3.

Sampling is a time-consuming and exhausting undertaking andmarine industry operatives should be aware of the eﬀorts involved
and adequately prepare for this.

4.

All parties in the marine industry should be aware of the
responsibility of creating statistically valid samples and relevant
parties should be willing to demonstrate their veracity withsupporting evidence.

P&I Loss Prevention Bulletin

Case study 1
A product tanker arrived at
Barcelona wi th 30,000 tons of jet
fuel to discharge. The arrival ullage
survey, with water dips, showed
there to be various amounts of freewater in most of the ship’s tanks.
Samples taken at upper middle
and lower levels showed that thecargo was on specification but thedead bottom samples revealed
mostly water. Analysis of thesesamples showed a water that wasneither fresh nor characteristicallysea water: the sodium/chloride
balance was not typical of sea
water. Further investigation showedthat the water was most likely to berefinery water and therefore fromthe loading port terminal.

quality with no significant free water.
The ship’s lines were stripped empty
to remove the water and discharge
was commenced.
At commencement of discharge theship’s manifold samples showed nosignificant water and the cargo was
accepted without further comment.
The quantity of de-bottomed
material drawn off was later
discharged separately. No claim
was made against the ship as thewater was demonstrably not of shipboard origin.
Effective sampling was the key tominimising loss in this case with asuccessful outcome for the ship.

With the cooperation of cargointerests, each cargo tank was debottomed to a slop tank on board.
Suction was briefly made with thepumps from each tank in turn until
all traces of free water had been
removed. During this operation
the ship’s ballast tank contents
was adjusted to give a list and trim
which allowed for the most effective
suction from each tank in turn.
After de-bottoming, the cargo in thetanks was found to be of acceptable− 26 −JAPAN P& I CLUBCase study 2
A product tanker arrived at Djiboutit o d i s c h a rg e s e p a r a t e p a rc e l sof jet fuel, gasoline and diesel,
all loaded at Jeddah. Sampling
prior to discharge showed that
one of the two jet fuel tanks wasoff specification on flash point.
Sampling and analysis showed thatthe tank had been contaminated withgasoline.
Investigation showed that thecontaminated tank had been the firstto receive jet fuel. The jet fuel was
loaded after gasoline through thesame ship’s manifold and bottom
line system. It was considered
likely that the single tank had been
contaminated by gasoline remaining
in the ship’s lines after that grade
had been loaded first. The line was
supposed to have been stripped dry
between grades but the arrangementof the line showed that this wasprobably not possible due to the line
having an undrainable belly.
No first foot samples of the jet fuelhad been taken and no analysis
had been carried out of the after
loading samples at the loading
port. However, sealed after loading
samples were carried by the ship tothe discharge port. These included
individual ship tank samples, being
the composites of upper, middle andlower samples taken after loading.
Analysis of the after loading sample
from the contaminated tank showedthat the contamination was alreadypresent after loading.
Discharge of the uncontaminatedtank of jet fuel went ahead at
Djibouti. However, the contaminatedtank of jet fuel was retained on
board, for later disposal elsewhere.
In this way the flash point
contamination was contained within
the ship. Had discharge of all the jet
fuel gone ahead in Djibouti, all the jet
fuel would have been contaminatedand the low flash point material
would also have soiled the receiving
shore terminal’s dedicated storage
facilities.
Proper sampling carried out at thedischarge port allowed the damage
to be restricted to just one of the twojet fuel tanks on board. However,a lack of proper sampling at theloading port had allowed the cargo
to be loaded with one of two tanks
being off specification, without thisfact being identified at the time.

− 27 −

P&I Loss Prevention Bulletin

Case study 3
A bulk cargo of maize was delivered
to receivers in Yemen. Heat leakage
from settling tanks in way of holdno.5 aft bulkhead was insufficient todamage the maize, but it did initiatemould growth on the cargo surface
in the vicinity of the aft bulkhead.
Samples taken by authorities in thisarea were found to have aflatoxins
above the required level and thecargo was rejected.

Receivers were encouraged to takesamples of the cargo according tointernational standard frequencies,
also incorporated into Yemeni
regulations. The new samples weremore representative of the cargo
and were all in specification, andthe authorities allowed offloading tocommence.

− 28 −JAPAN P& I CLUBMEMO

− 29 −

P&I Loss Prevention BulletinWith Collaboration from Brookes Bell
Brookes Bell House
13 Pak Kong Au Village
Sai Kung
New Territories
Hong Kong SAR
T:+852 2358 4794
www.brookesbell.com

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