Important note




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Guidance document for the sampling of cereals for mycotoxins
IMPORTANT NOTE
This document is an evolving document which will be updated to take account of the experience gained with the application of this document or of new information provided.

I. Scope
To elaborate the document providing guidance for sampling lots where the sampling provisions as provided for in Regulation (EC) 401/2006 of 23 February 2006 laying down methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs are practically impossible to apply, such is the case where large lots of cereals are stored in warehouses or where cereals are stored in silos (see Annex I – B.3, last indent – footnote 1)
This means that that the current guidelines are not applicable to

 situations in which sampling provisions provided for in Regulation (EC) 2006/401 can be applied

 sampling of lots/batches in lorries, trucks, train wagons, …. (of reasonable size not exceeding 500 tonnes)
However, the provisions on the sampling equipment (in particular the number of incremental samples taken per sampling point) are also applicable to the situations covered by the provisions of Commission Regulation (EC) 401/2006.
Situations to be covered

- ships (for typical sizes see further)

* dynamic

* static

- lots in warehouses

* dynamic

* static

- silo's (in particular cylindrical silo's) (large – small)

* dynamic

* static


- bulk consignments in closed containers
This guidance document can also be used for the control of mycotoxins of other commodities, such as oilseeds and feed, in situations silar to those covered by this guidance document..
II. Sampling of large batches /lots – silo's
II.1 Starting points
*one sampling regime for the control of all mycotoxins

*one sampling regime for the control of all cereals


II.2. Number of incremental samples to be taken (for lots > 500 tonnes)
100 incremental samples + √metric tonnes , this means for a consignment of 10 000 tonnes: 200 incremental samples, 20 kg sample
II.3. Sampling equipment
There are many different types of sampling equipment or devices. The most suitable equipment should be chosen taken into account the product to be sample, the quantity required and the containers to be used.
Examples of equipment (non-exhaustive) to sample flowing grain and static lots are provided for in Annex to this document. The source of information for the examples of sampling equipment is EN-ISO 24333-2009.
II.4. Sampling equipment and incremental samples
When sampling with a sampling probe (sampling probe) with several apertures/openings, the cereals collected by a single aperture/opening can be considered as one incremental sample on the condition that in each aperture/opening the minimum quantity of incremental sample size is collected (100 g in the case of cereals, 200 g in the case of oilseeds). Also a maximum of 1 incremental sample per 0.5 m length of sampling probe can be accepted

These provisions on the sampling equipment are also applicable to the situations covered by the provisions of Commission Regulation (EC) 401/2006.


Examples:
Sampling probe of 2 m with 4 apertures/openings, collected quantity 100-150 g per aperture/opening = 4 incremental samples

Sampling probe of 6 m with 4 apertures/openings, collected quantity 250 g per aperture/opening = 4 incremental samples

Sampling probe of 3 m with 8 apertures/openings, collected quantity 100-150 g per aperture/opening = 6 incremental samples

Sampling probe of 2 m with 1 aperture/opening, collected quantity 200 g = 1 incremental sample.


Vacuum sampling probe of 9 meters length, sample taken over the complete length: 18 incremental samples

II.5 Sizes of bulk shipments and large batches in storage
Bulk shipments are transported in vessels – the size of the vessels can vary from 500 t to cape size vessels of more than 90.000 t. The holds also vary as depending on the constitution of the vessel itself.
Some examples of transport by ship:
- Panamax  for about 60.000 metric tonnes in 7 up to 9 holds

- Handy-Max for about 35/45.000 metric tonnes in 5 up to 7 holds

- Handy for about 15/25.000 metric tonnes in 3 to 5 holds

- Coaster for about 2/5.000 metric tonnes in 2 to 3 holds

- River barges for 500 up to about 2.500 metric tonnes in 1 to 2 holds.

 

Consequently one hold can be from 2 up to 10/12 meters deep.


Rice is generally imported in 20 ton containers: length 6,10 m, height 2,60 m, width 2,20 m (max 24t)

Storage:

Storage facilities (warehouses and silos) vary also, as they depend from the material they are destined to – there are differences of storage facilities between grains and flour because it depends from the flowing of the material stored.


- Flat-(horizontal) warehouses have a size of 15/20 meters x 40 or 60 or 80 meters length or even more and cereals are stored 4 meters ( but very often more) high.

- Vertical silos (metallic or concrete) can have storage capacity between 500 to 20.000 tonnes per cell with 4 to 50 cells in the same building and the height can go from 10 to 50 meters.


Rice

The size of the silo destined to rice can range hugely depending on the different companies i.e.  from 20 tonnes to 1000 tonnes.


II.6. General principles when sampling large batches
In case the way of transport or storage of a batch does not enable to take incremental samples across the whole batch, sampling of such batches should preferably be done when the product/batch is in flow or in case it is feasible, the lot to be sampled should be moved to another silo, … to enable sampling across the batch.
In the case of large warehouses destined to store grains, operators should be encouraged to install equipment in the warehouse enabling (automatic) sampling across the whole stored batch.
II.7. Sampling of batches transported by ship
II.7,1, Sampling of batches transported by ship by dynamic sampling
The sampling of large batches in ships is carried out while the cereals are preferably done in flow (dynamic sampling).
The sampling has to be done per hold (entity that can physically be separated). However to keep the balance of the ship, holds are emptied partly one after the other so that the initial physical separation does no longer exist after transfer into silo’s. So sampling can be performed in function of the initial physical separation or in function of the separation after transfer into storage.
The unloading of a ship of cereals can take several days: 50.000 tonnes with an unload capacity of 100 to 750 tonnes an hour can take 65 hours (3 days) to 500 hours (20 days).

Even if the sample is taken automatically, the presence of an inspector is necessary. Therefore it is not (always) feasible or appropriate (from resources and cost point of view) for an inspector to have to be present during the whole operation of unloading. Therefore sampling is allowed to be undertaken of part of the portion to be sampled and the result is considered representative for the whole portion to be sampled, on the condition that the quantity of the sampled part is at least 10 % of the portion to be sampled. If the operator questions the representativity of the sampling then the operator must enable at his cost to sample the whole batch.


Example
Portion to be sampled : batch of 10.000 tonnes

Unloading speed is 500 tonnes an hour: total unloading time = 20 hours

Inspector decides to sample only part of the batch (at least 10 %) . He decides to sample 1000 tonnes which means that the sampling time is 2 hours.
Possibility 1

The number of incremental samples is determined taking into account the size of the whole batch to be sampled.

The sample must consist of 200 (100 + √10000 = 200) incremental samples of 100 grams, resulting in a bulk sample of 20 kg.

This means that an incremental sample must be taken every 36 sec. or every 5 tonnes


Possibility 2

The number of incremental samples is determined taking into account the size of the sampled part of the whole batch. The weight of the aggregate sample has to be determined in function of the whole batch to be sampled.

The sample must consist of 132 (100 + √1000 = 132) incremental samples of 150 grams, resulting in a bulk sample of 20 kg.

This means that an incremental sample must be taken every 54 sec. or every 7.5 tonnes


II.7.2. Sampling f batches transported by ship by static sampling
In case the sampling is done in a static way the same procedure as foreseen for silo's accessible from above has to be applied (see point II.9.1) this means:
The minimum length of the sampling probe (sampling probe) to be used for the sampling o ships in a static way is 2 meter
There has to be a representative sampling of the accessible part (from above) of the consignment/hold performed and the result of such sampling is considered to be valid for the whole batch in the ship/hold
The analytical result of this sample is decisive to determine the compliance/non compliance of the whole batch/hold
In case of non-compliance, and in case representativity of such sampling is questioned by the operator  operator has the possibility to request to the authorities on his costs an official representative sampling of the whole consignment in the ship  involving a movement of the whole lot from the ship into a storage facility.
For examples see point II.8.

.

II.8. Sampling of large batches stored in warehouses


See point II.6
The minimum length of the sampling probe (sampling probe) to be used for the sampling of static batch/consignment stored in warehouse is 2 meter
There has to be a representative sampling of the accessible part of the consignment performed and the result of such sampling is considered to be valid for the whole batch
The analytical result of this sample is decisive to determine the compliance/non compliance of the whole batch

In case of non-compliance, and in case representativity of such sampling is questioned by the operator  operator has the possibility to request to the authorities on his costs an official representative sampling of the whole consignment stored in the warehouse  involving a movement of the whole static lot.


Example 1:
Cereals stored at warehouse 30 m large – 50 m deep – 4 m high = 6000 m³ = about 4500 tonnes accessible from 1 side (30 meter side)
Possibility to sample with sampling probe of 2m: 30 m x 2 m x 4m = 240 m³ = about 180 tonnes

100 + √4500 = 167 incremental samples of 100 grams – resulting in 16.7 kg sample – considered to be representative for the whole 4500 tonnes batch

(if the sampling probe has 4 apertures/openings: the batch has to be sampled at 42 sampling points representatively located along the accessible side)
Possibility to sample with sampling probe (with engine) of 5 meter long: 30 m x 5 m x 4 m = 600 m³ = about 450 tonnes

100 + √4500 = 167 incremental samples of 100 grams – resulting in 16.7 kg sample – considered to be representative for the whole 4500 tonnes batch

(if the sampling probe has 10 apertures/openings: the batch has to be sampled at 17 sampling points representatively located along the accessible side)


Example 2:
Cereals stored at warehouse 30 m large – 50 m deep – 4 m high = 6000 m³ = about 4500 tonnes accessible from 4 sides (160 meter side)
Possibility to sample with sampling probe of 2m: 160 m x 2 m x 4m = 960 m³ = about 720 tonnes

100 + √4500 = 167 incremental samples of 100 grams – resulting in 16.7 kg sample – considered to be representative for the whole 4500 tonnes batch

(if the sampling probe has 4 apertures/openings: the batch has to be sampled at 42 sampling points, representatively located along the 4 sides)
Possibility to sample with sampling probe (with engine) of 5 meter long: 160 m x 5 m x 4 m = 3200 m³ = about 2400 tonnes

100 + √4500 = 167 incremental samples of 100 grams – resulting in 16.7 kg sample – considered to be representative for the whole 4500 tonnes batch

(if the sampling probe has 10 apertures/openings: the batch has to be sampled at 17 sampling points, representatively located along the 4 sides)
II. 9. Sampling of silo’s
II. 9.1. Sampling of silo’s (easily) accessible from above
See point II.6
The minimum length of the sampling probe (sampling probe) to be used for the sampling of static batch/consignment stored in silo is 2 meter
There has to be a representative sampling of the accessible part of the consignment performed and the result of such sampling is considered to be valid for the whole batch
The analytical result of this sample is decisive to determine the compliance/non compliance of the whole batch

In case of non-compliance, and in case representativity of such sampling is questioned by the operator  operator has the possibility to request to the authorities on his costs an official representative sampling of the whole consignment stored in silo  involving a movement of the whole lot from one silo into another silo.


For examples see point II.8.
II. 9.2. Sampling of silo’s not accessible from above (closed cylindrical silo’s)
See point II.6
II. 9.2.1. Sampling of silo’s not accessible from above (closed cylindrical silo’s) with size >>100 tonnes
Cereals are stored in such silo’s cannot be sampled in a static way and therefore in case the cereals in the silo has to be sampled and there is no possibility to move the consignment, the agreement has to be made with the operator that he has to inform the inspector when the silo will be unloaded in order to enable sampling when cereals are in flow.
II. 9.2.2. Sampling of silo’s not accessible from above (closed cylindrical silo’s) with reasonable size
Sampling procedure involves the release into a recipient of a quantity of 50 to 100 kg and to take the sample in a representative way from this 50 -100 kg
Example for a silo of 25 tonnes:

Silo of 25 tonnes / 50 – 100 kg to be released in recipient / sample taken from this 50 – 100 kg // size of aggregate sample relates to whole consignment (25 tonnes)  means 10 kg sample – number of incremental samples relate to quantity released: means 5 incremental samples  5 incremental samples of 2 kg .


The analytical result of this sample is decisive to determine the compliance/non compliance of the whole batch

In case of non-compliance, and in case representativity of such sampling is questioned by the operator  operator has the possibility to request to the authorities on his costs an official representative sampling of the whole consignment stored in silo  involving a movement of the whole lot from one silo into another silo.


II.10 Sampling of bulk consignments in closed containers
Can only be sampled when unloaded. Is in many cases not possible at point of import and therefore in case such containers are to be sampled the sampling must take place during unloading at point of destination.

III. Annex
The Annex is provided as separate document


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