Milestone 1.1 Identification and Definition of Geometries

Milestone 1.
1
Identification and Definition of
Geometries
1 Introduction
This project is being undertaken in order to provide the necessary expertise for the
establishment and commissioning of a radiological laboratory for the NNR. This
facility will serve as a verification laboratory for results reported by other
laboratories. The reports on this project are organised in terms of milestones.
The objective of this, the first report in Milestone 1.1, is to provide an overview of the
analytical procedures to be deployed in terms of the equipment and activities that are
necessary as well as the geometries of the measurements. This will produce a
landscape for the scope for the complete analytical requirements of the programme
outlined in Tables 2 and 3 of Attachment 1 of our proposal: Establishment and
Commissioning of a Radiological Laboratory. The details of the equipment and the
calibration methods will be addressed in the second report under this Milestone and
documentation for the calibration methods will be detailed in the third and final report
under this Milestone.
Various procedures including the specific methods will be provided in Milestone 1.2.
The final report, Milestone 1.3, will specify in detail the necessary activities for the
validation of the analytical methods and hence for the procedures.
In the development of the analytical methodology for the Verification Laboratory the
following terminology will be used. A procedure is a set of methods that will apply to
a particular type of sample and set of analytical requirements to provide a specific
result, or set of results. The idea is that when the manager receives a sample or a batch
of samples, the relevant procedure will be immediately available (to hand) and will
point to the particular methods and how they should be combined to produce the
desired results. The methods will be of different kinds: some will describe sample
preparation, some methods will be for dissolution, separation, counting, data
manipulation and also reporting. Thus each procedure will assemble a suite of
methods.
A total of 35 different procedures were identified by Mzesi in two tables in the

Attachment to the accepted proposal. Table 5 of the Attachment showed how these
procedures apply to the analytical requirements specified by the National Nuclear
Regulator (NNR) for the new Verification Laboratory. The procedures are specific to
the particular application as well as to the type of sample and the technique to be
applied.
It is envisaged that the number of samples will not be large but for a verification
laboratory the quality of the results must be excellent. The emphasis must be on the
quality of the data.
In the following sections the procedures are outlined in terms of the origins of the
samples, followed by the medium, the type of sample and the analytical technique.
The critical factors for each procedure that will determine its fitness for purpose are
the sensitivity, the accuracy and the precision. These must be evaluated in each case
and tested against the regulatory requirements. For each procedure the sensitivity is
crucial and the following table [ taken from the section on Validation (Milestone 1.3)]
acts as a guide in the establishment of the methods that constitute the different
procedures.
Table 1: Recommended minimum concentrations of radionuclides in individual

samples
[Maximum allowable??] CONCENTRATION

Specimen Type 60
Co, 137Cs, 90
Sr 3
H 131
I 238
U, 226Ra
134
Cs
Soil/Sediment/Sewage 15 [mBq/g] 20 [mBq/g]
Drinking water 1 [Bq/L] 0.5 [Bq/L] 10 [Bq/L] 20 [mBq/L]
Grass/Vegetation/Leafy 20 [mBq/kg] 20 [mBq/kg]

vegetable
Black mussels 20 [mBq/g]
Seawater 20 [mBq/g]
Surface water 20 [mBq/g]
Effluents 40[mBq/L] 5 [Bq/L] 0.2[Bq/L](1)
Milk 1 [Bq/L] 0.4[Bq/L]
KER-1 1 [Bq/L]
KER-2 40 [mBq/l] (1) 5 [Bq/l]
Fish 20 [mBq/g] 1 [Bq/kg]
[These values have been calculated by I. Petr on the basis of a maximum allowable
dose to a member of the public of 25 µSv per year from a single radionuclide in a
single source. I guess that they still have to be checked against the existing
regulations.]
2
2 Samples from Eskom – Koeberg operation
A number of different specimens will be received from Eskom in respect of the
operation of the Koeberg power station. In general these will be of a number of
different types and materials.
In this case there are specimens from a total of x different sources and a total of y
analytical procedures will be involved.
2.1 Biological Materials

There will be two kinds of biological materials in this suite, shell fish (black mussels)
and green leafy vegetables
2.2 Initial sample preparation

Sample preparation for all biological materials will involve the following initial steps.
After receipt and logging they will be dried and powdered. This will involve the use
of a fume hood and the possible need for filters to eliminate noxious or unpleasant
gasses.
2.2.1 Shell fish (black mussels)
It is expected that material may be received in either a raw or a pre-treated form. It is

recommended that the samples be received in an untreated form so that the chain of
analytical quality is completely under the control of the Verification Laboratory. In
this case it is expected that the sample size as received will be approximately 2 kg.
This will be dried and powdered. The powdered sample will be spread on a mixing
cloth and dip sampled into a suitable holder for further processing.
2.2.1.1 Gamma-ray spectroscopy
The most important analytical tool in this case will be gamma-ray spectroscopy. This
can be used to monitor the isotopes: Ce-144. I-131, Sb-125, Ru-103, Ba-140 (and La-
140), Cs-134, Cs-137, Zr-95, Mn-54 and Co-60, that may be present in the effluent
from a nuclear power station. The limits of detection will depend on the counting
geometry and the background, particularly the presence of NORM in the samples
themselves. Whether the sensitivity obtained is adequate for purpose will depend on
these factors as well as the actual sampling position and the model used to predict the
dispersion of the effluent in the environment. [In terms of Table 1]
The codes for the procedures that apply here are OfF1A and OfF1B
Sample preparation for gamma-ray spectroscopy
The dried and powdered sample will be mixed on a mixing sheet and dip sampled and
filled to a standard height in a suitable holder. This will be sealed and the mass of the
sample determined. In this case where the processed sample will be comparatively
small there are two options for the counting geometries.
3
The first one is to use a flat (”pill-box”) sample holder on a BEGe, high purity planar
detector. The second is to use a well-type HPGe detector, if available, with a “test-
tube” type of sample holder. The advantages and disadvantages of these two
approaches will be discussed under Milestone 1.2.
Methods for gamma-ray spectroscopy
Gamma-spectroscopy will be carried out according to detailed methods to be

described in Milestone 1.2. These will be part of the procedures coded under OfF1A
and OfF1B in Table 3 of Attachment 1 of the proposal.
Either a broad energy detector will be used with a flat sample holder or a well-type
detector will be used with a test-tube type of sample holder inside a suitable shield.
The details will be discussed in Milestone 1.2. [If the sample size could be of the
order of 500 g a Marinelli beaker sample holder could be used.]
The counting period will be of the order of 24 hours and the spectra will be processed
with standard software such as the Canberra software, Genie 2000. This will be
supplemented with additional software for reporting and quality control. In certain
cases, in a verification laboratory, it may be necessary to apply more advanced
methods, such as careful deconvolution, for the extraction of the intensities of
particular overlapping peaks in the gamma-ray spectra.
2.2.1.2 Other analytical methods
Although the Table of Specifications only provides for gamma-ray spectroscopy it

may be necessary to utilise other methods such as beta counting or alpha spectroscopy
for additional information on specific nuclides. [Elaborate]
2.2.2 Green leafy vegetables
Again it is expected that material may be received in either a raw or a pre-treated

form. It is again recommended that the samples be received in an untreated form so
that the chain of analytical quality is completely under the control of the Verification
Laboratory. In this case it is expected that the sample size as received will be
approximately 5 kg. This will be dried and powdered. spread on a mixing cloth and
dip sampled into a suitable holder
In this case as well the most important analytical tool will be gamma-ray
spectroscopy. This can be used to monitor the isotopes: Ce-144. I-131, Sb-125, Ru-
103, Ba-140 (and La-140), Cs-134, Cs-137, Zr-95, Mn-54 and Co-60, that may be
present in the effluent from a nuclear power station. The limits of detection will
depend on the counting geometry and the background, particularly the presence of
NORM in the samples themselves. Whether the sensitivity obtained is adequate for
purpose will depend on these factors as well as the actual sampling position and the
model used to predict the dispersion of the effluent in the environment.
The codes for the procedures that apply here are GrfF1A and GrfF1B.
4
The dried and powdered sample will be mixed on a mixing sheet and dip sampled to a
standard height in a suitable container. It will be sealed and its mass determined. In
this case where the processed sample will be comparatively small there are two
options for the counting geometries.
detector. The second is to use a well-type HPGe detector, if available, with a “test-
tube” type of sample holder. The advantages and disadvantages of these two
Method for gamma-ray spectroscopy

described in Milestone 1.2. These will be part of the procedures coded under GrfF1A
and GrfF1B as in Table 3 of Attachment 1 of the proposal.
The details will be discussed in Milestone 1.2. [Once again if sufficient sample is
available a Marinelli beaker will be considered]
with standard software such as the Canberra software, Genie 2000. This will be
supplemented with additional software for reporting and quality control.
Although the Table of specifications only provides for gamma-ray spectroscopy it

may be necessary to utilise other methods such as beta counting or alpha spectroscopy
following chemical treatment. For example it may well be necessary to check for
tritium. In this case the technique of liquid scintillation counting would be used. This
would require an additional procedure code.
2.3 Liquid samples

The liquid specimens received in respect of Koeberg operation will be of four types,
seawater, surface (fresh) water, milk and the actual discharged cooling water (KER).
In all cases it will be necessary to apply methods for the determination of nuclides
that can possibly be present in discharges from nuclear power stations. These include
a number of gamma-ray emitting nuclides such as Ce-144. I-131, Sb-125, Ru-103,
Ba-140 (and La-140), Cs-134, Cs-137, Zr-95, Mn-54, Co-58 and Co-60, but they will
also include Sr-89 and Sr-90 which are beta emitters as well as tritium. This last
isotope must be measured using liquid scintillation counting.
5
2.3.1 Initial sample preparation
It is envisaged that all the liquid samples may be received in either a raw or a pre-
treated form. It is recommended that the samples be received in an untreated form so
that the chain of analytical quality is completely under the control of the Verification
Laboratory.
Sample preparation for all these liquid samples will involve an initial concentration
step by evaporation. [I wonder if some chemistry is necessary before evaporation to
prevent loss of volatiles??]. After receipt and logging they will be treated and placed
in suitable containers under infra-red heat lamps to reduce the volume to
approximately 100 ml.
2.3.2 Sea water
Seawater contains a large amount of dissolved solids. In this case it is expected that
the sample size as received will be approximately 2 liters of sea water. After being
treated by using the initial sample preparation method to produce a sample size of 100
ml as described above, the sample will be further evaporated to dryness and
powdered.
Note that this is according to the requirements of the Table in the Attachment to our
Proposal (as obtained from the NNR). For gamma spectroscopy of these liquid
samples it may give better results if the entire liquid sample is counted in a different
geometry, using a large Marinelli beaker in a low background detector system.
In this case as well the most important analytical tool will be gamma-ray
spectroscopy. This technique can be used to monitor the isotopes: Ce-144, I-131, Sb-
125, Ru-103, Ba-140 (and La-140), Cs-134, Cs-137, Zr-95, Mn-54, Co-58 and Co-60,
that may be present in the effluent from a nuclear power station. The limits of
detection will depend on the counting geometry and the background, particularly the
presence of NORM in the samples themselves. Whether the sensitivity obtained is
adequate for purpose will depend on these factors as well as the actual sampling
position and the model used to predict the dispersion of the effluent in the
environment and therefore the effective population dose.
Of immediate importance is that it must be well below the maximum permissible

levels of these nuclides as specified in ????? [Table 1 above]
The codes for the procedures that apply here are SWaF1A and SWaF1B.
this case as well, where the processed sample will be comparatively small, there are
two options for the counting geometries.
6
detector. The second is to use a well-type HPGe detector, if this is available, with a
“test-tube” type of sample holder. The advantages and disadvantages of these two
For gamma spectroscopy of these liquid samples it may give better results if the entire
liquid sample is counted in a different geometry, using a large Marinelli beaker in a
low background detector system.

described in Milestone 1.2. These will be part of the procedures coded under
SWaF1A and SWaF1B in Table 3 of Attachment 1 of the proposal.
The details will be discussed in Milestone 1.2.
with standard software such as the Canberra software, Genie 2000. Details will be
described in the relevant methods in Milestone 1.2. This will be supplemented with
additional software for reporting and quality control.
Although the Table of Specifications only provides for gamma-ray spectroscopy for
these samples, it may be necessary to utilise other methods such as beta counting or
alpha spectroscopy following chemical treatment. For example it may well be
necessary to check for tritium. [What about C-14?] In this case the technique of liquid
scintillation counting would be used. The important nuclide, Sr-90 will be determined
by beta counting following chemical separation.
The development of additional procedures will be discussed in Milestone 1.2.
2.3.3 Surface (fresh) water
These samples will be obtained from various sources on and around the Koeberg site.
The amount of dissolved solids will be low. Again the sample size as received will be
approximately 2 l of water. After being treated by using the initial sample preparation
method to produce a sample size of 100 ml as described above, the sample will be
evaporated to dryness and powdered. [It is unlikely that we would obtain 10 g of solid
material from the evaporation of 2 l of fresh water. This would imply the
concentration of solids as 5 g per litre or 0.5% by mass.]
The most important analytical tool will be gamma-ray spectroscopy. This technique
140), Cs-134, Cs-137, Zr-95, Mn-54, Co-58 and Co-60, that may be present in the
effluent from a nuclear power station. The limits of detection will depend on the
7
counting geometry and the background, particularly the presence of NORM in the
samples themselves. Whether the sensitivity obtained is adequate for purpose will
depend on these factors as well as the actual sampling position and the model used to
predict the dispersion of the effluent in the environment.

levels of these nuclides as specified in ?????
The codes for the procedures that apply here are WaF1A and WaF1B.
this case as well, where the processed solid sample will be comparatively small, there
are two options for the counting geometries.

described in Milestone 1.2. These will be part of the procedures coded under WaF1A
and WaF1B in Table 3 of Attachment 1 of the proposal.
For the dried and powdered sample a broad energy detector will be used with a flat
sample holder or else a well-type detector will be used with a test-tube type of sample
holder inside a suitable shield, as discussed above. The details will be described in
Milestone 1.2.
8
2.3.4 Milk
These samples will be obtained from dairy farms in the vicinity of the Koeberg site.
The amount of dissolved solids will be low. Again the sample size as received will be
approximately 2 l of milk. After being treated by using the initial sample preparation
method to produce a sample size of 100 ml as described above, the sample will be
evaporated to dryness and powdered. [It is unlikely that we would obtain 10 g of solid
material from the evaporation of 2 l of milk. This would imply the concentration of
solids as 5 g per litre or 0.5% by mass. Actually it would probably be better to count
the entire sample in a large Marinelli beaker.
Arnaud has said that they reduce the volume to produce a kind of “porridge” and then
count that.
It must also be mentioned somewhere that all counting geometries for gamma-ray
spectroscopy should be calibrated with a standard source in the same geometry. Such
standard sources are not cheap, must be specially prepared by a specialist laboratory,
(for example by Eckert and Ziegler – allow six months) and do not last very long.]

levels of these nuclides as specified in ????? [Table 1]
The codes for the procedures that apply here are MiF1A and MiF1B.
this case as well, where the processed solid sample will be comparatively small, there
are two options for the counting geometries.
9

described in Milestone 1.2. These will be part of the procedures coded under MiF1A
and MiF1B in Table 3 of Attachment 1 of the proposal.
holder inside a suitable shield. The details will be discussed in Milestone 1.2.
2.3.5 Koeberg discharge (KER)
These samples are obtained directly from the cooling water discharge of the Koeberg
plant into the sea. Again the sample size as received will be approximately 2 l of
water. According to the stated requirements the initial sample preparation method will
be used to produce a sample size of 100 ml and this sample will be used in the
analytical methods outlined below. [Once more it should be noted that it may be
better to count the entire sample in a large Marinelli beaker.]

levels of these nuclides as specified in ?????
The codes for the procedures that apply here are KER1A and KER1B.
10
In one method the 100 ml sample obtained after the preliminary sample preparation
will be dried and powdered. This will be descanted onto a mixing sheet, mixed, dip
sampled and filled to a standard height in a suitable container. It will be sealed and its
mass determined. In this case as well, where the prepared solid sample will be
comparatively small, there are two options for the counting geometries in this case,
but see later.

described in Milestone 1.2. These will be part of the procedures coded under KER1A
and KER1B in Table 3 of Attachment 1 of the proposal.
holder inside a suitable shield. The details will be discussed in Milestone 1.2.
It may be advantageous to use the largest HPGe that can be obtained with the origonal
liquid sample (or one that is reduced in volume) in a (say) 2 l Marinelli beaker.
2.3.5.2 Beta spectroscopy
In the case of these discharge samples beta spectroscopy will be applied to the
samples in order to determine Sr-90 and Sr-89. This will require further sample
preparation as well as a gas-filled proportional counter. An alternative is to use
Cerenkov counting in a liquid scintillation counter
The procedure codes in this case are KER2A and KER2B depending on the sample
form received.
Sample preparation for beta spectroscopy
The 100 ml sample obtained after the preliminary sample preparation will be used
directly. Standard methods, to be described in Milestone 1.2, will be used to separate
strontium and to produce a sample suitable for introduction into the gas-flow
11
proportional counter [????]. Alternatively the liquid sample is mixed with a suitable
cocktail and counted in a liquid scintillation counter utilising the Cerenkov radiation.
Method for beta spectroscopy
The counting method will probably employ gas flow proportional counting. An
alternative method would be to use a liquid scintillation spectrometer to count the
Cerenkov radiation.
2.3.5.3 Tritium and C-14 using liquid scintillation
In order to measure the important isotopes H-3 (tritium) and C-14 it will be necessary
to use liquid scintillation counting. This will require a special instrument in the form
of a “Quantulus” liquid scintillation counter, or equivalent, together with personnel
with the necessary skills to operate it, to understand the analytical problems and to
obtain reliable results.
The procedure codes in this case are KER4A and KER4B depending on the sample
form received.
12

Milestone 1.1 Identification and Definition of Geometries

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Milestone 1.1 Identification and Definition of Geometries

Uploaded by

Copyright:

Available Formats

Milestone 1.

A total of 35 different procedures were identified by Mzesi in two tables in the

Table 1: Recommended minimum concentrations of radionuclides in individual

[Maximum allowable??] CONCENTRATION

Soil/Sediment/Sewage 15 [mBq/g] 20 [mBq/g]

Drinking water 1 [Bq/L] 0.5 [Bq/L] 10 [Bq/L] 20 [mBq/L]

Grass/Vegetation/Leafy 20 [mBq/kg] 20 [mBq/kg]

Black mussels 20 [mBq/g]

Surface water 20 [mBq/g]

Effluents 40[mBq/L] 5 [Bq/L] 0.2[Bq/L](1)

Milk 1 [Bq/L] 0.4[Bq/L]

KER-2 40 [mBq/l] (1) 5 [Bq/l]

Fish 20 [mBq/g] 1 [Bq/kg]

2.1 Biological Materials

2.2 Initial sample preparation

2.2.1 Shell fish (black mussels)

It is expected that material may be received in either a raw or a pre-treated form. It is

2.2.1.1 Gamma-ray spectroscopy

Sample preparation for gamma-ray spectroscopy

Methods for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.2.1.2 Other analytical methods

Although the Table of Specifications only provides for gamma-ray spectroscopy it

2.2.2 Green leafy vegetables

Again it is expected that material may be received in either a raw or a pre-treated

2.2.2.1 Gamma-ray spectroscopy

Method for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.2.2.2 Other analytical methods

Although the Table of specifications only provides for gamma-ray spectroscopy it

2.3 Liquid samples

2.3.2 Sea water

2.3.2.1 Gamma-ray spectroscopy

Of immediate importance is that it must be well below the maximum permissible

Sample preparation for gamma-ray spectroscopy

Method for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.3.2.2 Other analytical methods

The development of additional procedures will be discussed in Milestone 1.2.

2.3.3 Surface (fresh) water

2.3.3.1 Gamma-ray spectroscopy

Of immediate importance is that it must be well below the maximum permissible

Sample preparation for gamma-ray spectroscopy

Method for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.3.3.2 Other analytical methods

The development of additional procedures will be discussed in Milestone 1.2.

2.3.4.1 Gamma-ray spectroscopy

Of immediate importance is that it must be well below the maximum permissible

Sample preparation for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.3.4.2 Other analytical methods

The development of additional procedures will be discussed in Milestone 1.2.

2.3.5 Koeberg discharge (KER)

2.3.5.1 Gamma-ray spectroscopy

Of immediate importance is that it must be well below the maximum permissible

Method for gamma-ray spectroscopy

Gamma-spectroscopy will be carried out according to detailed methods to be

2.3.5.2 Beta spectroscopy

Sample preparation for beta spectroscopy

Method for beta spectroscopy

2.3.5.3 Tritium and C-14 using liquid scintillation

You might also like