NOORADILAH ABDULLAH Radiochemistry and Environment Group Waste and Environmental Technology Division Malaysian Nuclear Agency

1. Sampling, Pretreatment and
Preparation of Environmental
Samples
NOORADILAH ABDULLAH
Radiochemistry and Environment Group
Waste and Environmental Technology Division
Malaysian Nuclear Agency
The 4th Follow-up Training Course on Environmental Radioactivity
Monitoring in Malaysia
18 – 22 January 2016

2. Outline
• Introduction
▫ Sampling objectives
▫ Sampling location
▫ Example of monitoring in Japan
• Sample items
▫ Collecting methods & sample pretreatment
▫ Safety measures of collecting samples
• Conclusion

3. Introduction (1)
Sampling Objectives:
For proving the compliance of measured values with the established limits
For predicted values of radionuclide concentrations in environmental samples
To provide data on the levels, time dependence and spatial distribution of
radionuclides in air, soil, plants, foodstuffs and feedstuffs
To assess doses to critical groups of the population
To support decisions on mitigation and protective actions

4. Introduction (2)
To reduce the sample volume
To make uniform condition
To separate edible part in food
To preserve sample
Pre-treatment & Sample Preparation Objectives:

5. Introduction (3)
Sampling locations
Close to points where the
maximum exposure or
deposition is expected
Airborne discharges
preferentially in the main wind
direction
Aquatic discharges
downstream from the
release point
At the site boundary for
direct radiation from
the source
Should be conducted
regularly in nearby
population centers

6. Introduction (4)
Type of nuclear facilities
▫ Nuclear reactor facilities
▫ Reprocessing facilities
▫ Fuel fabrication facilities
▫ Fuel used facilities
▫ Radioisotope use facilities
▫ Radioactive waste disposal facilities

7. Example of monitoring in Japan (1/3)
Category Monitored
constituents
Frequency of
measurement
Sampling point Note
Local atmosphere condition
are well understood
Air
radiation
dose
Gamma dose rate Continuosly On the roof, on the ground NaI(Tl) detector on the roof
Integrated dose Quarterly Gas-monitor, dust monitor
Environmental
samples
Radioactivity
in
land
samples
Atmosphere (Dust) Continuously Avoid place directly
influenced building or trees.
Place the air intake of the
sampling device at least 1m
away from ground
Change the filter every week
River bed soil 2 times per year The river use for drinking
water or near the nuclear
facilities
Land water (River
water and water of
lakes)
2 times per year Collect at the center flow of
river/center of lake
Use for drinking water.
Do not collect sample if heavy
rain; caused cloudy.
Avoid mixing soil, sand or
sediment with the water
Drinking water 2 times per year Tab water near nuclear
facility within about 2 or 3
km

8. Example of monitoring in Japan (2/3)
Category Monitored
constituents
Frequency of
measurement
Sampling point Note
Local atmosphere condition are well
understood
Environmental
samples
Radioactivity
in
land
samples
Milk 2 times per year Near nuclear facility within about 2 or
3 km
131I Analysis
Soil 2 times per year Take into consideration local
geography; such as have little
vegetation, flat land, utilization of
land, etc.
Surface soil
Agricultural
products
Vegetables
Rice polishing
2 times per year
1 times per year
Near nuclear facility within about 2 or
3 km
Spinach, Chinese cabbage,
cabbage, edible roots, rice.
Purchased from farmhouse
Index plants Quarterly~1yr pine needle, etc
Fallout
Rain water
Dust
At the time of
rainfall (collecting
period 24hrs)
Monthly
Avoid place directly influenced
building or trees.
The height of the upper peripheral of
the received part should about 1m
above ground.
Funnel and bottle used to
collect rain water
Basin method
Sand at the
outlet drain
2 times per year collect the sample near the outlet
drain by trowels

9. Example of monitoring in Japan (3/3)
Category Monitored
constituents
Frequency of
measurement
Sampling point Note
Environmental
samples
Radioactivities
in
marine
samples
Sea water 4 times per year near the outlet drain of
nuclear facilities
Surface water
Sea soil 4 times per year near the outlet drain of
nuclear facilities(same points
of sea water)
collected by the instruments
in the sampling/monitoring
ship
Marine foods 2 times per year near the nuclear facilities Buy from market
Index plan Quarterly Buy from seaweed farm
Beach sand 2 times per year Near the nuclear facilities

11. Fig.1 Simplified pathways to man from radioactive materials released to atmosphere
Radioactive
materials
Air
Inhalation Resuspension Deposition
Soil
Animals Crops and Plants
Man
Direct
Radiation
Ingestion Ingestion
Direct
Radiation
11

12. Direct
radiation
Fig.2 Simplified pathways to man from radioactive materials released to ground or surface waters (including oceans)
Radioactive
materials
Surface or
Ground water Soil
Radioactive
materials
Ingestion Soil Irrigation water
Sand and
sediment
Land animals Land plants
Aquatic
animals
Aquatic
plants
Direct
radiation
Direct
radiation
Fishing and
Sports gear
Resuspension
and inhalation
Resuspension
and inhalation
Man
12

13. Sample Items
Type of
Sample
Dust
Water
Soil &
Sediment
Vegetation
& Farm
Products
Marine
Products

14. Dust
Sampling method
① Set the filter or both filter and activated charcoal cartridge in
the filter folder.
② Measure air flow rate at both the start and end of sampling, and
calculate the amount of sampling air (low volume air sampler
flow rate : 0.05-0.1 m3/min).
Sample pretreatment
• Gross β and Gross α
▫ Measure the filter direct by measuring instrument.
• Gamma emitter
▫ After measurement of gross β and gross α, put the filter into
polyethylene container and cover with plastic plate.

15. Dust Sampler
Filter paper,
HE40-T
Activated charcoal
cartridge, CP-20
Activated charcoal
cartridge, CHC-50
Flow rate meter
Filter folder
Activated charcoal
cartridge

16. Water Sample
• Fallout
• Rain
• River
• Lake
• Drinking water
• Seawater

17. Fallout (1)
Sampling method
① Pour the pure water into a basin
until 1 cm depth.
② Keep the water at 1 cm depth and
add water if the level is lower.
③ On the first day of every month,
let the total sample flow into the
collecting container. Rub off and
collect the attached dust on the
inner surface with a tool such as
a rubber spatula.
④ Rinse inner surface of the basin
with water. Add the rinse water
into the collecting container.
⑤ Measure the total volume or
weight of the collecting sample.
Sampling tools:
Stainless steel basin
receiving area : 5,000 cm2
(diameter : 80cm)
depth : 30 cm

18. Fallout (2)
Sampling pretreatment
Gamma emitter
① Pour the sample into ceramic
dish or glass beaker.
② Heat the dish or beaker on hot
plate to concentrate the sample.
③ Pour into small beaker and
concentrate more.
④ Pour the concentrated sample
into container for measurement
and heat by an infrared lamp.
⑤ After cooling, put the lid on
container.

19. Rain water (1)
Sampling method
① Collect the rain water
every day during
rainfall.
② In the case the
containing water is
possible to overflow for
a strong rain or other
causes, occasional
change of the bottle is
necessary.
 Sampling tools
 Funnel (Diameter : 252 mm)
 Bottle (Depth : 30 cm, Diameter: 20
cm)

20. Rain water (2)
Sampling pretreatment
Gross α and Gross β
① Measure the total sample volume by mess cylinder.
② In case of the sample volume is less than 100 mL, use all
volume samples. In case of the sample volume is more
than 100 mL, mix well and use 100 mL of sample.
③ Pour the sample into an evaporating dish and add few
drops nitric acid.
④ Concentrate the sample on the hot plate until volume
degrees 5-10 mL.
⑤ Put the measurement dish under infrared lamp, and drip
the concentrated sample in the evaporating dish drop by
drop by the pipette.

21. River water, water of lakes (1)
Sampling method
① Sample container is washed 3-4 times with water
from the site of sampling prior to taking sample.
② Sampling points is in the surface water layer
③ After sampling, add 1 mL of nitric acid or
hydrochloric acid per 1 L of water, except these
for analyzing 3H or measuring salinity. Check the
water temperature.
④ Sampling volume is about 2 L.

22. River water, water of lakes (2)
Sample pretreatment
Gamma emitter
① Pour the sample into ceramic dish or glass beaker.
② Heat the dish or beaker by gas banner or hot plate and
concentrate the sample.
③ When the sample volume is decrease, pour into small
beaker and more concentrate by an infrared
lamp/hotplate. Concentrate the sample until almost water
evaporates.
④ After cooling the sample, put the lid on container.

23. Drinking water (1)
Sampling method
① Before collect the water, discharge the water
for few minutes, and wash the bottle 3-4
times with drinking water.
② Collect the water directly from tap to bottle.
③ After sampling, add 1 mL of nitric acid or
hydrochloric acid per 1 L of water, except
these for analyzing 3H. Check the water
temperature.
④ Sampling volume is about 2 L.

24. Sea water (1)
Sampling method
① Collect the surface water in a bucket or directly
in container.
② Collected by means of suction pump installed in
the ship.
③ After sampling, add 1 mL of nitric acid or
hydrochloric acid per 1 L of sea water, except
these for analyzing 3H. Check the water
temperature and salinity. Check the latitude and
longitude of sampling points.

25. Co-precipitation technique for extraction
of Cs-137 from seawater
Cs in seawater
Fill tank with 200L seawater
Stir water with teflon rod
Add Cs tracer
Add 10 g Cu(II) nitrate
Add 10 g Potassium hexacyanoferrate(II)
trihydrate
Let precipitated for 24hrs
Transfer the precipitate into small
container

26. Co-precipitation technique for extraction of Pu,
Am and Cm from seawater
Pu, Am, Cm in seawater
Add Concentrated HCL
Add Pu and Am tracer. Rinse tracer bottle with seawater
Add 25 mL saturated KMnO4
Add 10M NaOH
pH 7 - 8
Add 1M MnCl2
Check pH
Let precipiated for 24 hrs
Transfer the precipitate into small container
Ensure pH<2
Let for 1hour
Yes
pH < 7
Add Concentrated HCl pH >8
pH 7 - 8
pH < 7
pH <7
pH not change
Use pH metre
Fill tank with 200L seawater
Stir water with teflon rod

27. Milk (1)
• Sampling method
▫ purchased from stockbreeder (volume:10 L)
▫ use the 10 L polyethylene container
• Sampling pretreatment
• Radioactive Iodine
① Add 10 mL of formalin per 1 L of milk.
② Pour the milk into 2 L mariner vessel and seal up the vessel.
 Gamma emitter
① Pour the 1 L of milk into the ceramic dish and evaporate in the
drier at 80-110oC.
② After dry up the milk, reduced to ashes in electric furnace at
450oC.
③ Grind ash and move the ash from ceramic dish to measurement
dish.

28. Vegetable (1)
• Sampling method
▫ purchased from farmhouse (Spinach, Chinese cabbage or Cabbage)
▫ sampling weight is about 10 kg
▫ use the polyethylene bag
• Radioactive Iodine
① Wash, make vegetable juice by a juicer.
② Pour the vegetable juice into 2 L mariner vessel. After seal up the
vessel, measure the sample weight.
• Gamma emitter
① Put the vegetable into the ceramic dish and dry in the drier at 80-
110oC.
② After dry up the vegetable, reduced to ashes in electric furnace at
450oC.
③ Grind ash and move the ash from ceramic dish to measurement dish.

29. Rice Polishing (1)
Sampling method
▫ purchased from farmhouse
▫ sampling weight is about 10 kg
▫ use the polyethylene bag
Temperature control in ashing
① It is necessary to control the tempt in the electric
furnace carefully
② Polished rice may be ignited if the temperature
gradient is too high
③ Three days heating by 450°C is necessary for
polished rice to be ashed well.

30. Soil (1)
• Sampling method
▫ collect samples from
the surface layer 0 to 5
cm deep with
polyethylene container
▫ sampling weight is
about 2 kg

31. Soil (2)
• Gamma emitter
① Move the soil sample from container to ceramic dish.
② Break the clod by spoon and remove the stones, grass and roots.
Dry in the drier at 105oC to prevent evaporation (in case of
iodine, at 70oC) and cool sample.
③ Break the clod and remove the small stones, roots of plant more
than 2 mm by 2 mm mesh sifter.
④ After sift the soil sample, put the sample into measurement
container and measure the sample weight.

32. River bed soil (1)
Sampling method
▫ takes the top 10 cm of river bed from both banks and center of
river
▫ sampling weight is about 2-3 kg
Grab sampler for surface sediment Core sampler for sediment in core

33. Beach sand (1)
Sampling method
▫ for each sampling point, take 3-5 samples from
the same area, and mix them well to form one
sample
▫ sampling weight is about 2-3 kg

34. Sea soil (1)
Sampling method
▫ collected by the instruments in the
sampling/monitoring ship

35. Marine products (1)
• Sample pretreatment
• Gamma emitter
① In case of fishes, separate fish the part of
edible meat, bones, skin, internal organs and
head. In case of shellfish, remove the shell. In
case of seaweeds, wash with fresh water.
② Dry the marine products at 105oC.
③ After dry up the sample, reduced to ashes in
electric furnace at 450oC.
④ Grind ash and move the ash from ceramic
dish to measurement dish.

36. !During pretreatment using temperature, it is
important to control the temperature not exceed
70oC for Iodine, while for Cs not exceed 650oC!

37. Safety measures during collecting the
sample
• Ocean
▫ Follow a captain’s instruction on the boat. Take safety measures
of boat, because the boat rolled and slipped on the deck of boat.
▫ Wear coverall, safety shoes.
▫ When go on board, put on a life jacket and inspect the equipment
of collecting sample.
• River, lakes and marshes
▫ Pay attention to the splinter of glass or river bed mud when enter
the river, lakes or marshes by walk.
▫ When collect the sample on the bridge, pay attention to the
walker and car.

38. Conclusion
• To make decisions on taking protective actions
in a particular area, average radiation levels
and/or activity concentrations in foodstuffs,
drinking water, crops and other relevant
materials should be determined.
• It should be confirmed that there has been
adequate monitoring for every important
radionuclide.

39. References
• International Atomic Energy Agency. Environmental
and Source Monitoring for Purposes of Radiation
Protection, IAEA Safety Guide No. RS-G-1.8, IAEA,
Vienna (2005)
• International Atomic Energy Agency. Measurement of
radionuclides in food and the environment, IAEA
Technical Reports Series No. 295, IAEA, Vienna
(1989)
• Junaya YAMADA. Lecture: Pretreatment of
Environmental Samples for Radiochemical Analysis.
The 61st Instructor Training Course (2015)
• Kenichi Matsuura. Lecture: Environmental
Radioactivity Monitoring. The 51st Instructor Training
Course (2013)