INTERNATIONAL STANDARD ISO 18589-2 Second edition 2015-02-01 Measurement of radioactivity in the environment — Soil — Part 2: Guidance for the selection of the sampling strategy, sampling and pretreatment of samples Mesurage de la radioactivité dans l’environnement — Sol — Partie 2: Lignes directrices pour la sélection de la stratégie d’échantillonnage, l’échantillonnage et le prétraitement des échantillons Reference number ISO 18589-2:2015(E) © ISO 2015 ISO 18589-2:2015(E) COPYRIGHT PROTECTED DOCUMENT © ISO 2015 All rights reserved Unless otherwise specified, no part o f this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission Permission can be requested from either ISO at the address below or ISO’s member body in the country o f the requester ISO copyright o ffice Case postale 56 • CH-1211 Geneva 20 Tel + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyright@iso.org Web www.iso.org Published in Switzerland ii © ISO 2015 – All rights reserved ISO 18589-2:2015(E) Page Contents Foreword v Introduction vi Scope Normative references Terms, definitions, and symbols Principle Sampling strategy 5.1 5.2 5 Typ es o 6.1 6.3 6.4 7.1 7.2 General f 6.2.1 General f f 6.2.4 Selection criteria of sampling areas and sampling units f f S electio n o 6.2 S amp ling o r us e with a p ro b ab ilis tic s trategy 6.2 S amp ling o r us e with an o rientated s trategy I dentificatio n o S electio n o s amp ling areas , units , and p o ints field equip ment 7.5 8.1 8.3 Principle 15 15 Procedure 15 9.1 General 16 f 16 f 17 7.2 S electio n o 7.2 S amp ling s o il p ro file s amp ling dep th vers us o b j ectives o I dentificatio n and p ackaging o the s tudy s amp les S amp le identificatio n Pre-treatment of samples 15 8.2 Lab o rato ry equip ment Determination of the activity deposited onto the soil 16 9.2 9.3 10 s amp ling areas , units , and p o ints General Collection of samples f f 7.2.2 Sampling surface soil 11 11 Preparation of the sorted sample 13 f 13 7.4.1 General 13 13 7.4.3 Sample sheet 13 Transport and storage of samples 14 7.4 the s amp ling s trategy Sampling process 7.3 s amp ling s trategies S electio n o Sampling plan 6.2 General Initial investigation f f D eterminatio n us ing s ur ace activity data D eterminatio n by integratio n o s o il p ro file activity data Recorded information 17 (informative) Annex A Diagram of the selection of the sampling strategy according to the objectives and the radiological characterization o f the site and sampling areas 18 (informative) Annex B Diagram of the evolution of the sample characteristics from the sampling site to the laboratory 19 (informative) Annex C Example of sampling plan for a site divided in three sampling areas (A, B, C) 20 Annex D (informative) Example of a sampling record for a single/composite sample 21 © ISO 2015 – All rights reserved iii ISO 18589-2:2015(E) Annex E B i iv b l i o g (informative) r a p h y 22 24 E x a m p l e f o r a s a m p l e r e c o r d f o r a s o i l p r o f i l e w i t h s o i l d e s c r i p t i o n © ISO 2015 – All rights reserved ISO 18589-2:2015(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation o f national standards bodies (ISO member bodies) The work o f preparing International Standards is normally carried out through ISO technical committees Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f electrotechnical standardization The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part In particular the di fferent approval criteria needed for the di fferent types o f ISO documents should be noted This document was dra fted in accordance with the editorial rules o f the ISO/IEC Directives, Part (see www.iso.org/directives) Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f patent rights ISO shall not be held responsible for identi fying any or all such patent rights Details o f any patent rights identified during the development o f the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents) Any trade name used in this document is in formation given for the convenience o f users and does not constitute an endorsement For an explanation on the meaning o f ISO specific terms and expressions related to formity assessment, as well as in formation about ISO’s adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the following URL: Foreword — Supplementary in formation The committee responsible for this document is ISO/TC 85, Nuclear energy, nuclear technologies, and radiological protection , Subcommittee SC 2, Radiological protection This second edition cancels and replaces the first edition ( ISO 18589-2 :2007), which has been technically revised ISO 18589 consists o f the following parts, under the general title Measurement of radioactivity in the environment — Soil: — Part 1: General guidelines and definitions — Part 2: Guidance for the selection of the sampling strategy, sampling and pre-treatment of samples — Part 3: Test method for gamma-emitting radionuclides using gamma ray spectrometry — Part 4: Measurement ofplutonium isotopes (plutonium 238 and plutonium 239+240) by alpha spectrometry — Part 5: Measurement of strontium 90 — Part 6: Measurement of gross alpha and gross beta activities — Part 7: In situ measurement of gamma-emitting radionuclides © ISO 2015 – All rights reserved v ISO 18589-2:2015(E) Introduction This International Standard is published in several parts to be used jointly or separately according to needs ISO 18589-1 to ISO 18589-6 concerning the measurements o f radioactivity in the soil, have been prepared simultaneously These parts are complementary and are addressed to those responsible for determining the radioactivity present in soils The first two parts are general in nature ISO 18589-3 to ISO 18589-5 deal with radionuclide-specific measurements and ISO 18589-6 deals with non-specific measurements of gross alpha or gross beta activities ISO 18589-7 deals with the measurement of gamma emitters radionuclides using in situ spectrometry Additional parts can be added to ISO 18589 in the future i f the standardization o f the measurement o f other radionuclides becomes necessary vi © ISO 2015 – All rights reserved INTERNATIONAL STANDARD ISO 18589-2:2015(E) Measurement of radioactivity in the environment — Soil — Part 2: Guidance for the selection of the sampling strategy, sampling and pre-treatment of samples Scope T h i s p ar t o f I S O 8 s p e c i fie s the genera l re qui rements , b as e d on I S O 110 74 a nd I S O/I E C 1702 , for a l l s tep s i n the pl an n i ng (de s k s tudy a nd are a re na i s s ance) o f the s ampl i ng and the prep aration o f s a mple s for te s ti ng I t i nclude s the s ele c tion o f the s ampl i ng s trateg y, the outl i ne o f the s a mpl i ng pl an, the pre s entation o f genera l s a mp l i ng me tho d s and e quipment, a s wel l as the me tho dolo g y o f the pre tre atment o f s a mple s adap te d to the me as u rements o f the ac tivity o f rad ionucl ide s i n s oi l T h i s p a r t o f I S O 8 i s add re s s e d to the p e ople re s p on s ib le i n s oi l for for de term i n i ng the rad io ac tivity pre s ent the pu rp o s e o f rad iation pro te c tion I t i s appl ic able to s oi l from ga rden s , farm land, u rb a n, or i ndu s tria l s ite s , a s wel l a s s oi l no t a ffe c te d by huma n ac tivitie s This part of ISO 18589 is applicable to all laboratories regardless of the number of personnel or the range of f f part of ISO 18589 the tes ting per ormed When a laborator y does not undertake one or more o the activities covered by this , s uch as planning, s ampling, or tes ting, the corres ponding requirements not apply Normative references T he fol lowi ng i nd i s p en s able c u ments , i n whole or i n p ar t, are normatively re ference d i n th i s c u ment a nd are for its appl ic ation For date d re ference s , on ly the e d ition cite d appl ie s For u ndate d re ference s , the late s t e d ition o f the re ference d c u ment (i nclud i ng any amend ments) appl ie s I S O 1-9, Quantities and units — Part 9: Atomic and nuclear physics I S O 110 74, Soil quality — Vocabulary I S O/I E C 1702 , General requirements for the competence of testing and calibration laboratories ISO 18589-1 Measurement of radioactivity in the environment — Soil — Part : General guidelines and definitions , Terms, definitions, and symbols For the pu rp o s e s o f th i s c ument, the term s , defi n ition s , and s ymb ol s given i n I S O 1-9, I S O 8 -1 , I S O 110 74, and the e fol lowi ng apply th ickne s s o f the layer s a mple d m′ss wet mass of the sorted sample wet mass of a subsample of the sorted sample m ts d r y ma s s o f the te s t s ample a ac tivity p er u n it o f mas s o f the te s t s ample AS ac tivity p er u n it are a m ss © ISO 2015 – All rights reserved ISO 18589-2:2015(E) S surface area sampled Principle The purpose o f the measurement o f soil radioactivity is to monitor the environmental impact o f radioactive substances[1] and/or to assess the radiological impact on the population [2 ] ,[3 ] ,[4] ,[5] The main objectives of the measurement of radionuclides in soil (see ISO 18589-1) are the following: — characterization o f radioactivity in the environment; — routine surveillance o f the impact o f radioactivity released from nuclear installations or o f the general evolution o f the radioactivity in a region; — investigations o f accidents and incidents; — planning and surveillance o f remedial action; — decommissioning of installations or the disposal of materials Consequently, measurements o f soil radioactivity are per formed in a variety o f situations, but a generic approach can be described, with the following steps as outlined in this part o f ISO 18589: a) Planning process — Selection o f the sampling strategy The selection o f the sampling strategy depends on the main objectives and on the results o f the initial investigation o f the area The sampling strategy shall lead to the knowledge o f the nature, activity concentrations, spatial distribution, as well as temporal evolution o f the radionuclides, taking into account changes caused by migration, atmospheric conditions, and land/soil use An initial investigation o f the area shall be carried out to determine the sampling strategy ISO 10381-1[6] gives general guidance on the selection of the sampling strategy; ISO 10381-4[7] gives specific guidance for the investigation o f natural, near-natural, and cultivated areas; and ISO 10381-5[8] deals with the investigation of soil contamination at urban and industrial sites Details are given in Clause and a scheme for the selection of the sampling strategy is given in Annex A b) Planning process — Sampling plan The sampling plan shall be developed according to the sampling strategy selected It shall speci fy the selection o f sampling areas and units, the sampling pattern, the sampling points, the types o f samples, the sampling procedures and equipment, as well as the sa fety requirements for the personnel Details, such as the selection o f sampling areas and the sampling units that result from the type o f grid applied to these areas, are given in Clause Definitions o f the types o f sample are given in ISO 18589-1 The relationship between sample types is given in Annex B c) Sampling process — Collection of samples The collection o f any soil samples in the field shall form to the established sampling plan — For sampling o f the top layer, a single sample or n increments o f a defined thickness are taken from each of the selected sampling units — For vertical sampling o f several soil layers, samples are taken at increasing depth vertically below the surface sampling point A single sample or n increments are collected from the various soil layers with di fferent thicknesses according to the sampling depth Special care should be exercised in order not to mix samples from di fferent soil layers Details are given in Clauses and © ISO 2015 – All rights reserved ISO 18589-2:2015(E) d) Sampling process — Preparation of the sorted sample The preparation of sorted samples is carried out by the reduction of single or composite samples A sorted sample should be representative of the average value of one or more given soil characteristics The identification, labelling, packaging, and transport procedures o f sorted samples to the laboratory shall guarantee the preservation of their characteristics Details are given in 7.3 , 7.4, and 7.5 e) Laboratory process — Handling o f the laboratory sample A fter arrival at the laboratory, the sorted samples are considered as laboratory samples for storage and further pre-treatment be fore their analysis Details are given in Clause f ) Laboratory process — Preparation o f the test sample Be fore any testing, the laboratory samples are pre-treated by drying, crushing, sieving, and homogenizing to produce test samples in the form o f a fine, homogeneous powder Pre-treatment shall guarantee that the physical and chemical characteristics o f the test sample are constant over time, thus rendering the results easier to interpret Representative subsamples with masses determined by the specifications o f the di fferent radioactivity measurements shall be isolated from the test sample as test portions Details are given in Clause I f some material is stored for future investigations or for the purpose o f settling a potential dispute, subsamples shall be taken from the laboratory sample or the test sample in an acceptable and documented manner 5.1 Sampling strategy General During the planning process, the sampling strategy for the site under investigation is determined according to the objectives described in Clause item a), resulting in the definition of a sampling plan [1] ,[2 ] ,[4] ,[9 ] ,[11] ,[12] 5.2 Initial investigation Whatever the objective o f the work being carried out, certain preliminaries shall be undertaken during the initial investigation phase to help define the sampling strategy, such as the following: — analysis o f historical and administrative data, company archives, previous studies, and interviews with former employees, which help identi fy potential sources o f radioactive contamination; — collection o f in formation on geological, hydrological, and pedological characteristics and on the main climatic parameters, in order to characterize the spatial and temporal development o f the characteristics o f the radioactivity o f an area; — survey o f the site under investigation to identi fy its topography, the nature o f the vegetation cover, and any peculiarities that can a ffect the techniques and the sampling plan; — for farmland, collection o f in formation from the farmers on the nature and depth o f works (subsoiling or drainage, ploughing and harrowing ditches, etc.) and on chemical fertilizers and additives that can lead to excessive natural radioactivity (nature and quantity o f products applied) © ISO 2015 – All rights reserved ISO 18589-2:2015(E) When data on radioactive soil contamination are not available or in case o f suspicion o f contamination, in situ analytical investigation using portable detectors or some preliminary sampling and subsequent laboratory analysis can be necessary in order to select the sampling areas and strategy 5.3 Types of sampling strategies Sampling strategies are either orientated or probabilistic depending upon the objectives and the initial knowledge o f radioactivity distribution over the area under investigation Orientated strategies are based on a priori constraints that lead to a selection of sampling units in a specific area under special scrutiny because o f particular interest or level o f contamination Probabilistic strategies are based on a selection o f sampling units without any a priori constraints The selection of sampling units and points is described in 6.2 5.4 Selection of the sampling strategy The approach or sampling strategy shall be selected depending on the objective pursued and the relevant end points, for example the protection o f humans and the environment, taking into account social and economic constraints The sampling strategy selected should ensure that the radioactivity o f the samples is representative of the distribution of radionuclides in the soil of the area under investigation [1] ,[2 ] ,[4] ,[6 ] ,[9] Although the strategy can only be defined on a case-by-case basis, the selection o f the sampling strategy should follow these stages: — analysis o f the records, which enables an historic study o f the sampling site, in particular o f its previous use (identification o f the source); — evaluation o f pre ferential migration pathways and/or accumulation areas; — site reconnaissance with respect to the boundaries o f the sampling areas and sampling undertaken; — site reconnaissance: a rapid analytical investigation using portable radioactivity detectors can be used to characterize the distribution o f the radioactivity o f the areas to be studied This step in the planning process determines a large number of choices and can generate important and costly activities It also includes the definition o f the objectives o f the data quality according to the parameters to be analysed Annex A gives a flow diagram that helps in the selection o f a sampling strategy according to the objectives of the investigation The choice o f the strategy determines the sampling density, the temporal and spatial distribution o f the units from which samples are collected and the timing o f the sampling, taking into account the following: — potential distribution o f radionuclide: homogeneous or heterogeneous (“hot” spots); — characteristics o f the environment; — minimum mass o f soil necessary to carry out all the laboratory tests; and — maximum number o f tests that can be per formed by the laboratory for the study In many cases, a prediction o f the possible presence o f soil contamination and its distribution (homogeneous or heterogeneous) can be drawn up It is then necessary to veri fy these hypotheses by an orientated sampling strategy One variant o f this strategy, which is systematic with selected representative sampling points, is adapted for the routine monitoring o f sites whose radioactive origins and distribution patterns are known This allows a more accurate definition o f the number and location o f the sampling points than a purely probabilistic sampling strategy This subjective selection o f the sampling points can be combined with a statistical approach to meet the quality requirements for the © ISO 2015 – All rights reserved ISO 18589-2:2015(E) When layers are sampled by successive sections with a thickness equal to the total profile depth examined divided by the number o f sampling levels, care shall be taken to prevent overlapping o f sample layers from di fferent soil horizons A description of the soil indicating the soil horizons, their physical characteristics (colour, texture, structure, coarse-element content, etc.) shall be joined to the sample file to aid in the interpretation of the results 7.2.3.2 Samples taken from a trench A trench is dug, with suitable equipment, having a su fficient cross-section (e.g 0,5 m to m wide with a length o f m to m) to observe the full range o f the stratification profile (log) o f the excavated soil The dimensions o f the trench are determined according to the tool used (e.g mechanical digger with bucket), the depth to be reached (on average m), and the nature o f the soil The vertical wall o f the trench is scraped using a kni fe to find the soil horizons that are not compacted or contaminated by the digging instrument Increments with a minimum mass o f kg are taken from this wall manually using a spatula and from each horizon with stated dimensions, while avoiding mixing separate soil horizons The number o f increments per horizon is defined according to the dimensions o f the sampling unit and the required test-sample mass Particular care shall be taken to prevent soil falling into the probe trench be fore and during sampling The increments from the same horizon are placed in a clean container or plastic bag The resulting composite sample is mixed thoroughly using a shovel or other suitable tool During the operation, the clods are broken up and the coarse elements larger than cm are removed (or collected separately, depending on the objective o f the study) 7.2.3.3 Samples at depth by core drilling First, a sur face sample with a minimum mass o f kg o f dry matter and from a maximum depth o f cm is taken using a suitable piece o f equipment as described in 7.2.2.3 Second, the samples at depth are taken to the required depth by core drilling using suitable equipment The core(s) is (are) removed and then extracted from the coring tool onto a clean, inert, dry sur face The direction o f the cores (top-bottom) and the depths o f the samples are marked When using a uni form approach with predefined depth layers, the cores are cut starting from the sur face layer and are sliced into a minimum o f five sections (including the sur face layer sampled separately), while avoiding mixing the di fferent soil layers These sections constitute the increments o f the di fferent layers sampled When using a horizon approach, the cores are cut starting with the sur face layer and are sliced according to the boundary o f the di fferent soil horizons identified along the core length These sections constitute the increment o f the di fferent horizons sampled The number o f cores to be extracted, and consequently the number o f increments per layer or per horizon, is defined relative to the diameter o f the coring tool, the dimensions o f the sampling unit, and the required test-sample mass The constitution o f the composite sample and laboratory sample is described in 7.3 When using a coring tool with an internal sheath, the sheaths can be removed from the coring tool for transportation to the laboratory, where the opening o f the sheath, identification, and cutting o f the sample horizons or layers, the combining o f the increments from the same horizon or layer, and their possible reduction with the elimination o f coarse elements can take place under conditions more favourable than those on-site 12 © ISO 2015 – All rights reserved ISO 18589-2:2015(E) 7.3 Preparation of the sorted sample The increments from the same sampling unit are placed in a clean container or plastic bag The resulting composite sample is spread out over a clean, level, inert sur face and mixed thoroughly using a shovel or other suitable tool During the operation, the clods are broken up and the coarse elements larger than cm are removed (or collected separately, depending on the objective o f the study) in order to obtain a sorted sample For certain studies, the respective proportion o f coarse elements compared to the mass o f the sampled soil should be estimated and their radioactive characteristics measured The petrographic nature or the anthropogenic origin for rubble and apparent porosity o f the sample should be noted Latest tests that require special techniques are not included in the scope The quartering technique (see ISO 11464[19] ) can be used to split the sorted sample to obtain a subsample o f approximately kg o f dry matter All sorted samples sent to the laboratory shall be identified and a sample sheet drawn up in formity with the instructions in 7.4 For a soil profile, the samples taken from di fferent soil horizons shall not be mixed, unless otherwise required, and increments shall not be combined or undergo any homogenization or clod-crushing treatment when investigating radionuclides in the form of volatile compounds I 7.4.1 d e n t i f i c a t i o n a n d p a c k a g i n g o f s a m p l e s General Each sample shall be packed in a container that does not react with the soil, is clean and care fully sealed to avoid loss o f the contents or exposure to external agents (infiltration o f water, dust, etc.) The identification label shall be attached to the outside o f the packaging S a m p l e i d e n t i f i c a t i o n The label o f the container shall identi fy each sample and contain the following in formation: — code identi fying the sample, the sampling area, and the sampling unit; — date o f sampling; — additional in formation, such as the depth and thickness o f the soil horizon sampled, may be added 7.4.3 Sample sheet The sample sheet enclosed with the sample or series ofsamples shall include at least the following information: — identification and characteristics o f the sample (for example: location, depth, and thickness o f the soil horizon sampled, etc.) as indicated on the packing label; — sampling technique and the associated equipment; — date and time the sample was taken; — name o f the operator; — any observations necessary to interpret the results The topography o f the sampling area, i f uneven, is specified, particularly i f the samples are taken from the following areas: 1) in low-lying areas (trenches, plough furrows, depressions, etc.); © ISO 2015 – All rights reserved 13 ISO 18589-2:2015(E) 2) on elevate d are as (emb an kments , ridge s , plate au s , e tc ) ; 3) i n are as where the u nderlyi ng ro ck i s e xp o s e d; 4) i n marl pits , s pri ngs; 5) on the edge of the area When the s tudy expre s s e s the re s u lts o f the ana lys i s i n term s o f the s u r face ac tivity (s e e sheet shall also include: Clause ) , the S; — the s u r face are a s ample d , — the th ickne s s o f e ach l ayer s ample d; — the mas s o f the s or te d s ample, — the mas s o f any s or te d s ub s a mple, m ss; m′ss T h i s s he e t i s comple te d , where ne ce s s a r y, with: — an eva luation o f are a homo geneity; — a de s c rip tion o f the u s e o f the land; — a de s crip tion o f s ample s T he i n formation whe ther i mpu ritie s s uch as large s tone s , ro o ts , e tc were from remove d — the s a mple b e fore p ackagi ng s hou ld b e i nclude d i n the s a mpl i ng she e t; the we ather cond ition s i f s ample s are ta ken For s ample s from fol lowi ng an i nc ident or acc ident s evera l dep th s , the s ample s he e t s l l b e comple te d with a de s crip tion o f the s oi l hori z on s , i nd icati ng the d i fferent layers and thei r phys ic a l cha rac teri s tic s (colou r, te xtu re, s truc tu re, p ercentage o f co ars e elements , e tc ) E xample s o f s ampl i ng she e ts and Annex E 7.5 for a s i ngle/comp o s ite s a mple a nd for a s oi l pro fi le are given i n Annex D , re s p e c tively Transport and storage of samples T he p ackage d s a mple s and thei r s a mp le s he e ts shou ld b e tran s p or te d as qu ickly as p o s s ible to the lab orator y for ana lys i s Transport and storage conditions shall be such as to avoid all contamination of the material The [18 20 21] where f tra n s p o r t a nd p re s er vation temp eratu re s o the s a mp le s s ho u ld be s p e c i fie d ] ,[ ] ,[ ne ce s s a r y, i n the te s t rep o r t T he fol lowi ng — to avoid any warm i ng o f the s ample du ri ng tran s p or tation to the lab orator y a nd to u s e, where are p ar tic u l arly re com mende d: p o s s ible, i n s u late d contai ners; — to s tore the s ample up on arriva l at the lab orator y at a temp eratu re le s s tha n or e qua l to ° C and i n the dark when ne ce s s ar y and i f the ti me b e twe en s ampl i ng a nd tre atment o f the s ample exce e d s a few days; for longer p erio d s , the s ample may either b e pre s er ve d i n a fre e z er at −1 ° C , or d rie d at a ma xi mu m temp eratu re o f ° C and pre s er ve d i n an a i r tight p ackage; — to l i m it the ti me b e twe en s a mpl i ng a nd rad io ac ti ve ana lys e s , e s p e ci a l ly when re s e arch i ng rad ionucl ide s with s hor t h a l f-l ive s; — to ta ke p a r tic u lar pre c aution s i n the c a s e o f the i nve s tigation o f volati le, orga n ic a l ly b ound, or h igh ly s olub le rad ionucl ides (io d i ne, tritiu m, ch lori ne, e tc ) to avoid lo s s du ri ng the s torage o f the s ample s; 14 © ISO 2015 – All rights reserved ISO 18589-2:2015(E) to c arr y out the me a s urement as s o on a s p o s s ible a fter the s ample i s ta ken; i f later te s ts i nclude — the de term i nation o f the bu l k den s ity o f s ample s ta ken i n thei r natu l s tate, or even when the de term i nation o f thei r water content i s p er forme d, add itiona l pre c aution s a re ne ce s s a r y to avoid compacting or loss of water Pre-treatment of samples 8.1 Principle T he phys ic a l pro ce s s i ng o f s oi l lab orator y s a mple s to me as u re rad io ac tive nucl ide s re qu i re s d r yi ng , cr u sh i ng , s ievi ng , and homo gen i z i ng s tep s to b e c arrie d out B e fore any pre -tre atment, a prel i m i nar y a na lys i s o f the lab orator y s ample b y ga m ma s p e c trome tr y c an a l low de te c tion o f volati le rad ionucl ide s and, i f s o, the s ele c tion o f the ade quate pre -tre atment pro ce du re comp atible with the qua nti fic ation o f thei r ac tivity L a b o r a t o r y e q u i p m e n t T he fol lowi ng e quipment i s ne ce s s ar y to c arr y out the pre -tre atment o f the lab orator y s a mple: — a venti l ate d d r yi ng ro om or d r yi ng c abi ne t with a temp eratu re o f (4 ± ) ° C; — a he ate d , venti late d oven with a temp eratu re o f (10 ± 10) ° C; — e qu ipment for the re duc tion o f clo d s , p o s s ibly combi ne d with a s ieve, p e s tle and mor tar, p ounder, gri nder, c ru s her, or grip bre a ker; — a s ieve with a m m me sh s i z e; — a s ieve with a 0 µm or µm me sh s i z e; — a me ta l o r pla s tic tray with rai s e d e dge s; — a m i xer or b a l l m i l l; — fre e z e - d r yi ng 8.3 e quipment (when appropriate) Procedure With s ideration — — for the comp o s ition o f the te s t s ample, the fol lowi ng s tep s sh a l l b e c arrie d out Weigh the l ab orator y s ample Spre ad a th i n layer o f c m to cm o f the enti re i n iti a l te s t s a mple onto fl at contai ners a nd manua l ly bre a k up the s ample u s i ng a s u itable i n s tru ment — Remove a l l rema i n i ng pla nt p ar ts (tu fts o f gra s s , ro o ts , e tc ) — L e ave the s ample to d r y at ambient temp eratu re or i n a venti late d c abi ne t he ate d to a temp eratu re le s s tha n ° C for h to h, accord i ng to the moi s ture i n the s a mple — B re a k up the remai n i ng clo d s o f e ar th with s uitable e quipment — S ep arate the fi ne e ar th — D r y the p owder at (10 ± 10) ° C to a s ta nt weight When me as u ri ng volati le rad ionucl ide s , it i s b e tter to fre e z e - d r y from the co ars e elements u s i ng a m m s ieve and no te thei r mas s e s the s a mple or d r y it to a ma xi mu m fi xe d temp erature o f (4 ± ) ° C — C ru s h with a mor ta r, a m i xer, or a b a l l m i l l — Sieve u s i ng a 0 µm or µm s ieve, then homo gen i z e the p owder ob tai ne d © ISO 2015 – All rights reserved 15 ISO 18589-2:2015(E) — Repeat the crushing and sieving steps until the entire sample has been processed — Weigh the total powder and the unsieved material, then discard Record the mass obtained The powder part constitutes the test sample The above steps should be carried out in accordance with the procedures in ISO 11465[22] with respect to the drying temperatures and grain sizes Any modification o f the above procedure shall be justified and shall be included in the test report The operator is warned o f the risks o f possible contamination from the laboratory environment or by mixing the samples o f di fferent layers or origins Where possible, the samples should be treated in increasing the order o f activity When it is necessary to quickly obtain the results o f radioactive analysis, the sample can be dried directly in the oven then crushed and sieved without being dried at ambient temperature The mass o f removed parts such as plants, coarse elements, and water can be weighted When the radioactivity characterization o f the unsieved material above 200 µm or above 250 µm, made o f petrographic nature or o f anthropogenic origin such as building materials rubble, is required, this material is crushed in order to obtain a homogeneous powder for testing Determination of the activity deposited onto the soil 9.1 General I f the objective o f the sampling is to estimate the total amount o f the radionuclides deposited onto the soil, for example from fallout following radioactive gaseous e ffluent discharges from a nuclear installation or from past atmospheric nuclear tests, then samples shall be taken from depths o f cm and at least 20 cm to 30 cm, respectively The thickness, ei, and the sur face area, Si, o f the sampled layer are noted 9.2 Determination using surface activity data A specific procedure can be deduced from the following generic example It re fers to the sampling o f a regular square grid from which five increments are taken to make up a composite sample For each grid, a composite sample is made up from the five increments taken from the centre and at the four nodes o f the grids Each increment is taken from a known sur face area, for example using a frame o f 20 cm on a side and a maximum depth of cm See Figure F i g u r e — S c h e m a t i c s k e t c h o f a r e g u l a r s q u a r e g r i d surface area a n d o f i t s f i v e i n c r e m e n t s w i t h k n o w n The sum, S, o f the areas corresponding to the soil sur face increments, Si, for the five sur face increments, is defined by Formula (1): i, S= ∑ Si i (1) The five increments from the same gridding are placed in a clean container or plastic bag The resulting composite sample is spread out over a clean, level, inert sur face and mixed thoroughly using a shovel or other suitable tool During the operation, the clods are broken up and the coarse elements larger than 16 © ISO 2015 – All rights reserved ISO 18589-2:2015(E) cm are removed (or collected separately, depending on the objective o f the study) The resulting mass, o f the sorted sample is noted m ss, I f the test-sample mass, m ts, represents the whole mass o f the sorted sample o f the sampled layer, the sur face activity, A S, is calculated from the activity per unit o f mass, a, using Formula (2): AS = a × m ts S (2) The quartering technique (see ISO 11464[19] ) can be used to split the laboratory sample to obtain a mass o f kg o f dry matter Then the test sample represents a mass fraction, m ’ /m , o f the sorted sample and the sur face activity is calculated using Formula (3): AS = a × ss ss m ts m ss × S m' ss (3) 9.3 Determination by integration o f soil profile activity data This operation involves sampling across the entire area a ffected by the deposition to determine the extent o f the contamination on the sur face and at depth The sur face layer is sampled to a maximum depth o f cm and the underlying layers are sampled in 10 cm sections, or at each change in soil horizon, until the radionuclides studied are no longer detected The sur face activity, A S, is computed from the activities per unit o f mass, aj, over a soil profile o f j layers using Formula (4): AS = ∑a j × j m ts , j (4) S The quartering technique (see ISO 11464[19] ) can be used to split the laboratory sample to obtain a mass o f kg o f dry matter Then the test sample represents a mass fraction, m ’ /m , o f the sorted sample and the sur face activity is calculated using Formula (5): AS = ∑a j × j m ts S , j × m ss m ' j , ss j ss ss (5) , 10 Recorded information All steps and procedures carried out to establish the radioactivity o f soil samples shall be completely traceable as specified in ISO/IEC 17025 This implies a complete documentation o f the sampling strategy, the plan chosen, the sampling operations per formed, and the chain o f custody o f the sample preparation Sheets detailing the sampling and laboratory steps shall be recorded Each o f such records shall be dated and signed by a responsible person to attest the correctness o f the results Any relevant in formation recorded during the di fferent steps described in this part o f ISO 18589 likely to have a ffected the results should be mentioned in the final test report Records o f all relevant in formation on the measuring equipment needed for the confirmation process o f a result shall be kept These records shall demonstrate that each item o f the measuring equipment (balance, oven temperature, etc.) satisfies the metrological requirements specified within the confirmation process for the equipment Calibration certificates or verification reports and other relevant information shall be available © ISO 2015 – All rights reserved 17 ISO 18589-2:2015(E) Annex A (informative) Diagram of the selection of the sampling strategy according to the o b j e c t i v e s a n d t h e r a d i o l o g i c a l c h a r a c t e sampling areas r i z a t i o n o f t h e s i t e a n d See Figure A.1 Figure A.1 18 © ISO 2015 – All rights reserved ISO 18589-2:2015(E) Annex B (informative) Diagram of the evolution of the sample characteristics from the s a m p l i n g s i t e t o t h e l a b o r a t o r y See Figure B.1 Figure B.1 © ISO 2015 – All rights reserved 19 ISO 18589-2:2015(E) Annex C (informative) Example of sampling plan for a site divided in three sampling areas (A, B, C) See Figure C.1 Key A, B, C unsampled zone boundaries unsampled zone too small sampling unit sample unsampled points: low point, outcrop sampling areas 10 composite sample of n increments samples mix and eliminate coarse elements composite sorted sample subsampling laboratory samples Figure C.1 20 © ISO 2015 – All rights reserved ISO 18589-2:2015(E) Annex D (informative) Example of a sampling record for a single/composite sample Sample identification: Operator: Customer: SAMPLE SHEET Sampling area: Sampling unit: Date: Weather Conditions: SAMPLING UNIT CHARACTERISTICS: Reference topographic map: Increment Geographical Co-ordinates a SAMPLE CHARACTERISTICS number of increments Depth: Thickness a): : Topographic situation: X: Y: X: Y: X: Y: X: Y: Z: Z: Z: Z: Surface area a) , S: Mass a) , mss: Mass a) , m ss: ’ To be completed where necessary NATURE OF THE SAMPLING AREA NORTH Use of the land: LOCATION OF INCREMENTS VIII VII VI V IV III II I A B C D E F G H Basic grid: x metres OBSERVATIONS: CHARACTERIZATION OF SAMPLE Surface dose Special rate requirements needed for handling Colour FOLLOW-UP (LABORATORY) Search for the following radionuclides: © ISO 2015 – All rights reserved Texture Coarse elements % Coarse elements (nature) Organic products Type of soil horizon ADDITIONAL INFORMATION Description of pedological profiles Physical-chemical pedological analysis Other 21 ISO 18589-2:2015(E) Annex E (informative) E x a m p l e f o r a s a m p l e Sample identification: Operator: Customer: r e c f o r a s o i l p r o f i l e w i t h s o i l d e Sampling unit: Date: Weather Conditions: Reference topographic map: a r d SAMPLE SHEET Sampling area: AREA CHARACTERISTICS: Geographical Co-ordinates o Use of the land: i p t i o n ’ - Permanent - Temporary OBSERVATIONS: r Depth: Thickness a) : Surface area a) , S: Mass a) mss: Mass a) m ss: To be completed where necessary NATURE OF THE AREA Degree of artificialization c SAMPLE OR SAMPLE SERIES Topographic situation: X: Y: Z: s NORTH LOCATION OF SAMPLES VIII VII VI V IV III II I A B C D E F G H Basic grid: x metre CHARACTERIZATION OF SAMPLES TAKEN Type Number Depth Colour Texture FOLLOW-UP (LABORATORY) Search for the following elements: 22 Coarse elements % Coarse elements (nature) Organic Degree of Type of soil products eutrophication horizon ADDITIONAL INFORMATION Description of pedological profiles Physico-chemical pedological analyses Other © ISO 2015 – All rights reserved © ISO 2015 – All rights reserved DESCRIPTION OF THE SOIL Soil horizons Texture PROFILE N Colour(s) Moisture ° Coarse elements Organic Roots Structure(s) 10 Porosity Consistency Secondary elements 11 Various ISO 18589-2:2015(E) 23 ISO 18589-2:2015(E) Bibliography [1] [2] [3] MERIWETHER J.R., BURNS S.F and BECK J.N Evaluation o f soil radioactivities using pedologically based sampling techniques Health Phys 1995, pp 406–409 I nternational Atomic E nergy Agenc y 1989 Measurement o f Radionuclides in Food and the Environment Technical Report Series, No 295 Vienna IPSN, 2000 Guide méthodologique Gestion des sites industriels potentiellement contaminés par des substances radioactives [4] UNE 73311-1, 2002 Procedimiento de toma de muestras para la determinación de la radioactividad ambiental — Parte 1: Suelos, capa superficial [5] AKU 1999 Recommendations for the surveillance of environmental radioactivity (in German), Loseblattsammlung des Arbeitskreise s Umweltüberwachung (AKU) des Fachverbandes für Strahlenschutz e.V., November 1999, Winter M., Narrog J., Kukla W., Vilgis M (eds.) ISSN 1013-4506 [6] ISO 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes [7] ISO 10381-4, [8] Soil quality — Sampling — Part 4: Guidance on the procedure for investigation of natural, near-natural and cultivated sites ISO 10381-5, Soil quality — Sampling — Part 5: Guidance on the procedure for the investigation of urban and industrial sites with regard to soil contamination [9] RICHARD O.G., 1987 Statistical Methods for Environmental Pollution Monitoring, Van Nostrand Reinhold, New York [10] SCHEFFER, F and SCHACHTSCHNABEL, P, 1998 Lehrbuch der Bodenkunde, 14, neu bearbeitete und erweiterte Auflage, Ferdinand Enke Verlag [11] NUREG – 1575, EPA 402-R-97-106, DOE/EH-0624, 2000 Multi-Agency Radiation Survey and Site Investigation Manual (MARSSIM) [12] CEEM Comparative Evaluation o f European Methods for Sampling and Sample Preparation o f Soils Sci Total Environ 2001, 264 () [13] MUNSELL Soil Color Charts GretagMacbeth, New York, 2000 [14] PORTA J., et al 1994 Eda fología para la agricultura y el medio ambiente, Ed Mundi-Prensa, Madrid [15] DUCHAUFOUR Ph., 1995 Abrégé de pédologie, sol, végétation, environnement, MASSON (Paris) [16] Soil Survey Sta ff, 1975 Soil Taxonomy A Basic System o f Soil Classification for Making and Interpreting Soil Surveys, USDA, Handbook No 436 [17] ASTM C998-90, 2005 revision Standard Practice for Sampling Sur face Soil for Radionuclides [18] NF M 60-790-2, [19] [20] [21] 24 Mesure de la radioactivité dans l’environnement-Sol — Partie : Guide pour la sélection des zones de prélèvement, l’échantillonnage, le transport et la conservation des échantillons de sol (Measurement ofradioactivity in the environment-Soil — Part : Guide on selection ofsampling zones, soil sampling, transport and preservation of soil samples), 1998 ISO 11464, Soil quality — Pretreatment of samples for physico-chemical analysis UNE 73311-5, 2002 Procedimiento para la conservación y preparación de muestras de suelo para la determinación de radioactividad ambiental HASL – 300, 1997 The Procedures Manual of the Environmental Measurements Laboratory U.S Department of Energy 28th Edition © ISO 2015 – All rights reserved ISO 18589-2:2015(E) Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method Soil quality — Sampling — Part 2: Guidance on sampling techniques Measurement ofradioactivity in the environment — Soil — Part 7: In situ measurement of gamma-emitting radionuclides [2 ] ISO [2 ] I S O 1-2 , [2 4] 14 , I S O 8 -7, © ISO 2015 – All rights reserved 25 ISO 18589-2:2015(E) ICS 17.240; 13.080.01 Price based on pages © ISO 2015 – All rights reserved