1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58physico-chemical analysisICS 13.080.05Soil quality Pretreatment of samples for BRITISH STANDARDBS I
2、SO 11464:2006BS ISO 11464:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2006 BSI 2006ISBN 0 580 49365 2Amendments issued since publicationAmd. No. Date CommentsThis publication does not purport to include all the necessary pr
3、ovisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard was published by BSI. It is the UK implementation of ISO 11464:2006. It supersedes BS 7755-3.5:1995 which
4、is withdrawn.The UK participation in its preparation was entrusted by Technical Committee EH/4, Health and Environment Sector Policy and Strategy Committee, to Subcommittee EH/4/3, Soil quality.A list of organizations represented on EH/4/3 can be obtained on request to its secretary.INTERNATIONALSTA
5、NDARDISO11464Second edition2006-07-01Reference numberISO 11464:2006(E)Soil quality Pretreatment of samples for physico-chemical analysisQualit du sol Prtraitement des chantillons pour analyses physico-chimiquesBS ISO 11464:2006iiiiiContents Page1 Scope 12 Normative references 13 Principle 14 Apparat
6、us . 35 Procedure . 35.1 General . 35.2 Sample description . 45.3 Drying . 45.3.1 General 45.3.2 Air drying 45.3.3 Oven drying 45.3.4 Freeze-drying 45.4 Crushing and removal of coarse materials . 55.4.1 Separation of stones, etc. 55.4.2 Crushing 55.5 Subsampling 55.5.1 General 55.5.2 Subsampling by
7、hand (quartering) . 65.5.3 Use of the sample divider 65.5.4 Mechanical subsampling . 65.6 Milling . 66 Test report 6Annex A (informative) Examples of apparatus 8Bibliography . 11BS ISO 11464:2006ivForewordISO (the International Organization for Standardization) is a worldwide federation of national
8、standards bodies(ISO member bodies). The work of preparing International Standards is normally carried out through ISOtechnical committees. Each member body interested in a subject for which a technical committee has beenestablished has the right to be represented on that committee. International or
9、ganizations, governmental andnon-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the InternationalElectrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given i
10、n the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standardsadopted by the technical committees are circulated to the member bodies for voting. Publication as anInternational Standard requires approval by at least 75 % of
11、 the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of patentrights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 11464 was prepared by Technical Committee ISO/TC 190, Soil qualit
12、y, Subcommittee SC 3, Chemicalmethods and soil characteristics.This second edition cancels and replaces the first edition (ISO 11464:1994), which has been technicallyrevised.BS ISO 11464:20061Soil quality Pretreatment of samples for physico-chemical analysis1ScopeThis International Standard specifie
13、s the pretreatments required for soil samples that are to be subjected tophysico-chemical analyses of stable and non-volatile parameters and describes the following five types ofpretreatment of samples: drying, crushing, sieving, dividing and milling.The pretreatment procedures described in this Int
14、ernational Standard are not applicable if they affect the resultsof the determinations to be made. This International Standard is also not applicable to samples when volatilecompounds are measured. In general, International Standards for analytical methods will state when it isnecessary to adopt oth
15、er procedures.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of the referenced document(including any amendments) applies.ISO 565, Test si
16、eves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes ofopeningsISO 10381-8, Soil quality Sampling Part 8: Guidance on sampling of stockpilesISO 16720, Soil quality Pretreatment of samples by freeze-drying for subsequent analysis3 PrincipleSoil samples are dried in air,
17、 or in an oven at temperature not exceeding , or freeze-dried (see 5.3). Ifnecessary, the soil sample is crushed while still damp and friable, and again after drying (see 5.4). The soil issieved and the fraction smaller than is divided into portions mechanically, or by hand, to enablerepresentative
18、subsampling for analysis (see 5.5). If small subsamples ( ) are required for analysis, thesize of the particles of the fraction smaller than is further decreased (see 5.6). The necessary proceduresare given in the flow diagram in Figure 1.A drying temperature of in an oven is preferable to air dryin
19、g at room temperature because the increasedspeed of the drying limits changes due to microbial activity.It should be noted that every type of pretreatment will have an influence on several soil properties.The sieve aperture size of is generally used. However, before the pretreatment is started, it s
20、hould bechecked if any of the analytical methods to be applied later require other sieve sizes.NOTE Storing soil samples, including samples that are as received, air dried, refrigerated or stored in the absence of light,for a long time may have an influence on a number of soil parameters, especially
21、 solubilities of both inorganic and organicfractions. See Reference 1.Special measures should usually be taken for samples from contaminated soils. It is important to avoid contactwith the skin and special provisions should be taken when drying such samples (air discharge, ventilation, etc.).40C2mm
22、2g2mm40C2mmBS ISO 11464:20062Figure 1 Diagram for sample pretreatmentBS ISO 11464:20063Samples may be hazardous because of the presence of chemical contaminants, fungal spores, or pathogenssuch as leptospirosis, and appropriate safety precautions should be taken.In this International Standard, it is
23、 generally assumed that at least of fresh soil is available.Keeping an archive sample (see Figure 1) is optional and should be clearly stated in the overall description ofthe investigation programme.4 ApparatusIt is essential that the apparatus used does not add or remove any of the substances under
24、 investigation (e.g.heavy metals). If the use of certain equipment and/or materials is not permitted in pretreatment of samplesrequired for a particular physico-chemical analysis, this shall be mentioned in the relevant InternationalStandards on analysis (see Note).4.1 Drying oven, thermostatically
25、controlled, with forced ventilation and capable of maintaining a temperaturenot exceeding .4.2 Freeze-drier, optional.4.3 Crusher(s), mill(s), mortar and pestle, wooden or other soft-faced hammer (see Note).4.4 Plate sieve, complying with ISO 565, with an aperture of .4.5 Mechanical mixer(s).4.6 Mec
26、hanical sieve shaker, optional (see Note).4.7 Subsampler or sample divider (see Note).4.8 Mesh sieve, complying with ISO 565, with apertures of or of the size specified in the relevant testmethod.4.9 Analytical balance, readable and accurate to .4.10 Balance, readable and accurate to .NOTE The appar
27、atus to be used is not specified in detail, although drawings of some suitable items of equipment areprovided in Figures A.1 to A.4. Most comparable national standards contain detailed equipment specifications and thesemay be used, provided they meet the basic performance requirements indicated in t
28、his International Standard.5 Procedure5.1 GeneralThe procedures for drying, fraction separation and size reduction are set out in 5.3 and 5.4. At several stages inthe procedure, the analyst will be required to make decisions, referring in particular to whether size fractions areto be combined or tre
29、ated separately: this will depend on the nature of the soil and the objectives of theanalytical programme.The sample shall be rehomogenized after any separation, sieving, crushing or milling operation (that may haveresulted in segregation of different sized particles) has been carried out.WARNING Ta
30、ke special precautions with samples from potentially hazardous soil. Avoid any contactwith the skin and make special provisions concerning drying (air discharge, ventilation, etc.).Care should be taken to avoid contamination of the sample via the air or by dust (e.g. from the ambientlaboratory atmos
31、phere or between samples stored or processed close to one another).500 g40C2mm250m0,1 g1gBS ISO 11464:20064It is recommended that pretreatment of soil material always be performed in a room used only for this purposeand remote from locations where analytical measurements are made.NOTE If the sample
32、has a dust-like consistency, part of it may be lost, and this may alter its physico-chemical properties.5.2 Sample descriptionExamine the sample as received and record the description including details of extraneous matter, remains ofvegetation, and other noticeable or relevant features.5.3 Drying5.
33、3.1 GeneralDry the complete sample in air or in a ventilated drying oven from which the moist air is removed or in a freezedryer. Depending on the chosen method of drying, follow the procedure set out in 5.3.2, 5.3.3 or 5.3.4. Dry untilthe loss in mass of the soil sample is not larger than (mass fra
34、ction) per . After the drying process hasbeen completed, determine and record the total mass of the dried sample.To accelerate the drying process, break down the size of larger aggregates (larger than ) during theprocess. When samples are dried in air, crush them lightly by hand using a wooden hamme
35、r or a mortar andpestle, taking great care to avoid contamination. When samples are dried in an oven, remove them temporarilyfrom the oven and treat them in the same way. This procedure also makes it easier to separate the particleslarger than .Freeze-drying has the advantage that the sample to be d
36、ried rarely dries into clods; it usually breaks up intoparts.The drying time depends on the type of material, the thickness of the layer, the initial moisture content of thematerial and of the air, and on the rate of ventilation. In a drying oven, the drying time for sandy soils is usuallynot more t
37、han and for clay soils more than . For soils containing a large proportion of fresh organicmatter (e.g. plant roots, etc.), to may be required.5.3.2 Air dryingSpread all the material, in a layer not thicker than , on a tray which does not absorb any moisture from thesoil and which does not cause con
38、tamination.It is essential that direct sunlight be avoided and the temperature does not exceed .NOTE Direct sunlight could create large temperature differences in the sample, especially between the partly or completelydried top layer and the lower layers.5.3.3 Oven dryingSpread all the material, in
39、a layer not thicker than 5 cm, on a tray made of material which does not absorb anymoisture from the soil and which does not cause contamination. Put the tray in the drying oven (4.2) and dry ata temperature that does not exceed .5.3.4 Freeze-dryingFreeze-drying shall be performed according to ISO 1
40、6720.5% 24 h15 mm2mm24 h 48 h72 h 96 h5cm40C40CBS ISO 11464:200655.4 Crushing and removal of coarse materials5.4.1 Separation of stones, etc.Before crushing, which isnecessary if soil samples have dried into large aggregates, extraneous matter, such asstones, fragments of glass and rubbish, should b
41、e removed from the dried sample. This process may befacilitated by the use of a sieve (4.5) and by hand picking (see the following paragraph). Care should betaken to minimize the amount of fine material adhering to the extraneous matter removed. Determine andrecord the mass of any matter removed at
42、this stage.If the material under examination is a contaminated soil or waste, the analyst may wish to crush the completesample, including, for example, pieces of slag, to pass the sieve.5.4.2 CrushingIf a sieve has been used to facilitate removal of extraneous matter, any large dried particles remai
43、ning onthe sieve should be crushed (using suitable apparatus) to smaller than . The apparatus used shouldbe adjusted so that any crushing of the large particles is minimized to enable crushed particles to pass throughthe sieve.If a sieve has not been used to facilitate removal of extraneous matter,
44、then the dried sample should besieved through a sieve. Any large dried particles remaining on the sieve should be crushed (usingsuitable apparatus) to smaller than . The apparatus used shall be adjusted in such a way that completecrushing of particles larger than before drying is minimized.The whole
45、 sample passing through the sieve should be weighed and well mixed.If the fraction of aggregates larger than is low, it may be more efficient to sieve out particles smaller thanprior to crushing.In special cases, the entire sample may be crushed.Fractions may be recombined after crushing using a mec
46、hanical mixer (4.6).5.5 Subsampling5.5.1 GeneralSubsampling is necessary when the sample cannot be stored (laboratory sample and archive sample) or used(test sample) completely, because of its size. For the preparation of a laboratory sample, divide the dried,crushed and sieved sample (now ) into re
47、presentative portions of to according to 5.5.2 or5.5.3. For the preparation of a test sample, split up the laboratory sample into representative portions until therequired sizes of samples are obtained. Avoid the production of dust as much as possible.In the case of larger sample masses, subsampling
48、 methods according to ISO 10381-8 shall be used to reducethe initial sample size.It may be necessary to mill the material (5.6) between subsampling stages, to ensure homogeneity as the massof the subsample is decreased. The procedures described in 5.5.2 and 5.5.3 may be used to producesubsamples/tes
49、t portions of the materials smaller than , and not smaller than in mass.When replicate analyses are required, it shall be clarified in the overall investigation plan at which stage ofsubsampling replicates must be separated. The most representative stage would be a very early one.Select the method of subsampling (5.5.2, 5.5.3 or 5.5.4) according to the nature of the sample, therequirements of the subsequent determinations and the equipment available.2mm2mm2mm2mm 2mm2mm2mm2mm 2mm2mm2mm2mm2mm2mm 2mm 200 g 300
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