NEN 7340Nederlandse

Leaching characteristics of solid earthyand stony building and waste materials.Leaching tests. General instructions

Uitloogkarakteristieken van vaste grond- en steenachtigebouwmaterialen en afvalstoffen. Uitloogproeven. Algemene aanwijzingen

1st edition, February 1995ICS 13.030-70;91.100

� 1995 Nederlands Normalisatie-instituutKalfjeslaan 2, Postbus 5059, 2600 GB Delft, Telefoon (015) 2 690 390, Fax (015) 2 690 190

Contents

page

Introduction 2

1 Scope 3

2 Normative references 5

3 Terms and definitions 53.1 Leaching characterization 53.2 Materials 53.3 Leaching tests 53.4 Accuracy 6

4 Principle 6

5 Procedure 65.1 Identification of the starting points 65.2 Choice of leaching tests for inorganic components 6

6 Report 7

Annex A – Commentary 9

Annex B – Informative references and overview of literature 11

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NEN 7340:1995Blz. 2

Introduction

In order to determine the various aspects of the leachingbehaviour (leaching characteristics) of solid (earthy andstony) building materials and wastes, a number of stagesmust be carried out. These stages are sampling, samplepretreatment, performance of leaching tests, digestionand chemical analysis of the solid substance and eluaterespectively. Each stage has its own coordinating stan-dard which gives general instructions. This documentspecifies the correlation between all standards relating tothe stage with a specific area of application for each. Forthe determination of the leaching characteristics, thegeneral instructions and the specific standards cited shallbe followed in close mutual correlation.

The general instructions for the leaching tests aredescribed in NEN 7340. This standard indicates whichleaching tests can be used in what situation and for whichmaterials. The result of the use of this standard is thechoice of the test or a combination of tests which shall becarried out in a given situation to unambigeously deter-mine the leaching characteristics of the material to betested.

The standards which characterize the various aspects ofthe leaching behaviour are produced and published inphases. This means that on publication of NEN 7340,some of the relevant standards will not yet have appearedas drafts or standards. For the missing stages, users ofNEN 7340 shall select the method to be applied. The stan-dards listed in Annex B and other publications availablein this context may also be used.

Since it is expected that in the years to come a largenumber of additions will have to be made to this standard,a regular update is planned.

The numbered chapters are normative with the exceptionof the passages marked ”Note”; the introduction andannexes are informative.

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NEN 7340:1995Blz. 3

1 Scope

This standard describes the way in which a choice shallbe made from standardized laboratory tests to determinethe leaching behaviour of inorganic and/or organic com-ponents from solid earthy and stony building and wastematerials.

Both NEN 7340 and the specific standards to which thisstandard refers (the leaching tests) are applicable to solidearthy and stony building materials and wastes. Liquidwastes are explicitly excluded from the scope of thesestandards.

The leaching tests relate to the elution in water of one ormore of the following types of components:

Inorganic components:

– Elements including arsenic, barium, cadmium, cobalt,chromium, copper, mercury, molybdenum, nickel,lead, antimony, selenium, tin, vanadium and zinc;

– Oxi-anions, including sulphate;– Halogen(ide)s, including bromide, chloride and fluor-

ide;– Cyanides.

Organic components:

– Aromatic hydrocarbons, including benzene, ethyl ben-zene, toluene and xylenes (BETX);

– Phenols;– PAH (polycyclic aromatic hydrocarbons);– PCB (polychlorinated biphenyls);– EOX (extractable organohalogens);– Mineral oil.

NOTES1. The field of application is established on the basis

of experience with a large number of materials, ofwhich examples are mentioned in table 1. Theclassification of the materials by grain-size classand category is based on the practical consider-ations with regard to the execution of the leachingtests.

2. Because of the open nature of the field of applica-tion the leaching tests cannot be validated inadvance for all solid (earthy and stony) buildingmaterials and wastes and the components occur-ring in them. For the materials marked in the lastcolumn of table 1 the applicability of the leachingtests is tested for certain components by means ofa a ring test according to NEN-ISO 5725; for thosematerials the precision in terms of repeatabilityand reproducibility is described [6].

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NEN 7340:1995Blz. 4

Table 1: Overview of solid (earthy and stony) building and waste materials to which the leaching tests apply

Grain-size class Category Examples1) Validation 9)

1. Powdered materials andsludges(0 �m to 125 �m)

1.a Binders CementLime

1.b Fly ashes Pulverized coal fly ashMSWI fly ashSilicafumeFluidized bed fly ash

1T2T3T

1.c Gypsum Phosphoric acid gypsumFluegas desulfurization gypsum

1.d Sludge Dredged earthWaste water treatment sludge 2)

Drinking water treatment sludge

2. Fine-grained materials(0 mm to < 4 mm)

2.a Clay and sandymaterials

Natural clayLoamNatural sandSifter sandCleaned soilCrusher sandsRecycling crusher sandsEuro ClayBentoniteDrilling mud

2.b Granulates Pulverized coal bottom ashGranulated blast furnace slagCoal gassification residuesSand blasting wasteFluidized bed bottom ash

1T2T3T

3. Coarse-grained materials(0 mm to > 4 mm)

3.a Quarryd materials GravelLavaliteSilex

3.b Granulates Hydrotherm. PCFAG 3)

Sintered PCFAG 4)

Cold bound PCFAG 5)

MSWI bottom ash 6)

Concrete granulateBlack quarry stoneAsphalt granulateMasonry granulateMixed granulateExpanded clay granulate

1T2T3T

3.c Slag Blast furnace slagPhosphorous slagLD-steelslag 7)

Copper slagLead slagElo-slagChromium slagFoam slag

4. Products or monolithicmaterials

4.a Cold-bondedproducts

Cement concreteConcrete productsAsphalt concreteCement stabilized mixturesBituminous bound mixturesMortarFoam concrete

1T4T

4.b Autoclavedproducts

Calcium silicate bricksAutoclaved aerated concrete(AAC) 8)

1T4T

4.c Coarse ceramics Clay bricksPaving clinckerRoof tilesStoneware pipe

1T4T

4.d Coarse slag Blast-furnace slagphosphorous slagSteel slag 7)

Copper slagLead slag

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NEN 7340:1995Blz. 5

Legends for Table 1:1) The materials mentioned as an example are classified

in the category in which they most commonly occur;For the definitions: see NNI publication SPE 80001.

2) Sludge from a waste or sewage treatment plant3) Hydrothermally bonded pulverized coal fly ash granu-

late, for example aardelite4) Sintered pulverized coal fly ash granulate, for example

lytag5) Cold-bonded pulverized coal fly ash granulate6) In NNI publication SPE 80001 called ’AVI-slak’ (MSWI

bottom ash)7) In NNI publication SPE 80001 called ’LD-slak’ (steel

slag)8) In NNI publication SPE 80001 called ’gasbeton’ (light

weight concrete)9) 1 = NEN 7341; 2 = NEN 7343; 3 = NEN 7349;

4 = NEN 7345;T = tested in round robin test according toNEN-ISO 5735 [6].

2 Normative references

NEN 7310:1995 Leaching characteristics of solid earthyand stony building materials andwaste products. Sample pretreatment.General instructions.

NEN 7341:1995 Leaching characterisctics of solidearthy and stony building and wastematerials. Leaching tests. Determina-tion of the availability of inorganiccomponents for leaching.

NEN 7343:1995 Leaching characterisctics of solidearthy and stony building and wastematerials. Leaching tests. Determina-tion of the leaching of inorganic com-ponents from granular materials withthe column test.

NEN 7345:1995 Leaching characteristics of solid earthyand stony building and waste ma-terials. Leaching Tests. Determinationof the leaching of inorganic compo-nents from building and monolithicwaste materials with the diffusion test.

NEN 7349:1995 Leaching characterisctics of solidearthy and stony building and wastematerials. Leaching tests. Determina-tion of the leaching of inorganic com-ponents from granular materials withthe cascade test.

SPE 80001:1992 Definities en toepassingen van steen-achtige bouwstoffen. Stand van zaken.publication of NNI (SPE 80001), CUR(report 92-11) and C.R.O.W (publica-tion 62).

3 Terms and definitions

3.1 Leaching characterization

3.1.1 leaching: The elution of inorganic and/or organiccomponents from materials by static or dynamic contactwith a leachant.

3.1.2 leachant: Liquid to which the material is exposed.

NOTEIn this standard reference is always made to leachingtests with acidified water as leaching liquid.

3.1.3 eluate: Leachant containing the inorganic and/ororganic components leached from the material.

3.1.4 value of L/S: The quotient of the cumulative vol-ume of leachant and the mass of the material exposed toleaching (expressed in l/kg).

3.1.5 availability: The quantity of a certain componentwhich can leach out of a material, in an aerobic environ-ment, exposed to extreme conditions (such as in the verylong term, after disintegration of the material, after fulloxidation and/or upon elimination of the acid-neutrali-zation capacity).

3.2 Materials

3.2.1 solid earthy and stony building and wastematerials: Materials with a dry matter content of at least30 % (m/m), characterized by a matrix which largely con-sists of silicon and aluminium (hydr)oxides and/or cal-cium compounds and in which one or more inorganicand/or organic components as referred to in section 1may be present because of the way they are formed, theirproduction and management or pollution.

3.2.2 powdered materials and sludges: Solid earthy andstony building and waste materials with such a grain sizedistribution that at least 95 % (m/m) (dry matter) is smallerthan 125 �m.

3.2.3 fine-grained materials: Solid earthy and stonybuilding and waste materials, not being powdered ma-terial or sludge, with such a grain size distribution that atleast 95 % (m/m) (dry matter) is smaller than 4 mm.

3.2.4 coarse-grained materials: Solid earthy and stonybuilding and waste materials with such a grain size dis-tribution that more than 5 % (m/m) (dry matter) is greaterthan 4 mm.

3.2.5 products: Solid earthy and stony building andwaste materials which are made by homogeneously mix-ing one or more granular materials and, possibly, one ormore different types of additional materials (such aswater), after which such a bonding between the raw ma-terials is achieved that form, dimensions and propertiesof the resulting product meet predetermined require-ments.

NOTEThe process, during which the bonding occurs, maytake place under ambient conditions (cold-bondedproducts), at a raised temperature (sintered and vitri-fied products) or at a raised temperature and pressure(autoclaved products). Product requirements areamong other things set for the dimensions, fracturestrength, etc.

3.2.6 monolithic materials: Solid earthy and stonybuilding and waste materials which are formed in a pro-cess from one or more compounds without the form andproperties of the resulting product meeting predeter-mined requirements and for which the piece size has aminimum dimension of at least 40 mm.

NOTEMonolithic materials arise in natural or industrial pro-cesses in which a melt occurs. The biggest pieceswhich arise after cooling and breaking of the melt, witha minimum dimension of more than 40 mm, fall withinthe category of monolithic materials (or bulk slags).

3.3 Leaching tests

3.3.1 availability test: Test to simulate the availability forleaching of certain components.

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NEN 7340:1995Blz. 6

NOTEIn the availability test very fine-grained material isused so as not to hinder leaching because of diffusionlimitations. Leaching takes place at a high value of L/S,so that there is a minimum solubility limitation with pHcontrol at pH = 7 and pH = 4, or without pH control,where the pH is found to be adjusted to a lower value.

3.3.2 column test: Test to simulate the leaching behav-iour of powdered and granular materials as a function ofthe value of L/S over a range of L/S of 0 l/kg to 10 l/kg.

NOTEIn the column test the material is placed in a verticalcolumn and a leachant (up to pH = 4 acidified water) ispassed through the material from the bottom,whereby at several times the concentrations of theleached components are measured in the eluate. ThepH value of the eluate is enforced by the material itself.

3.3.3 cascade test (serial batch test): Test to simulatethe leaching behaviour of powdered and granularmaterials as a function of the value of L/S over a range ofL/S of 20 l/kg to 100 l/kg.

NOTEIn the cascade test the material is shaken five times insuccession with an equal quantity of (fresh) leachant(up to pH = 4 acidified water) whereby the concentra-tions of the leached components in the successivelyobtained eluates are measured. The pH value at whichleaching is carried out is always enforced by thematerial itself.

3.3.4 diffusion test: Test to simulate the leaching beha-viour of products and monolithic materials.

NOTEBy placing a whole test piece in the leachant (up topH = 4 acidified water) and refreshing the eluate at sev-eral times, diffusion-controlled leaching is simulated.Parameters can be deduced from the course of the elu-tion of components over time, including the long termdiffusion coefficient which can be used to estimateleaching on the long-term.

3.4 Accuracy

3.4.1 precision: The degree to which mutually indepen-dent results of tests carried out in accordance with thestandard approximate with each other. The precision isexpressed in terms of repeatability and reproducibilityand is expressed as a mean percentage error.

3.4.2 repeatability: The difference between the resultsof two determinations, carried out in singular, shortlyafter one another on the same sample material, carriedout in the same laboratory, with the same equipment andby the same person.

3.4.3 reproducibility: The difference between the resultsof two determinations, carried out in singular, on thesame sample material in different laboratories, with dif-ferent equipment and by different persons.

3.4.4 lower detection limit (LDL): The content of a com-ponent in the material or its eluate which can just bequantitatively determined by the method of analysisused.

NOTES1. For the determination of the precision of the leach-

ing tests a ring test was carried out with a numberof materials in accordance with NEN-ISO 5725 [6].

2. Standards are being prepared to determine thecontent of a component in the eluate.

4 Principle

The aim of the standard is to determine the leachingbehaviour of inorganic and/or organic components fromsolid earthy and stony building and waste materialsunder laboratory conditions. To reach this, the material tobe tested shall be submitted to the most suitable leachingtest or series of leaching tests. This standard describesthe route which must be followed to make a correctchoice from the available standardized leaching tests.

5 Procedure

5.1 Determination of the starting points

Determine the nature of the information expected on theleaching behaviour of the material to be tested. To thisend establish:a) whether the test is necessary to determine– the availability for leaching and/or– the leaching of granular material as a function of the

value of L/S (on dynamic contact with the leachant)and/or

– the diffusion-controlled leaching of a product ormonolithic material (on static contact with the leach-ant).

b) for what components the leaching behaviour must bedetermined.

NOTES1. For a full characterization of the leaching beha-

viour of a material all or most of the above-men-tioned determinations are necessary. Where thequestion is more limited or there is prior know-ledge, a selection of one or a few of these determi-nations may be sufficient, whereby a limited selec-tion can also be made of the components to bemeasured/determined.

2. Annex A includes a brief description of the ways inwhich the leaching of a material can be tested. Thisannex includes a diagram (figure A.1) in which theline to be followed in choosing standardizedmethods is illustrated.

5.2 Choice of leaching tests for inorganic components

NOTES1. At the moment standards are only available to

determine the leaching of inorganic components.The development of standards relating to theleaching of organic components is still in prepara-tion. For the time being only an informative refer-ence can be made to the methods to determinePAHs as described in [5].

2. In the following only the possible choices are ela-borated for which at present standardized tests aredescribed. In the light of the development pro-gramme for NEN-standards in this respect, thissection will be regularly supplemented and up-dated.

5.2.1 AvailabilityWhere the availability shall be determined, the availabi-lity test in accordance with NEN 7341 shall be carried out.

The requirements for the samples to be tested are speci-fied in clause 5 of NEN 7341: 1995. Powdered materialsand sludges do not have to be crushed. Other materialsshall be crushed, for example in accordance withNEN 7310.

5.2.2 Leaching as a function of the value of L/S toL/S = 10 l/kgWhere the leaching shall be determined for a value of L/Sof between 0 l/kg and 10 l/kg, the column test shall be car-ried out in accordance with NEN 7343.

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