CEN/TC 308/WG 1 - Characterization methods

This document specifies a method for determining the zone settling velocity (ZSV) and the Compression point.
This document is applicable to sludge and sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   plants treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
-   water supply treatment plants.
This method is also applicable to sludge and sludge suspensions of other origins.

This document specifies a method for the determination of the sludge (bulk) density. The procedure to determine density of the liquid and of the solid fractions of a suspension is described in Annex C.
This document is applicable to sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   treating industrial wastewater similar to urban wastewater [7];
-   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin, provided the necessary verifications are done.

This document specifies a method for the determination of drainability of flocculated sludge. It is applicable to sludge and sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
-   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

This part of the European Standard specifies a method for determining the flowability, as defined in CEN/TR 15463, of sludge by means of the extrusion tube apparatus.
This part of this European Standard is applicable to sludge and sludge suspensions from:
—   storm water handling;
—   urban wastewater collecting systems;
—   urban wastewater treatment plants;
—   plants treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
—   water supply treatment plants.
This method is also applicable to sludge and sludge suspensions of other origins.

The laboratory assessment of sludge dewaterability is sensitive to the operating procedure adopted for the conditioning step. No generalized ranking of products in order of effectiveness can be given since the ranking changes with the sludge type, dosage of conditioning agent, degree of shearing and dewatering device.
The scope of this European Standard applies for sludges and suspensions from:
- storm water handling;
- urban wastewater collecting systems;
- urban wastewater treatment plants;
- industrial wastewater that has been treated similarly to urban wastewater (as defined in Directive 91/271/EEC);
- water supply plants.
This method is applicable to sludge and suspensions of other origin.

CEN/TC 308 origin - editorial modification in 5.1.2 in the mother standard (concerns the English language version).

This Technical Report deals with methodologies for preparing synthetic suspensions. Synthetic suspensions can be used for:
a)   evaluating or testing new devices or techniques for suspension treatment;
b)   studying the influence of different compounds on suspension behaviour with regard to specific parameters, e.g. settleability, dewaterability, physical consistency, etc.
The chemical, physical and biological characteristics of suspensions are subjected to changes as soon as they are collected. Guidance exists on the sampling and handling techniques (see ISO 5667 12 and EN ISO 5667 13), and on the preservation and storage procedures (EN ISO 5667 15) that help minimize changes in the composition. This is mainly achieved by suppressing chemical and/or biological activity and by avoiding contamination.

This European Standard specifies a method for determining the specific resistance to filtration of conditioned and non-conditioned sludges, provided that no sedimentation occurs during filtration (i.e. single phase suspension with particles in suspension).
This European Standard is applicable to sludges and sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   industrial wastewater that has been treated similarly to urban wastewater (as defined in Directive 91/271/EEC);
-   water supply treatment plants.
This method is also applicable to sludge and sludge suspensions of other origins.

ISO 5667-13:2011 gives guidance on the sampling of sludges from wastewater treatment works, water treatment works and industrial processes. It is applicable to all types of sludge arising from these works and also to sludges of similar characteristics, e.g. septic tank sludges. Guidance is also given on the design of sampling programmes and techniques for the collection of samples.

ISO 5667-15:2009 provides guidance on procedures for the preservation, handling and storage of samples of sewage and waterworks sludge, suspended matter, saltwater sediments and freshwater sediments, until chemical, physical, radiochemical and/or biological examination can be undertaken in the laboratory.
The procedures in ISO 5667-15:2009 are only applicable to wet samples of sludge, sediment and suspended matter.

This European Standard specifies a method for the determination of the gross calorific value of sludge at constant volume and at the reference temperature 25 °C in a bomb calorimeter calibrated by combustion of certified benzoic acid.
The result obtained is the gross calorific value of the sample at constant volume with both the water of the combustion products and the moisture of the sludge as liquid water. In practice, sludges are burned at constant (atmospheric) pressure and the water is not condensed but is removed as vapour with the flue gases. Under these conditions, the operative heat of combustion to be used is the net calorific value of the fuel at constant pressure. In this European Standard the net calorific value at constant volume is described as it requires less additional determinations.
This method is applicable to all kinds of sludges.

ISO 16720:2005 specifies a method for pretreatment of soil samples by freeze-drying for subsequent analysis.
ISO 16720:2005 is applicable to soil samples for subsequent determination of elements or organic compounds recognized as non-volatile under freeze-drying conditions. Generally, ISO 16720:2005 can also be applied to samples from sludges and sediments.
This method is also applicable as a first step for the determination of dry matter (or water) content, for instance in the case of samples with high water content.

This CEN-Report "Physical Consistency" derives from the Desk Studies "Physical Properties -Flowability"(HORIZONTAL Report No. 21 [60]) and "Physical Properties - Solidity, Thixotropic Behaviour andPiling Behaviour" (HORIZONTAL Report No. 22 [61]) of the Horizontal Project. The "Horizontal" project hasthe objective to develop horizontal and harmonised European standards in the fields of sludge, bio-waste andsoil to facilitate regulation of these major streams in the multiple decisions related to different uses anddisposal governed by EU Directives. The Horizontal Project includes the Work Package 7 "Mechanicalproperties" consisting in the development of Desk Studies on physical consistency, because it is recognizedthat this property is very important for the characterization of sludge, since it affects almost all treatment,utilization and disposal operations, such as storage, pumping, transportation, handling, land-spreading,dewatering, drying, landfilling. The importance of the physical consistency is also true for the characterizationof bio-waste and soil. Also handling and utilization of many other materials, such as cement and asphalt arestrictly depending on their physical consistency. The needs for control of operations and also materialcharacteristics are described.

This document specifies a method for the determination of the settleability of sludge suspensions. This document is applicable to sludge suspensions from:
¾   storm water handling;
¾   urban wastewater collecting systems;
¾   urban wastewater treatment plants;
¾   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271 EEC);
¾   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

This document specifies a method for the determination of the thickenability of sludge suspensions. This document is applicable to sludge suspensions from:
¾   storm water handling;
¾   urban wastewater collecting systems;
¾   urban wastewater treatment plants;
¾   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271 EEC);
¾   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

This document specifies a method for the determination of the capillary suction time. This document is applicable to sludge and sludge suspensions from:
¾   storm water handling;
¾   urban wastewater collecting systems;
¾   urban wastewater treatment plants;
¾   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
¾   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

This Technical Report specifies procedures for validating characterization methods for physical properties of sludge.
This Technical Report is applicable to sludge and sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
-   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

This document specifies a method to determine the compressibility of sludges, conditioned or not.
This document is applicable to sludges and sludge suspensions from:
   storm water handling;
   urban wastewater collecting systems;
   urban wastewater treatment plants;
   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
   water supply treatment plants.
This method is also applicable to sludge and sludge suspensions of other origin.

This European standard specifies a procedure for the determination of extractable ammonia using a 2 mol/l potassium chloride solution in raw and digested sewage sludges. The range of the method is up to 100 g/kg N assuming appropriate dilution of the potassium chloride extract in the final measurement step.
   The above wording will be modified once the round robin results are available. It may be suitable for other types of sludges, but the user should validate the method using these sludges.

This Technical Report specifies the requirements for interlaboratory tests to validate chemical and microbiological methods for sludges.

This European Standard specifies a procedure for complete digestion of raw/digested sludge, suitable for the subsequent determination of phosphorus.
Phosphorus in environmental samples can be present in many forms. This method of pre-treatment enables the analyst to determine all forms - i.e. total phosphorus, by quantitative oxidation yielding an aqueous solution of orthophosphate which should be analysed for phosphate according to method EN ISO 6878, EN ISO 10304-2 or an equivalent validated method.
The range of the method is up to 50 g/kg P assuming appropriate dilution of the digest in the final measurement step.

This part of the CEN Technical Report specifies a membrane filtration procedure for the quantitative resuscitation and enumeration, by culture of individual colonies on chromogenic agar media, of Salmonella spp. including potentially sub-lethally damaged Salmonella spp. in sewage sludges. It may be suitable for other sludges, soils, soil improvers, growing media and biowastes but the user shall validate the method using these materials.  The fully defined scope will be determined after the proposed validation trials have been agreed and carried out.
NOTE 1   The objective is to cover untreated and treated sludges, soils, soil improvers, growing media and biowastes.
The method is particularly suited to determining the efficiency of treatment procedures for the elimination of pathogens in sewage sludge as outlined in the Revision of Directive 86/278/EEC (3rd Draft, CEN/TC 308 – doc 525). Treatment type A processes are initially to be validated through a to be defined Log10 reduction with a test organism such as Salmonella senftenberg W775.
The method has a limit of detection of approximately 1 cfu/g wet weight sludge, dependent on the solids content which at high concentrations (> 20 % (w/v)) can restrict filtration of the sample volume through the membrane if not first diluted.
NOTE 2   Salmonella spp. can be present in biosolids including untreated and treated sewage sludge as both vegetative and sub-lethally damaged cells; the latter require resuscitation to enable colony growth for accurate enumeration on agar media.
NOTE 3   This method is not suitable for treated sludges containing less than 1 viable Salmonella spp. per 1 g wet weight.
NOTE 4   This method is not suitable for untreated sludges containing low levels of Salmonella.

This part of the CEN Technical Report describes a miniaturized most probable number (MPN) method for the quantitative detection of Escherichia coli in sludges, soils, soil improvers, growing media and biowastes. It is suitable to evaluate the log reduction of E. coli through treatment as well as the quality of the end product.
This method is convenient for material with dry residue of more than 10 %. For materials with dry residue less than 20 %, the procedure specified in CEN/TR 15214-1 will be used.

This part of the CEN Technical Report specifies a most probable number (MPN) method for the quantitative detection of Escherichia coli in sludges, soils, soil improvers, growing media and biowastes. It allows further differentiation within the test than part 2 of this standard. It is suitable to evaluate the log reduction of E.coli through treatment as well as the quality of the end product.
The method is for material with dry residues of more than 10 %.
For materials with dry residues less than 10 %, the procedure given in CEN/TR 15214-1 should be used.

This part of the CEN Technical Report method describes a method to detect and semi-quantitatively determine Salmonellae in sludges, soils, soil improvers, growing media and biowastes in accordance with the requirements of the European Sewage Sludge Regulation Revision of Directive 86/278/EEC (3rd Draft, CEN/TC 308 - doc525).
The fully defined scope will be determined after the proposed validation trials have been agreed and carried out. The method has a limit of detection of approximately 1cfu/g wet weight sample.
NOTE   The objective is to cover untreated and treated sludges, soils, soil improvers, growing media, biowastes and associated materials.

This part of the CEN Technical Report specifies a presence/absence procedure to detect Salmonella spp using a four-stage presence/absence method in up to 50g (wet weight) sample.
The method has a limit of detection of approximately 10 cfu/50 g wet weight sludge.
NOTE   The objective is to cover untreated and treated sludges, soils, soil improvers, growing media and biowastes.

This part of the CEN Technical Report specifies a membrane filtration procedure for the quantitative detection, by culture of individual colonies on chromogenic agar media, of Escherichia coli. in sludges, soils, soil improvers, growing media and biowastes. This part of the Technical Report is not suitable for materials whose treatment will significantly reduce bacterial levels to less than 10 viable E. coli per g wet weight, such as lime addition, drying or pasteurisation. A liquid enrichment and most probable number estimation method may be suited for such purpose.
This membrane filtration method is not appropriate for enumeration and detection of other coliform bacteria without modifications to the chromogenic agar media.
It is suitable to evaluate the log reduction of E.coli through treatment, as well as the quality of the end product.
This method is for materials with dry residues less than 20 %. For materials with dry residues greater than 20 % and low numbers of E. coli,  CEN/TR 15214-2 and CEN/TR 15214-3  should be used.

This European Standard describes an empirical method for the direct determination of an amount ranging from 5 mg/kg to approximately 6 g/kg dry matter in sludge of organically bound chlorine, bromine and iodine (but not fluorine) adsorbed and occluded to the sludge matrix. Non-volatile organically bound halogens adsorbable on activated carbon present in the aqueous phase of sludge prior to drying are included in the determination.
NOTE   The upper range of the method is instrument dependent.

This European Standard specifies a method for the determination of drainability of flocculated sludges. It is applicable to sludge and sludge suspensions from:
a)   storm water handling;
b)   urban wastewater collecting systems;
c)   urban wastewater treatment plants;
d)   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
e)   water supply treatment plants.
This method is also applicable to sludge suspensions from other origin.

ISO 23161:2009 specifies a gas-chromatographic method for the identification and quantification of organotin compounds (OTCs) in soils as specified in Table 1. The method is also applicable to samples from sediments, sludges and wastes (soil-like materials). The working range depends on the detection technique used and the amount of sample taken for analysis. The limit of quantification for each compound is about 10 µg/kg.
Organotin cations can only be determined in accordance with ISO 23161:2009 after derivatization. The anionic part bound to the organotin cation is mainly dependent on the chemical environment and is not determined using this method. The peralkylated organotin compounds behave in a completely different way from their parent compounds. Tetraalkylated organotin compounds which are already peralkylated, such as tetrabutyltin, are determined directly without derivatization.

This Technical Report specifies a procedure for the chemical conditioning in laboratory of sludges.
This Technical Report is applicable to sludges and sludge suspensions from:
-   storm water handling;
-   urban wastewater collecting systems;
-   urban wastewater treatment plants;
-   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
-   water supply treatment plants.
This method is applicable to sludge and sludge suspensions of other origin

This European Standard specifies a method for the determination of the loss on ignition of dry mass of sludges and sludge products at 550 °C after the dry residues have been determined in accordance with the method of EN 12880. NOTE It should be noted that inorganic substances or decomposition products (e.g. H2O, CO2, SO2, O2) are released or absorbed and some inorganic substances are volatile under the reaction conditions.

This standard specifies methods for the extraction, with aqua regia, of trace elements and phosphorus from sludges and sludge products. The resulting solution is suitable for the determination of As, Cd, Cr, Cu, Hg, Ni, Pb, Se, Zn and P using spectrometric techniques. NOTE 1 With high solute concentrations in extract solutions, spectral interferences and background enhancement should be expected. NOTE 2 This method can be used for other elements except that portion of the elements bonded to silica.

The scope of this standard is the sludges, i.e. and sludges products from: - storm water handling; - night soil; - urban wastewater collecting systems; - urban wastewater treatment plants; - treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271 EEC); - water supply treatment plants; - water distribution systems; - but excluding hazardous sludges from industry.

This document specifies a method for determining the specific resistance to filtration of sludges, conditioned or non-conditioned.
This document is applicable to sludges and sludge suspensions from:
   storm water handling;
   urban wastewater collecting systems;
   urban wastewater treatment plants;
   treating industrial wastewater similar to urban wastewater (as defined in Directive 91/271/EEC);
   water supply treatment plants;
This method is also applicable to sludge and sludge suspensions of other origins.

Migrated from Progress Sheet (TC Comment) (2000-07-10): ISO/CD 5667-13 ISO Lead