Characterization of sludges - Protocol for preparing synthetic suspensions

Fresh sludges are unsuitable for circulation of samples for interlaboratory trials. The circulation of analysts is needed for standards validation dealing with physical properties of sludges.
For purposes of comparison and reproductibility, it would be useful to have a European reference for organic synthetic suspension. Elaborating such a standard aims at having an alternative to fresh sludges because :
- Sludge characteristics change with storage time
- Sludge characteristics are strongly affected by transport and handling
- Fresh sludges require particular precautions and authorization for transportation
Aerobic sludge first targeted ; potentially: anaerobic sludges, physico-chemical sludges, water supply treatment sludges ; potentially inorganic sludges (sediments)

Charakterisierung von Schlämmen - Protokoll zur Herstellung synthetischer Suspensionen

Dieser Technische Bericht befasst sich mit den Verfahrensweisen bei der Herstellung synthetischer Suspensionen. Synthetische Suspensionen können eingesetzt werden für:
a)   die Bewertung oder Prüfung neuer Geräte oder Techniken zur Behandlung von Suspensionen;
b)   das Studium des Einflusses von verschiedenen Verbindungen auf das Suspensionsverhalten in Bezug auf bestimmte Parameter, z. B. Absetzbarkeit, Entwässerbarkeit, physikalische Konsistenz usw.
Die chemischen, physikalischen und biologischen Eigenschaften von Suspensionen sind Veränderungen unterworfen, sobald deren Probenahme erfolgt. Es gibt Anleitungen zur Probenahme und zu Handhabungstechniken (siehe ISO 5667 12 und EN ISO 5667 13) und zu Verfahren der Konservierung und Lagerung (EN ISO 5667 15), die mithelfen, die Veränderungen in der Zusammensetzung zu verringern. Hauptsächlich wird das durch Unterdrückung der chemischen und/oder biologischen Aktivität sowie durch Vermeiden von Kontamination erreicht.

Caractérisation des boues - Protocole de préparation de suspensions synthétiques

Le présent Rapport technique traite des méthodologies de préparation de suspensions synthétiques. Les suspensions synthétiques peuvent être utilisées pour :
a)   évaluer ou soumettre à essai de nouveaux dispositifs ou de nouvelles techniques de traitement des suspensions ;
b)   étudier l'influence des différents composés sur le comportement des suspensions selon certains paramètres spécifiques tels que la décantation, la déshydratation, la consistance physique, etc.
Les caractéristiques chimiques, physiques et biologiques des suspensions sont sujettes à variations dès le prélèvement. Les lignes directrices existantes en matière de techniques d'échantillonnage et de manipulation (voir l’ISO 5667-12 et l’EN ISO 5667-13), et de modes opératoires de conservation et de stockage (EN ISO 5667-15) visent à réduire au maximum les variations de composition. Pour y parvenir, il faut avant tout supprimer toute activité chimique et/ou biologique et éviter la contamination.

Karakterizacija blata - Protokol za pripravo sintetičnih suspenzij

Sveže blato ni primerno za izmenjavo vzorcev za medlaboratorijske poskuse. Izmenjava analitikov je potrebna za potrjevanje standardov, ki obravnavajo fizične lastnosti blata.
Za namene primerjave in ponovljivosti bi bila uporabna evropska referenca za organsko sintetično suspenzijo. Cilj takšnega standarda je določitev alternative svežemu blatu, saj:
– se značilnosti blata med skladiščenjem spremenijo;
– transport in delo/ravnanje z blatom močno vplivata na njegove značilnosti;
– sta pri transportu svežega blata potrebna posebna previdnost in dovoljenje.
Aerobno blato (prva obdelava), potencialno: anaerobno blato, fizikalno-kemijsko blato, blato v sistemih oskrbe z vodo; potencialno neorgansko blato (usedline).

General Information

Status
Published
Public Enquiry End Date
31-May-2012
Publication Date
18-Jan-2015
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
16-Dec-2014
Due Date
20-Feb-2015
Completion Date
19-Jan-2015

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SLOVENSKI STANDARD
SIST-TP CEN/TR 16394:2015
01-februar-2015
.DUDNWHUL]DFLMDEODWD3URWRNRO]DSULSUDYRVLQWHWLþQLKVXVSHQ]LM
Characterization of sludges - Protocol for preparing synthetic suspensions
Charakterisierung von Schlämmen - Protokoll zur Herstellung synthetischer
Suspensionen
Caractérisation des boues - Protocole de préparation de suspensions synthétiques
Ta slovenski standard je istoveten z: CEN/TR 16394:2014
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
SIST-TP CEN/TR 16394:2015 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 16394:2015
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SIST-TP CEN/TR 16394:2015
TECHNICAL REPORT
CEN/TR 16394
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
November 2014
ICS 13.030.20
English Version
Characterization of sludges - Protocol for preparing synthetic
suspensions

Caractérisation des boues - Protocole de préparation de Charakterisierung von Schlämmen - Protokoll zur

suspensions synthétiques Herstellung synthetischer Suspensionen

This Technical Report was approved by CEN on 18 August 2014. It has been drawn up by the Technical Committee CEN/TC 308.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United

Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16394:2014 E

worldwide for CEN national Members.
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Contents Page

Foreword ..............................................................................................................................................................3

Introduction .........................................................................................................................................................4

1 Scope ......................................................................................................................................................5

2 Normative references ............................................................................................................................5

3 Terms and definitions ...........................................................................................................................5

4 Preparation of inorganic synthetic suspensions ...............................................................................5

4.1 General ....................................................................................................................................................5

4.2 Materials .................................................................................................................................................5

4.3 Modalities of preparation ......................................................................................................................6

5 Preparation of organic synthetic suspensions ..................................................................................7

5.1 General ....................................................................................................................................................7

5.1.1 General ....................................................................................................................................................7

5.1.2 Materials .................................................................................................................................................7

5.1.3 Modalities of preparation ......................................................................................................................8

5.2 Preparation of organic synthetic suspensions by concentration of synthetic waters ..................9

Annex A (informative) Example of composition of activated suspension and its evolution over

storage time ......................................................................................................................................... 10

Bibliography ..................................................................................................................................................... 11

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CEN/TR 16394:2014 (E)
Foreword

This document (CEN/TR 16394:2014) has been prepared by Technical Committee CEN/TC 308

“Characterization of sludges”, the secretariat of which is held by AFNOR.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

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CEN/TR 16394:2014 (E)
Introduction

In order to carry out lab-scale tests of suspensions, and interlaboratory validation trials for standardized

methods, it is necessary to have samples with constant characteristics available. When dried suspension

samples cannot be used and testing requires fresh sludge samples, problems arise because:

a) most suspension characteristics change over time, which makes them unfit for storage;

b) some preservation practices (e.g. freezing) are not applicable, or their effects unknown;

c) some suspension characteristics are strongly affected by handling;
d) transporting sludge samples requires special precautions and authorization.

This means that fresh suspension samples cannot be used to guarantee results reliability and reproducibility.

As a consequence, fresh suspension samples should be examined by laboratories very close to wastewater

or waterworks plants and analysed as soon as possible, minimizing their manipulation. As a result, the

circulation of fresh suspension samples to laboratories in several countries is analytically not feasible.

Interlaboratory analysis on these suspensions should be carried out through circulation of analysts, close to

the place where samples are collected according to the Modified Round Robin tests procedure

(CEN/TR 15252).
A valid alternative is the creation and testing of synthetic suspensions.

Synthetic suspensions are prepared on-site on the basis of a defined recipe and specified ingredients. This

will also allow the comparison of results obtained from different places, at different times.

This Technical Report establishes methods for preparing synthetic suspensions, both inorganic and organic,

in repeatable and quantified conditions, able to describe the behaviour of a real suspension with regard to

specific parameters, and suitable for circulation as samples in interlaboratory trials for validation of standards

when fresh suspensions cannot be used. It represents the state of the art of the available knowledge on

synthetic suspensions.
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1 Scope

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.
2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated references,

the latest edition of the referenced document (including any amendments) applies.

EN 12832:1999, Characterization of sludges - Utilization and disposal of sludges - Vocabulary

EN ISO 17353, Water quality - Determination of selected organotin compounds - Gas chromatographic

method (ISO 17353)
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 12832:1999 apply.

4 Preparation of inorganic synthetic suspensions
4.1 General

The procedure specified in this Technical Report refers to the preparation of inorganic synthetic suspensions

to simulate the behaviour of real inorganic suspensions. Inorganic suspensions produced by waterworks

plants exhibit wide variations in their physical and chemical properties due to the raw water differences and

the design and operation of each individual treatment plant. Many different products could be used for

preparation of such suspensions depending on the properties to be evaluated.

Quartz sand, calcite and kaolin are the three most commonly used minerals in large industrial sectors. Hence,

a combination of these three minerals is perfectly suited to simulate the behaviour of real inorganic

suspensions. Role and characteristics of such materials have been discussed in [6] and [7].

4.2 Materials

Primary particle properties, such as particle shape, size distribution, specific surface area, density, surface

structure, dry bed porosities, as well as their dispersion properties, for example solid concentration, or pH,

have a strong influence on the physical properties of inorganic suspensions (e.g. compressibility, settleability,

specific resistance), which have to be known and defined for a standardized synthetic suspension.

Table 1 gives an example of the main characteristics of kaolin, calcite, and quartz sand [6].

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Table 1 — Characteristics of materials composing inorganic synthetic suspension
Kaolin Calcite Quartz sand
Average particle size (µm) 5 10 20
Crystal structure monoclinic rhombohedric tetragonal
Specific surface area (m /g) 9 3 2
Dry bed porosity (tapped-poured) 0,6 to 0,7 0,5 to 0,6 0,4 to 0,5
Density (g/cm ) 2,60 2,70 2,65
SiO (%) 46 2 99
Al O (%) 39 0,4 0,2
2 3
Fe O (%) 0,2 < 0,1 0,3
2 3
CaO (%) 1 55 0,1
MgO (%) 0,1 2 0,1
K O (%) < 0,1 < 0,1 < 0,1
Na O (%) 0,2 1 0,1
Loss on ignition (%) 13 39 < 0,1
Compressibility range 0,7 to 1,1 0,2 to 0,3 0,1 to 0,2

Only binary mixtures can be used for evaluation of specific parameters. For example, mixtures of kaolin (75 %

to 90 %) and quartz sand were used for rheological measurements [8]. Suppliers of polymers prefer using

mixtures of kaolin (30 g/l to 100 g/l) and calcium chloride (0,5 g/l to 1,65 g/l) to prepare inorganic synthetic

suspensions which easily flocculate both with anionic and cationic polymers.

For ternary mixtures, comparison tests were performed on a 30 g/l industrial suspension sampled at a

granulate extraction plant.

Reasonably good compliance in terms of settleability, capillary suction time (CST), specific resistance,

compressibility and suspension dryness (after compression) was achieved using a synthetic suspension

consisting of 90 % kaolin, 5 % quartz sand and 5 % calcite [9].
4.3 Modalities of preparation

Ingredients are kaolin, quartz sand and/or calcite which can be mixed in different proportions to be fixed for

the development of a standard inorganic suspension.

The suspensions have to be prepared from mineral powders before the start of each set of experiments in

order to avoid modification of surface properties of powders. All samples shall be prepared in the same way

because the preparation has a significant influence on the final state of the suspension (degree of dispersity,

rheological behaviour).
A good preparation of inorganic synthetic suspension usually requires:
— fine particles and narrow particle size distribution to ensure homogeneity;

— a defined proportion of ingredients, whose respective weights should be adjusted to prepare the

suspension of chosen concentration;

— a defined quality (e.g. pH, turbidity, conductivity, alkalinity, hardness) of water for suspension preparation

as defined for example in EN ISO 17353;
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