SIST-TP CEN/TR 15175:2006

Characterization of sludges - Protocol for organizing and conducting inter-laboratory tests of methods for chemical and microbiological analysis of sludges

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

Charakterisierung von Schlämmen - Protokoll zur Durchführung von Ringversuchen für Verfahren zur chemischen, mikrobiologischen und physikalischen Analyse von Schlämmen

Caractérisation des boues - Protocole d'exécution d'essais interlaboratoires portant sur des méthodes d'analyses chimiques et microbiologiques des boues

Karakterizacija blata – Protokol za organiziranje in vodenje medlaboratorijskih preskušanj metod za kemijske in mikrobiološke analize blata

General Information

• Status: Published
• Publication Date: 30-Jun-2006
• ICS: 13.030.20 - Liquid wastes. Sludge
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Jul-2006
• Due Date: 01-Jul-2006
• Completion Date: 01-Jul-2006
• Ref Project: CEN/TR 15175:2006 - Characterization of sludges - Protocol for organizing and conducting inter-laboratory tests of methods for chemical and microbiological analysis of sludges

Overview

SIST-TP CEN/TR 15175:2006 is a Technical Report developed by the European Committee for Standardization (CEN) providing a protocol for organizing and conducting inter-laboratory tests of methods for chemical and microbiological analysis of sludges. This standard is crucial for ensuring the reliability and accuracy of analytical methods used in sludge characterization, promoting harmonization across laboratories in different countries. It defines the requirements and best practices for interlaboratory testing aimed at validating chemical and microbiological analytical procedures for various sludge types.

Key Topics

• Interlaboratory Test Planning
  Specifies key variables such as organizing laboratory, sample types and quantities, spiking protocols, statistical calculations, and deadlines for test completion.

• Sample Preparation and Homogeneity
  Emphasizes the necessity of homogeneous bulk sludge samples and provides guidance for sample preservation, labeling, and shipment under controlled temperatures (below 4 °C).

• Lab Participation Criteria
  Laboratories should have demonstrable experience with sludge analysis and agree to strictly follow the prescribed method and timelines.

• Testing Protocol and Documentation
  Details the process for sample dispatch, courier arrangements with 24-hour guaranteed delivery, chain-of-custody maintenance, and documentation including detailed instructions, spiking materials, and result submission forms.

• Statistical Analysis
  Follows ISO 5725 for evaluation of precision and accuracy, including outlier detection and reproducibility assessments to ensure confidence in test results.

• Reporting
  Requires a comprehensive final report covering all data collected, including sample temperatures at receipt, reproducibility, repeatability, recovery rates, and lab participation details-all with anonymity preserved.

• Special Protocols for Sample Preparation Methods
  Annex A discusses managing methods focused solely on sample preparation, such as aqua regia digestion, to separate preparation errors from measurement errors.

• Participant Agreement
  Annex B provides a formal agreement template ensuring participant laboratories commit to compliance, enabling coordinated and effective testing.

Applications

SIST-TP CEN/TR 15175:2006 is vital for:

• Environmental Laboratories performing routine sludge chemical and microbiological analyses for regulatory compliance and environmental monitoring.

• Method Validation Programs where new or updated sludge analysis methods require standardized interlaboratory testing prior to official publication or adoption.

• Sludge Treatment Facilities and Waste Management Authorities leveraging validated analytical protocols to assess sludge quality, treatment performance, and safety.

• Research & Development efforts aiming to develop or improve analytical methods for diverse sludge matrices, ensuring comparability of results across multiple testing sites.

• Quality Assurance frameworks requiring objective statistical evaluation of analytical accuracy, reproducibility, and laboratory proficiency.

Related Standards

• ISO 5725 - Accuracy (trueness and precision) of measurement methods and results. This ISO standard underpins the statistical approaches for interlaboratory test evaluations specified in CEN/TR 15175.

• Other CEN standards related to sludge characterization and environmental sampling may complement this technical report to provide a comprehensive quality and method validation system.

---

By adhering to SIST-TP CEN/TR 15175:2006, laboratories and organizations involved in sludge analysis can ensure consistent, robust, and internationally harmonized chemical and microbiological data, enhancing method validation and environmental compliance outcomes. This contributes significantly to the effective management of sludge treatment and disposal processes while supporting regulatory frameworks across Europe and beyond.

Standards Content (Sample)

SLOVENSKI STANDARD
01-julij-2006
Karakterizacija blata – Protokol za organiziranje in vodenje medlaboratorijskih
preskušanj metod za kemijske in mikrobiološke analize blata
Characterization of sludges - Protocol for organizing and conducting inter-laboratory
tests of methods for chemical and microbiological analysis of sludges
Charakterisierung von Schlämmen - Protokoll zur Durchführung von Ringversuchen für
Verfahren zur chemischen, mikrobiologischen und physikalischen Analyse von
Schlämmen
Caractérisation des boues - Protocole d'exécution d'essais interlaboratoires portant sur
des méthodes d'analyses chimiques et microbiologiques des boues
Ta slovenski standard je istoveten z: CEN/TR 15175:2006
ICS:
13.030.20
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 15175
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
March 2006
ICS 13.030.20
English Version
Characterization of sludges - Protocol for organizing and
conducting inter-laboratory tests of methods for chemical and
microbiological analysis of sludges
Caractérisation des boues - Protocole d'exécution d'essais Charakterisierung von Schlämmen - Protokoll zur
interlaboratoires portant sur des méthodes d'analyses Durchführung von Ringversuchen für Verfahren zur
chimiques et microbiologiques des boues chemischen, mikrobiologischen und physikalischen
Analyse von Schlämmen
This Technical Report was approved by CEN on 30 September 2005. It has been drawn up by the Technical Committee CEN/TC 308.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15175:2006: E
worldwide for CEN national Members.

Contents Page
Foreword.3
Introduction .4
1 Scope .5
2 Planning protocol .5
3 Interlaboratory test protocol issues .5
4 Interlaboratory test procedure .6
5 Final report of the test.7
6 Other comments .8
Annex A (informative) Proposed protocol for sample preparation methods.9
Annex B (informative) Agreement to participate in the ……………………. sludge method
interlaboratory validation test .10
Bibliography .11

Foreword
This Technical Report (CEN/TR 15175:2006) 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.

Introduction
For international harmonization it is essential that a fit for purpose interlaboratory test using a range of typical
sludges with relevant analyte concentrations be carried out prior to proposing for publication any method as a
Technical Report.
At least ten laboratories from three different countries should participate in this test.
Only experienced laboratories routinely carrying out sludge analysis should participate.
The organizer should aim for 12 to 15 laboratories to participate in each test in as many countries as possible.
Efforts are needed to ensure that there is a minimum of intersample variation amongst the circulated samples.
It is recommended that each test includes a range of sludges that is representative of the proposed scope of
the method, as a minimum this should include an untreated (raw) sludge, a treated (an aerobically digested)
sludge, a presscake and samples of any other sludges relevant to the method being tested. In addition a
spiking solution and a calibration check standard will generally be distributed.
If possible, samples should be in the same form as would normally be submitted to a laboratory for analysis.
For sample preparation methods without a final measurement stage (e.g. Aqua regia digestion for metal
analysis), see Annex A.
1 Scope
This Technical Report specifies the requirements for interlaboratory tests to validate chemical and
microbiological methods for sludges.
2 Planning protocol
The main test variables to be agreed are:
a) organising laboratory;
b) documented method to be tested;
c) number and nature of the samples;
d) statistical calculations including rejection of outliers;
e) deadlines for sending out samples, receipt of results from participants and final test report from the
organizer;
f) spiking protocol to calculate recovery;
g) analysis of a calibration check standard. It will also allow a check to be made on the comparative
accuracy of the calibration standards used by all the participants. This can sometimes explain differences
between laboratories).
3 Interlaboratory test protocol issues
3.1 Test organiser and dispatch of samples
It is essential that the bulk material is homogeneous. This should be checked using a suitable low cost
parameter (e.g. Cu, Zn).
The organizer will compile a test contact list with:
a) contact name;
b) contact full address;
c) contact phone numbers (named contact and switchboard);
d) contact fax number;
e) contact E-mail address.
The organizer will obtain a written statement (see Annex B) from each laboratory agreeing to participate,
agreeing to follow the provided method exactly and meet the deadlines for start and completion of analysis
and for submission of the results on the appropriate form.
An additional 20 % of samples shall be prepared and held by the organizer at –18 °C or less. These can be
used if any problems are encountered during the test. For microbiology this may not be appropriate.
3.2 Participating laboratories
Participating laboratories should be laboratories that routinely carry out sludge analysis.
3.3 Statistical calculations
An initial check should be made to confirm a normal distribution of results. If the distribution is not normal then
appropriate robust statistics should be employed.
Assuming a normal distribution, the statistical calculations should be carried out according to ISO 5725 by a
suitably experienced person for chemical parameters.
Suitable rejection procedures should be used for microbiological parameters.
Rejection of outliers should also follow ISO 5725. All Type B (reproducibility) outliers should be eliminated.
All Type C outliers from the mean of one lab (repeatability) should be included.
In addition the elimination of ‘obvious’ outliers by the statistical organizer (Type D) shall be allowed as long as
they are fully documented with the reason for elimination.
Each sample shall be analysed in replicate (x times) on y separate days (x and y to be agreed for each
individual t
...