ISO 5667-14:2014

Water quality — Sampling — Part 14: Guidance on quality assurance and quality control of environmental water sampling and handling

ISO 5667-14:2014 provides guidance on the selection and use of various quality assurance and quality control techniques relating to the manual sampling of surface, potable, waste, marine and ground waters. NOTE The general principles outlined in this part of ISO 5667 might, in some circumstances, be applicable to sludge and sediment sampling.

Qualité de l'eau — Échantillonnage — Partie 14: Lignes directrices sur l'assurance qualité et le contrôle qualité pour l'échantillonnage et la manutention des eaux environnementales

ISO 5667-14:2014 fournit des lignes directrices sur le choix et l'utilisation de différentes techniques d'assurance qualité et de contrôle qualité liées à l'échantillonnage manuel des eaux de surface, potables, résiduaires, marines et souterraines. NOTE Dans certains cas, les principes généraux exposés dans la présente partie de l'ISO 5667 peuvent s'appliquer à l'échantillonnage de boues et de sédiments.

Kakovost vode - Vzorčenje - 14. del: Navodilo za zagotavljanje in kontrolo kakovosti vzorčenja vode v okolju ter ravnanje z vzorci

Ta del standarda ISO 5667 ponuja načela glede izbire in uporabe različnih tehnik za zagotavljanje in kontrolo kakovosti, ki so povezane z ročnim vzorčenjem površinske, pitne, odpadne in morske vode ter podtalnice.
OPOMBA Splošna načela, opisana v tem delu standarda ISO 5667 lahko v nekaterih okoliščinah veljajo za vzorčenje blata in usedlin.

General Information

• Status: Published
• Publication Date: 11-Dec-2014
• ICS: 13.060.45 - Examination of water in general
• Technical Committee: ISO/TC 147/SC 6 - Sampling (general methods)
• Drafting Committee: ISO/TC 147/SC 6/WG 1 - Sampling management
• Current Stage: 9093 - International Standard confirmed
• Completion Date: 04-Mar-2020
• Ref Project: SIST ISO 5667-14:2015 - Water quality - Sampling - Part 14: Guidance on quality assurance and quality control of environmental water sampling and handling

Relations

• Revises: ISO 5667-14:1998 - Water quality — Sampling — Part 14: Guidance on quality assurance of environmental water sampling and handling
• Effective Date: 24-Oct-2009

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 5667-14
Second edition
2014-12-15
Water quality — Sampling —
Part 14:
Guidance on quality assurance and
quality control of environmental
water sampling and handling
Qualité de l’eau — Échantillonnage —
Partie 14: Lignes directrices pour le contrôle de la qualité dans
l’échantillonnage et la manutention des eaux environnementales
Reference number
ISO 5667-14:2014(E)
ISO 2014
---------------------- Page: 1 ----------------------
ISO 5667-14:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 5667-14:2014(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ................................................................................................................................................................................................................................vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Sources of sampling error ........................................................................................................................................................................... 4

5 Sampling quality ................................................................................................................................................................................................... 5

5.1 General ........................................................................................................................................................................................................... 5

5.2 Technical and personnel requirements ............................................................................................................................. 6

5.3 Sampling manual ................................................................................................................................................................................... 6

5.4 Training of sampling staff .............................................................................................................................................................. 7

6 Strategy and organization ........................................................................................................................................................................... 7

6.1 Time, duration and frequency of sampling..................................................................................................................... 7

6.2 Sampling collection locations ..................................................................................................................................................... 8

7 Sample collection and handling ............................................................................................................................................................ 8

7.1 Equipment and vehicle check prior to carrying out a sampling programme ................................... 8

7.2 Preparation for sampling on-site ............................................................................................................................................ 9

7.3 Field measurements ........................................................................................................................................................................... 9

7.4 Taking the samples .............................................................................................................................................................................. 9

8 Sample identification ....................................................................................................................................................................................12

9 Field sample protocol ...................................................................................................................................................................................12

10 Transport and storage of samples ...................................................................................................................................................12

11 Sampling quality control techniques ...........................................................................................................................................13

11.1 General ........................................................................................................................................................................................................13

11.2 Replicate quality control samples .......................................................................................................................................15

11.3 Field blank samples .........................................................................................................................................................................16

11.4 Rinsing of equipment (sampling containers) ............................................................................................................17

11.5 Filtration recovery ............................................................................................................................................................................18

11.6 Technique 1 — Spiked samples .............................................................................................................................................20

11.7 Technique 2 — Spiked environmental samples ......................................................................................................22

12 Analysis and interpretation of quality control data .....................................................................................................22

12.1 Shewhart control charts...............................................................................................................................................................22

12.2 Construction of duplicate control charts .......................................................................................................................23

13 Independent audits.........................................................................................................................................................................................23

[7]

Annex A (informative) Common sources of sampling error ...............................................................................................25

Annex B (informative) Control charts ..............................................................................................................................................................27

Annex C (informative) Sub-sampling using a homogenizer ......................................................................................................31

Bibliography .............................................................................................................................................................................................................................34

© ISO 2014 – All rights reserved iii
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ISO 5667-14:2014(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any

patent rights identified during the development of the document will be in the Introduction and/or on

the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT), see the following URL: Foreword — Supplementary information.

The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 6, Sampling

(general methods).

This second edition cancels and replaces the first edition (ISO 5667-14:1998), which has been

technically revised.

ISO 5667 consists of the following parts, under the general title Water quality — Sampling:

— Part 1: Guidance on the design of sampling programmes
— Part 3: Preservation and handling of water samples
— Part 4: Guidance on sampling from lakes
— Part 5: Guidance on sampling of drinking water
— Part 6: Guidance on sampling of rivers and streams
— Part 7: Guidance on sampling of water and steam in boiler plants
— Part 8: Guidance on sampling of wet deposition
— Part 9: Guidance on sampling from marine waters
— Part 10: Guidance on sampling of waste waters
— Part 11: Guidance on sampling of groundwaters
— Part 12: Guidance on sampling of bottom sediments;
— Part 13: Guidance on sampling of water, waste water and related sludges

— Part 14: Guidance on quality assurance and quality control of environmental water sampling and handling

— Part 15: Guidance on preservation and handling of sludge and sediment samples
iv © ISO 2014 – All rights reserved
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ISO 5667-14:2014(E)
— Part 16: Guidance on biotesting of samples
— Part 17: Guidance on sampling of suspended sediments
— Part 19: Guidance on sampling of marine sediments

— Part 20: Guidance on the use of sampling data for decision making – Compliance with thresholds and

classification systems

— Part 21: Guidance on sampling of drinking water distributed by tankers or means other than

distribution pipes
— Part 22: Guidance on design and installation of groundwater sample points
— Part 23: Guidance on passive sampling in surface waters
© ISO 2014 – All rights reserved v
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ISO 5667-14:2014(E)
Introduction

Sampling is the first step in carrying out chemical, physical and biological examinations. Therefore, the

goal of sampling should be to obtain a representative sample for the research question and to supply it

to the laboratory in the correct manner. Errors caused by improper sampling, sample pre-treatment,

transport and storage cannot be corrected.

This part of ISO 5667 specifies quality assurance and quality control procedures and provides additional

guidance on sampling of the various types of water covered in the specific parts of ISO 5667.

Quality control procedures are necessary for the collection of environmental water samples for the

following reasons:
a) to monitor the effectiveness of sampling methodology;

b) to demonstrate that the various stages of the sample collection process are adequately controlled

and suited to the intended purpose, including adequate control over sources of error such as

sample contamination, loss of determinand and sample instability. To achieve this, quality control

procedures should provide a means of detecting sampling error, and hence a means of rejecting

invalid or misleading data resulting from the sampling process;

c) to quantify and control the sources of error which arise in sampling. Quantification gives a guide to

the significance that sampling plays in the overall accuracy of data; and

d) to provide information on suitably abbreviated quality assurance procedures that might be used for

rapid sampling operations such as pollution incidents or groundwater investigations.

This part of ISO 5667 is one of a group of International Standards dealing with the sampling of waters.

It should be read in conjunction with the other parts of ISO 5667 and in particular with parts 1 and 3.

The general terminology is in accordance with that published.
vi © ISO 2014 – All rights reserved
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INTERNATIONAL STANDARD ISO 5667-14:2014(E)
Water quality — Sampling —
Part 14:
Guidance on quality assurance and quality control of
environmental water sampling and handling

WARNING — Consider and minimize any risks and obey safety rules. See ISO 5667-1 for certain

safety precautions, including sampling from boats and from ice-covered waters.
1 Scope

This part of ISO 5667 provides guidance on the selection and use of various quality assurance and quality

control techniques relating to the manual sampling of surface, potable, waste, marine and ground waters.

NOTE The general principles outlined in this part of ISO 5667 might, in some circumstances, be applicable to

sludge and sediment sampling.
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.

ISO 5667-1:2006, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and

sampling techniques

ISO 5667-3:2012, Water quality — Sampling — Part 3: Preservation and handling of water samples

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
accuracy

closeness of agreement between a test result or measurement result and the true value

Note 1 to entry: In practice, the accepted reference value is substituted for the true value.

Note 2 to entry: The term accuracy, when applied to a set of test or measurement results, involves a combination

of random components and a common systematic error or bias component.
Note 3 to entry: Accuracy refers to a combination of trueness and precision.
[SOURCE: ISO 3534-2:2006, 3.3.1]
3.2
bias

difference between the expectation of the test results or measurement result and a true value

Note 1 to entry: Bias is the total systematic error as contrasted to random error. There may be one or more

systematic error components contributing to the bias. A larger systematic difference from the true value is

reflected by a larger bias value.
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ISO 5667-14:2014(E)

Note 2 to entry: The bias of a measuring instrument is normally estimated by averaging the error of indication

over an appropriate number of repeated measurements. The error of indication is the: “indication of a measuring

instrument minus a true value of the corresponding input quantity”.

Note 3 to entry: In practice, the accepted reference value is substituted for the true value.

[SOURCE: ISO 3534-2:2006, 3.3.2]
3.3
precision

closeness of agreement between independent test/measurement results obtained under stipulated

conditions

Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true value

or the specified value.

Note 2 to entry: The measure of precision is usually expressed in terms of imprecision and computed as a standard

deviation of the test results or measurement results. Less precision is reflected by a larger standard deviation.

Note 3 to entry: Quantitative measures of precision depend critically on the stipulated conditions. Repeatability

conditions and reproducibility conditions are particular sets of extreme stipulated conditions.

[SOURCE: ISO 3534-2:2006, 3.3.4]
3.4
representativeness

extent to which the condition of all the samples taken from the body of water reflects conditions in

water of interest
3.5
blank

observed value obtained when measurement is made on a sample identical to the sample of interest, but

in the absence of the determinand

Note 1 to entry: Deionised water; distilled water can be used as blank samples which are prepared in the laboratory

prior to sampling.
3.6
field blank

container prepared in the laboratory, using reagent water or other blank matrix, and sent with the sampling

personnel for exposure to the sampling environment to verify possible contamination during sampling

[SOURCE: ISO 11074:2005, 4.5.3]
3.7
spike

known quantity of determinand which is added to a sample, usually for the purpose of estimating the

systematic error of an analytical system by means of a recovery exercise
3.8
recovery

extent to which a known, added quantity of determinand in a sample can be measured by an

analytical system

Note 1 to entry: Recovery is calculated from the difference between results obtained from a spiked (3.7) and an

unspiked aliquot of sample and is usually expressed as a percentage.
3.9
control chart

chart on which some statistical measure of a series of samples is plotted in a particular order to steer

the process with respect to that measure and to control and reduce variation

Note 1 to entry: The particular order is usually based on time or sample number order.

2 © ISO 2014 – All rights reserved
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ISO 5667-14:2014(E)

Note 2 to entry: The control chart operates most effectively when the measure is a process variable which is

correlated with an ultimate product or service characteristic.
[SOURCE: ISO 3534-2:2006, 2.3.1]
3.10
Shewhart control chart

control chart with Shewhart control limits intended primarily to distinguish between the variation in

the plotted measure due to random causes and that due to special causes

Note 1 to entry: This could be a chart using attributes (for example, proportion nonconforming) for evaluating a

process, or it could be a chart using variables (for example, average and range) for evaluating a process. Examples are:

a) X-bar chart — the sample means are plotted in order to control the mean value of a variable;

b) R chart — the sample ranges are plotted in order to control the variability of a variable;

c) s chart — the sample standard deviations are plotted in order to control the variability of a variable;

d) s chart — the sample variances are plotted in order to control the variability of a variable;

e) C chart — the number of defectives (per batch, per day, per machine, etc.) is plotted.

[SOURCE: ISO 3534-2:2006, 2.3.2, modified — Note 1 to entry has been added.]
3.11
action limits

control limits between which the statistic under consideration lies with a very high probability when

the process is under statistical control

Note 1 to entry: Action lines are drawn on a control chart to represent action limits.

Note 2 to entry: When the measure plotted lies beyond an action limit, appropriate corrective action is taken

on the process.

Note 3 to entry: These limits are based on the assumption that only 0,3 % of normally distributed results will fall

outside these limits. Such an occurrence would strongly indicate that additional, assignable causes of variation

might be present and that action might be required to identify and reduce them.
[SOURCE: ISO 3534-2:2006, 2.4.4, modified — Note 3 to entry has been added.]
3.12
warning limits

control limits between which the statistic under consideration lies with a high probability when the

process is under statistical control

Note 1 to entry: Warning lines are drawn on a control chart to represent warning limits.

Note 2 to entry: When the value of the statistic plotted lies outside a warning limit, but within the action limit

(3.11), increased supervision of the process, to pre-specified rules, is generally required.

Note 3 to entry: The limits are calculated from the standard deviation of the statistic under consideration of at

least 10 samples. Warning and action control limits are applied to individual sampling results.

[SOURCE: ISO 3534-2:2006, 2.4.3, modified — Note 3 to entry has been added.]
3.13
uncertainty
measurement uncertainty

non-negative parameter characterizing the dispersion of the quantity values being attributed to a

measurand based on the information used

[SOURCE: ISO/IEC Guide 99:2007, 2.26, modified — The notes to entry are not included here.]

© ISO 2014 – All rights reserved 3
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ISO 5667-14:2014(E)
3.14
true value

value which characterizes a quantity or quantitative characteristic perfectly defined in the conditions

which exist when that quantity or quantitative characteristic is considered

Note 1 to entry: The true value of a quantity or quantitative characteristic is a theoretical concept and, in general,

cannot be known exactly.

[SOURCE: ISO 3534-2:2006, 3.2.5, modified — Note 2 to entry is not included here.]

3.15
accepted reference value
value that serves as an agreed-upon reference for comparison
Note 1 to entry: The accepted reference value is derived as:
a) a theoretical or established value, based on scientific principles;

b) an assigned or certified value, based on experimental work of some national or international organization;

c) a consensus or certified value, based on collaborative experimental work under the auspices of a scientific or

technical group;

d) the expectation, i.e. the mean of a specified set of measurements, when a), b) and c) are not available.

[SOURCE: ISO 3534-2:2006, 3.2.7]
4 Sources of sampling error
Sources of sampling errors include the following:
a) Contamination

Contamination can be caused by sampling equipment materials (sampling containers and sample

containers) by cross-contamination between samples and by sample preservation and inappropriate

storage and transport arrangements.
b) Sample instability

The type of sampling vessels and containers used can affect the stability of the determinand between

sampling and analysis due to the inherent instability of the sample itself and the conditions in which

samples are stored and transported.
c) Incorrect preservation

The choice of sampling vessels and containers affects the integrity of the determinand and the

options for preservation which may be available, as detailed in ISO 5667-3.
d) Incorrect sampling

Deviation from the sampling procedure, or the procedure itself, might be a source of error.

e) Sampling from non-homogenized water bodies
f) Sample transportation

Figure 1 illustrates various sources of sampling error: environment, personnel, materials, methods,

preservation and transportation. Further examples of common sources of sampling error are given in

Annex A.
4 © ISO 2014 – All rights reserved
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ISO 5667-14:2014(E)
Figure 1 — Sources of sampling error
5 Sampling quality
5.1 General

A programme to establish sampling quality should be established for every series of sampling, so as to

ensure that data resulting from sampling programmes are both trustworthy and scientifically credible.

Mistakes in any step of the sampling procedure can result in substantial errors within the resulting data.

Laboratories that analyse collected samples usually have rigorous programmes of quality assurance and

quality control (QA/QC) as required by national regulation and conforming to ISO/IEC 17025. However,

such laboratory programmes of QA/QC cannot substitute for the rigorous sampling quality programmes

required for the collection and handling of samples prior to delivery to laboratories for analysis.

Sampling quality programmes comprise all the steps taken to ensure that valid results are produced.

Sampling quality programmes include documented evidence that the individuals who collect samples

are competent and well trained, that appropriate sample collection and sample handling methods were

employed, that equipment were maintained and calibrated, that correct practices were followed and

that records are both complete and secure. It is important to establish a quality assurance programme

and quality control effective for the characterization and reduction of errors. Depending on the objective

(e.g. to check for any contamination of the sample at different points in the sampling procedure, and

identify potential problems), the quality control set up will be different. See Table 1.

Table 1 — Means of quality control for different objectives
Objective Means to implement

Check the absence of contamination Blank environmental, Field blank, Transport blank, Equipment

blank, Filter blank
Calculate the sampling precision Duplicate sample
Check the stability of the sample Spiking

Particular importance should be given to careful measurement of analyses performed on-site and

to correct recording of determinand results. Reference should be made to ISO/TS 13530 regarding

© ISO 2014 – All rights reserved 5
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ISO 5667-14:2014(E)

analytical quality control for water analysis and to ISO 15839 regarding online sensors/analysing

equipment for water.

Since analysing laboratories have expertise regarding QA/QC, it is suggested they be actively involved

in the design and evaluation of sampling quality programmes.
5.2 Technical and personnel requirements

To take a sample correctly, adequate and cleaned equipment [such as sample containers, sampling devices,

filtration equipment, a homogenizer, an intermediate container (funnel, spoon), and measurement

equipment for on-site analysis] should be held in sufficient numbers. Regular maintenance of all

equipment should be guaranteed.

The sampling vehicle and the facility should be equipped in accordance with the requirements for

sampling (laboratory vehicle).

The sampling personnel should have relevant professional training, e.g. completed vocational education

as a chemical laboratory assistant or specialist for waste water engineering. An essential prerequisite

is appropriate initial job-training and regular training of sampling personnel. Participation in internal

and/or external training should be documented (see 5.4).

A regular exchange of information between client, sampling personnel and laboratory personnel

improves the quality of sampling and testing. All the necessary information for a sampling of ensured

[7]
quality should be placed at the sampling personnel’s disposal.
5.3 Sampling manual

5.3.1 For sampling, the general requirements related to the competence of testing and calibration

laboratories should be applied.
[7]

Procedures or operating instructions should be prepared and should include the following issues:

a) sampling (matrix-based);
b) on-site measurement;
c) pre-treatment of samples;
d) preservation of samples (parameter-based);
e) sample transport, storage and sample delivery/reception.

Each person responsible for collecting water samples should carry an up-to-date sampling manual on-

site. This manual should provide specific guidance regarding the sampling methods to be employed,

sample handling and preservation, analytical methods for measurements to be performed at the

sampling site, procedures to be followed when transporting samples to the laboratory and method

details pertaining to any online continuous sensor type equipment to be utilized. It is suggested that

the sampling manual should additionally detail all quality assurance procedures to be employed when

collecting samples, when taking on-site measurements, when transporting samples to laboratory and

when using or checking continuous monitoring equipment.
5.3.2 The sampling manual should specify:

a) the types of bottles or containers, their closures and the specific purposes for which they are to be used;

b) where relevant, the cleaning procedure and shelf life for bottles, containers and closures used for

each parameter, including the amount and type of preservative to be added (e.g. first draw, flushed,

stagnation) and the procedure for coll
...

SLOVENSKI STANDARD
SIST ISO 5667-14:2015
01-marec-2015
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SIST ISO 5667-14:1999
.DNRYRVWYRGH9]RUþHQMHGHO1DYRGLOR]D]DJRWDYOMDQMHLQNRQWUROR
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Water quality - Sampling - Part 14: Guidance on quality assurance and quality control of

environmental water sampling and handling

Qualité de l'eau - Échantillonnage - Partie 14: Lignes directrices pour le contrôle de la

qualité dans l'échantillonnage et la manutention des eaux environnementales
Ta slovenski standard je istoveten z: ISO 5667-14
ICS:
13.060.10 Voda iz naravnih virov Water of natural resources
13.060.45 Preiskava vode na splošno Examination of water in
general
SIST ISO 5667-14:2015 en

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

---------------------- Page: 1 ----------------------
SIST ISO 5667-14:2015
---------------------- Page: 2 ----------------------
SIST ISO 5667-14:2015
INTERNATIONAL ISO
STANDARD 5667-14
Second edition
2014-12-15
Water quality — Sampling —
Part 14:
Guidance on quality assurance and
quality control of environmental
water sampling and handling
Qualité de l’eau — Échantillonnage —
Partie 14: Lignes directrices pour le contrôle de la qualité dans
l’échantillonnage et la manutention des eaux environnementales
Reference number
ISO 5667-14:2014(E)
ISO 2014
---------------------- Page: 3 ----------------------
SIST ISO 5667-14:2015
ISO 5667-14:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 5667-14:2015
ISO 5667-14:2014(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ................................................................................................................................................................................................................................vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Sources of sampling error ........................................................................................................................................................................... 4

5 Sampling quality ................................................................................................................................................................................................... 5

5.1 General ........................................................................................................................................................................................................... 5

5.2 Technical and personnel requirements ............................................................................................................................. 6

5.3 Sampling manual ................................................................................................................................................................................... 6

5.4 Training of sampling staff .............................................................................................................................................................. 7

6 Strategy and organization ........................................................................................................................................................................... 7

6.1 Time, duration and frequency of sampling..................................................................................................................... 7

6.2 Sampling collection locations ..................................................................................................................................................... 8

7 Sample collection and handling ............................................................................................................................................................ 8

7.1 Equipment and vehicle check prior to carrying out a sampling programme ................................... 8

7.2 Preparation for sampling on-site ............................................................................................................................................ 9

7.3 Field measurements ........................................................................................................................................................................... 9

7.4 Taking the samples .............................................................................................................................................................................. 9

8 Sample identification ....................................................................................................................................................................................12

9 Field sample protocol ...................................................................................................................................................................................12

10 Transport and storage of samples ...................................................................................................................................................12

11 Sampling quality control techniques ...........................................................................................................................................13

11.1 General ........................................................................................................................................................................................................13

11.2 Replicate quality control samples .......................................................................................................................................15

11.3 Field blank samples .........................................................................................................................................................................16

11.4 Rinsing of equipment (sampling containers) ............................................................................................................17

11.5 Filtration recovery ............................................................................................................................................................................18

11.6 Technique 1 — Spiked samples .............................................................................................................................................20

11.7 Technique 2 — Spiked environmental samples ......................................................................................................22

12 Analysis and interpretation of quality control data .....................................................................................................22

12.1 Shewhart control charts...............................................................................................................................................................22

12.2 Construction of duplicate control charts .......................................................................................................................23

13 Independent audits.........................................................................................................................................................................................23

[7]

Annex A (informative) Common sources of sampling error ...............................................................................................25

Annex B (informative) Control charts ..............................................................................................................................................................27

Annex C (informative) Sub-sampling using a homogenizer ......................................................................................................31

Bibliography .............................................................................................................................................................................................................................34

© ISO 2014 – All rights reserved iii
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SIST ISO 5667-14:2015
ISO 5667-14:2014(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any

patent rights identified during the development of the document will be in the Introduction and/or on

the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT), see the following URL: Foreword — Supplementary information.

The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 6, Sampling

(general methods).

This second edition cancels and replaces the first edition (ISO 5667-14:1998), which has been

technically revised.

ISO 5667 consists of the following parts, under the general title Water quality — Sampling:

— Part 1: Guidance on the design of sampling programmes
— Part 3: Preservation and handling of water samples
— Part 4: Guidance on sampling from lakes
— Part 5: Guidance on sampling of drinking water
— Part 6: Guidance on sampling of rivers and streams
— Part 7: Guidance on sampling of water and steam in boiler plants
— Part 8: Guidance on sampling of wet deposition
— Part 9: Guidance on sampling from marine waters
— Part 10: Guidance on sampling of waste waters
— Part 11: Guidance on sampling of groundwaters
— Part 12: Guidance on sampling of bottom sediments;
— Part 13: Guidance on sampling of water, waste water and related sludges

— Part 14: Guidance on quality assurance and quality control of environmental water sampling and handling

— Part 15: Guidance on preservation and handling of sludge and sediment samples
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— Part 16: Guidance on biotesting of samples
— Part 17: Guidance on sampling of suspended sediments
— Part 19: Guidance on sampling of marine sediments

— Part 20: Guidance on the use of sampling data for decision making – Compliance with thresholds and

classification systems

— Part 21: Guidance on sampling of drinking water distributed by tankers or means other than

distribution pipes
— Part 22: Guidance on design and installation of groundwater sample points
— Part 23: Guidance on passive sampling in surface waters
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Introduction

Sampling is the first step in carrying out chemical, physical and biological examinations. Therefore, the

goal of sampling should be to obtain a representative sample for the research question and to supply it

to the laboratory in the correct manner. Errors caused by improper sampling, sample pre-treatment,

transport and storage cannot be corrected.

This part of ISO 5667 specifies quality assurance and quality control procedures and provides additional

guidance on sampling of the various types of water covered in the specific parts of ISO 5667.

Quality control procedures are necessary for the collection of environmental water samples for the

following reasons:
a) to monitor the effectiveness of sampling methodology;

b) to demonstrate that the various stages of the sample collection process are adequately controlled

and suited to the intended purpose, including adequate control over sources of error such as

sample contamination, loss of determinand and sample instability. To achieve this, quality control

procedures should provide a means of detecting sampling error, and hence a means of rejecting

invalid or misleading data resulting from the sampling process;

c) to quantify and control the sources of error which arise in sampling. Quantification gives a guide to

the significance that sampling plays in the overall accuracy of data; and

d) to provide information on suitably abbreviated quality assurance procedures that might be used for

rapid sampling operations such as pollution incidents or groundwater investigations.

This part of ISO 5667 is one of a group of International Standards dealing with the sampling of waters.

It should be read in conjunction with the other parts of ISO 5667 and in particular with parts 1 and 3.

The general terminology is in accordance with that published.
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INTERNATIONAL STANDARD ISO 5667-14:2014(E)
Water quality — Sampling —
Part 14:
Guidance on quality assurance and quality control of
environmental water sampling and handling

WARNING — Consider and minimize any risks and obey safety rules. See ISO 5667-1 for certain

safety precautions, including sampling from boats and from ice-covered waters.
1 Scope

This part of ISO 5667 provides guidance on the selection and use of various quality assurance and quality

control techniques relating to the manual sampling of surface, potable, waste, marine and ground waters.

NOTE The general principles outlined in this part of ISO 5667 might, in some circumstances, be applicable to

sludge and sediment sampling.
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.

ISO 5667-1:2006, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and

sampling techniques

ISO 5667-3:2012, Water quality — Sampling — Part 3: Preservation and handling of water samples

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
accuracy

closeness of agreement between a test result or measurement result and the true value

Note 1 to entry: In practice, the accepted reference value is substituted for the true value.

Note 2 to entry: The term accuracy, when applied to a set of test or measurement results, involves a combination

of random components and a common systematic error or bias component.
Note 3 to entry: Accuracy refers to a combination of trueness and precision.
[SOURCE: ISO 3534-2:2006, 3.3.1]
3.2
bias

difference between the expectation of the test results or measurement result and a true value

Note 1 to entry: Bias is the total systematic error as contrasted to random error. There may be one or more

systematic error components contributing to the bias. A larger systematic difference from the true value is

reflected by a larger bias value.
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Note 2 to entry: The bias of a measuring instrument is normally estimated by averaging the error of indication

over an appropriate number of repeated measurements. The error of indication is the: “indication of a measuring

instrument minus a true value of the corresponding input quantity”.

Note 3 to entry: In practice, the accepted reference value is substituted for the true value.

[SOURCE: ISO 3534-2:2006, 3.3.2]
3.3
precision

closeness of agreement between independent test/measurement results obtained under stipulated

conditions

Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true value

or the specified value.

Note 2 to entry: The measure of precision is usually expressed in terms of imprecision and computed as a standard

deviation of the test results or measurement results. Less precision is reflected by a larger standard deviation.

Note 3 to entry: Quantitative measures of precision depend critically on the stipulated conditions. Repeatability

conditions and reproducibility conditions are particular sets of extreme stipulated conditions.

[SOURCE: ISO 3534-2:2006, 3.3.4]
3.4
representativeness

extent to which the condition of all the samples taken from the body of water reflects conditions in

water of interest
3.5
blank

observed value obtained when measurement is made on a sample identical to the sample of interest, but

in the absence of the determinand

Note 1 to entry: Deionised water; distilled water can be used as blank samples which are prepared in the laboratory

prior to sampling.
3.6
field blank

container prepared in the laboratory, using reagent water or other blank matrix, and sent with the sampling

personnel for exposure to the sampling environment to verify possible contamination during sampling

[SOURCE: ISO 11074:2005, 4.5.3]
3.7
spike

known quantity of determinand which is added to a sample, usually for the purpose of estimating the

systematic error of an analytical system by means of a recovery exercise
3.8
recovery

extent to which a known, added quantity of determinand in a sample can be measured by an

analytical system

Note 1 to entry: Recovery is calculated from the difference between results obtained from a spiked (3.7) and an

unspiked aliquot of sample and is usually expressed as a percentage.
3.9
control chart

chart on which some statistical measure of a series of samples is plotted in a particular order to steer

the process with respect to that measure and to control and reduce variation

Note 1 to entry: The particular order is usually based on time or sample number order.

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Note 2 to entry: The control chart operates most effectively when the measure is a process variable which is

correlated with an ultimate product or service characteristic.
[SOURCE: ISO 3534-2:2006, 2.3.1]
3.10
Shewhart control chart

control chart with Shewhart control limits intended primarily to distinguish between the variation in

the plotted measure due to random causes and that due to special causes

Note 1 to entry: This could be a chart using attributes (for example, proportion nonconforming) for evaluating a

process, or it could be a chart using variables (for example, average and range) for evaluating a process. Examples are:

a) X-bar chart — the sample means are plotted in order to control the mean value of a variable;

b) R chart — the sample ranges are plotted in order to control the variability of a variable;

c) s chart — the sample standard deviations are plotted in order to control the variability of a variable;

d) s chart — the sample variances are plotted in order to control the variability of a variable;

e) C chart — the number of defectives (per batch, per day, per machine, etc.) is plotted.

[SOURCE: ISO 3534-2:2006, 2.3.2, modified — Note 1 to entry has been added.]
3.11
action limits

control limits between which the statistic under consideration lies with a very high probability when

the process is under statistical control

Note 1 to entry: Action lines are drawn on a control chart to represent action limits.

Note 2 to entry: When the measure plotted lies beyond an action limit, appropriate corrective action is taken

on the process.

Note 3 to entry: These limits are based on the assumption that only 0,3 % of normally distributed results will fall

outside these limits. Such an occurrence would strongly indicate that additional, assignable causes of variation

might be present and that action might be required to identify and reduce them.
[SOURCE: ISO 3534-2:2006, 2.4.4, modified — Note 3 to entry has been added.]
3.12
warning limits

control limits between which the statistic under consideration lies with a high probability when the

process is under statistical control

Note 1 to entry: Warning lines are drawn on a control chart to represent warning limits.

Note 2 to entry: When the value of the statistic plotted lies outside a warning limit, but within the action limit

(3.11), increased supervision of the process, to pre-specified rules, is generally required.

Note 3 to entry: The limits are calculated from the standard deviation of the statistic under consideration of at

least 10 samples. Warning and action control limits are applied to individual sampling results.

[SOURCE: ISO 3534-2:2006, 2.4.3, modified — Note 3 to entry has been added.]
3.13
uncertainty
measurement uncertainty

non-negative parameter characterizing the dispersion of the quantity values being attributed to a

measurand based on the information used

[SOURCE: ISO/IEC Guide 99:2007, 2.26, modified — The notes to entry are not included here.]

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3.14
true value

value which characterizes a quantity or quantitative characteristic perfectly defined in the conditions

which exist when that quantity or quantitative characteristic is considered

Note 1 to entry: The true value of a quantity or quantitative characteristic is a theoretical concept and, in general,

cannot be known exactly.

[SOURCE: ISO 3534-2:2006, 3.2.5, modified — Note 2 to entry is not included here.]

3.15
accepted reference value
value that serves as an agreed-upon reference for comparison
Note 1 to entry: The accepted reference value is derived as:
a) a theoretical or established value, based on scientific principles;

b) an assigned or certified value, based on experimental work of some national or international organization;

c) a consensus or certified value, based on collaborative experimental work under the auspices of a scientific or

technical group;

d) the expectation, i.e. the mean of a specified set of measurements, when a), b) and c) are not available.

[SOURCE: ISO 3534-2:2006, 3.2.7]
4 Sources of sampling error
Sources of sampling errors include the following:
a) Contamination

Contamination can be caused by sampling equipment materials (sampling containers and sample

containers) by cross-contamination between samples and by sample preservation and inappropriate

storage and transport arrangements.
b) Sample instability

The type of sampling vessels and containers used can affect the stability of the determinand between

sampling and analysis due to the inherent instability of the sample itself and the conditions in which

samples are stored and transported.
c) Incorrect preservation

The choice of sampling vessels and containers affects the integrity of the determinand and the

options for preservation which may be available, as detailed in ISO 5667-3.
d) Incorrect sampling

Deviation from the sampling procedure, or the procedure itself, might be a source of error.

e) Sampling from non-homogenized water bodies
f) Sample transportation

Figure 1 illustrates various sources of sampling error: environment, personnel, materials, methods,

preservation and transportation. Further examples of common sources of sampling error are given in

Annex A.
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Figure 1 — Sources of sampling error
5 Sampling quality
5.1 General

A programme to establish sampling quality should be established for every series of sampling, so as to

ensure that data resulting from sampling programmes are both trustworthy and scientifically credible.

Mistakes in any step of the sampling procedure can result in substantial errors within the resulting data.

Laboratories that analyse collected samples usually have rigorous programmes of quality assurance and

quality control (QA/QC) as required by national regulation and conforming to ISO/IEC 17025. However,

such laboratory programmes of QA/QC cannot substitute for the rigorous sampling quality programmes

required for the collection and handling of samples prior to delivery to laboratories for analysis.

Sampling quality programmes comprise all the steps taken to ensure that valid results are produced.

Sampling quality programmes include documented evidence that the individuals who collect samples

are competent and well trained, that appropriate sample collection and sample handling methods were

employed, that equipment were maintained and calibrated, that correct practices were followed and

that records are both complete and secure. It is important to establish a quality assurance programme

and quality control effective for the characterization and reduction of errors. Depending on the objective

(e.g. to check for any contamination of the sample at different points in the sampling procedure, and

identify potential problems), the quality control set up will be different. See Table 1.

Table 1 — Means of quality control for different objectives
Objective Means to implement

Check the absence of contamination Blank environmental, Field blank, Transport blank, Equipment

blank, Filter blank
Calculate the sampling precision Duplicate sample
Check the stability of the sample Spiking

Particular importance should be given to careful measurement of analyses performed on-site and

to correct recording of determinand results. Reference should be made to ISO/TS 13530 regarding

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analytical quality control for water analysis and to ISO 15839 regarding online sensors/analysing

equipment for water.

Since analysing laboratories have expertise regarding QA/QC, it is suggested they be actively involved

in the design and evaluation of sampling quality programmes.
5.2 Technical and personnel requirements

To take a sample correctly, adequate and cleaned equipment [such as sample containers, sampling devices,

filtration equipment, a homogenizer, an intermediate container (funnel, spoon), and measurement

equipment for on-site analysis] should be held in sufficient numbers. Regular maintenance of all

equipment should be guaranteed.

The sampling vehicle and the facility should be equipped in accordance with the requirements for

sampling (laboratory vehicle).

The sampling personnel should have relevant professional training, e.g. completed vocational education

as a chemical laboratory assistant or specialist for waste water engineering. An essential prerequisite

is appropriate initial job-training and regular training of sampling personnel. Participation in internal

and/or external training should be documented (see 5.4).

A regular exchange of information between client, sampling personnel and laboratory personnel

improves the quality of sampling and testing. All the necessary information for a sampling of ensured

[7]
quality should be placed at the sampling personnel’s disposal.
5.3 Sampling manual

5.3.1 For sampling, the general requirements related to the competence of testing and calibration

laboratories should be applied.
[7]

Procedures or operating instructions should be prepared and should include the following issues:

a) sampling (matrix-based);
b) on-site measurement;
c) pre-treatment
...

NORME ISO
INTERNATIONALE 5667-14
Deuxième édition
2014-12-15
Qualité de l’eau — Échantillonnage —
Partie 14:
Lignes directrices sur l’assurance
qualité et le contrôle qualité pour
l’échantillonnage et la manutention
des eaux environnementales
Water quality — Sampling —
Part 14: Guidance on quality assurance and quality control of
environmental water sampling and handling
Numéro de référence
ISO 5667-14:2014(F)
ISO 2014
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ISO 5667-14:2014(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2014, Publié en Suisse

Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée

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l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
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ii © ISO 2014 – Tous droits réservés
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ISO 5667-14:2014(F)
Sommaire Page

Avant-propos ................................................................................................................................................................................................................................v

Introduction ..............................................................................................................................................................................................................................vii

1 Domaine d’application ................................................................................................................................................................................... 1

2 Références normatives ................................................................................................................................................................................... 1

3 Termes et définitions ....................................................................................................................................................................................... 1

4 Sources d’erreurs d’échantillonnage .............................................................................................................................................. 5

5 Qualité de l’échantillonnage ..................................................................................................................................................................... 6

5.1 Généralités .................................................................................................................................................................................................. 6

5.2 Exigences techniques et humaines ........................................................................................................................................ 6

5.3 Manuel d’échantillonnage ............................................................................................................................................................. 7

5.4 Formation de l’équipe d’échantillonnage ........................................................................................................................ 8

6 Stratégie et organisation .............................................................................................................................................................................. 9

6.1 Date, durée et fréquence d’échantillonnage .................................................................................................................. 9

6.2 Points de prélèvement/échantillonnage .......................................................................................................................... 9

7 Prélèvement et manipulation des échantillons ................................................................................................................... 9

7.1 Contrôle du véhicule et du matériel avant l’exécution du programme d’échantillonnage .... 9

7.2 Préparation à l’échantillonnage sur site ........................................................................................................................10

7.3 Mesurages sur site ............................................................................................................................................................................10

7.4 Prélèvement des échantillons .................................................................................................................................................11

7.4.1 Échantillons ponctuels.............................................................................................................................................11

7.4.2 Échantillons composites ........................................................................................................................................11

7.4.3 Prétraitement d’échantillonnage ....................................................................................................................12

7.4.4 Homogénéisation et sous-échantillonnage ............................................................................................12

7.4.5 Filtration ..............................................................................................................................................................................13

7.4.6 Conservation des échantillons ..........................................................................................................................13

8 Identification des échantillons ...........................................................................................................................................................14

9 Protocole d’échantillonnage de terrain .....................................................................................................................................14

10 Transport et stockage des échantillons .....................................................................................................................................14

11 Contrôle qualité de l’échantillonnage .........................................................................................................................................15

11.1 Généralités ...............................................................................................................................................................................................15

11.2 Doubles échantillons .......................................................................................................................................................................17

11.3 Blanc de terrain ...................................................................................................................................................................................19

11.4 Rinçage du matériel (matériel d’échantillonnage) ...............................................................................................20

11.5 Filtration (blanc et dopage) ......................................................................................................................................................20

11.5.1 Généralités .........................................................................................................................................................................20

11.5.2 Blanc de filtration (eau désionisée) .............................................................................................................21

11.5.3 Échantillon d’assurance qualité dopé .........................................................................................................22

11.6 Technique 1 — Échantillons dopés ....................................................................................................................................23

11.6.1 Généralités .........................................................................................................................................................................23

11.6.2 Échantillons d’eau désionisée dopés ...........................................................................................................23

11.7 Technique 2 — Échantillons environnementaux dopés ...................................................................................25

12 Analyse et interprétation des données de contrôle qualité .................................................................................26

12.1 Cartes de contrôle de Shewhart ............................................................................................................................................26

12.2 Construction des cartes de contrôle pour les doubles ......................................................................................26

13 Audits indépendants .....................................................................................................................................................................................27

[7]

Annexe A (informative) Sources courantes d’erreur d’échantillonnage ..............................................................28

Annexe B (informative) Cartes de contrôle .................................................................................................................................................30

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ISO 5667-14:2014(F)

Annexe C (informative) Sous-échantillonnage à l’aide d’un système d’homogénéisation ........................34

Bibliographie ...........................................................................................................................................................................................................................37

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ISO 5667-14:2014(F)
Avant-propos

L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes

nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est

en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude

a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,

gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.

L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui

concerne la normalisation électrotechnique.

Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont

décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents

critères d’approbation requis pour les différents types de documents ISO. Le présent document a été

rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www.

iso.org/directives).

L’attention est portée sur le fait que certains des éléments du présent document peuvent faire l’objet de

droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable

de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant

les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de

l’élaboration du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de

brevets reçues par l’ISO (voir www.iso.org/patents).

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un

engagement.

Pour une explication de la signification des termes et expressions spécifiques de l’ISO liés à l’évaluation

de la conformité, ou pour toute information au sujet de l’adhésion de l’ISO aux principes de l’OMC

concernant les obstacles techniques au commerce (OTC), voir le lien suivant : Avant-propos —

Informations supplémentaires.

Le présent document a été élaboré par le comité technique ISO/TC 147, Qualité de l’eau, sous-comité

SC 6, Échantillonnage (méthodes générales).

Cette deuxième édition annule et remplace la première édition (ISO 5667-14:1998) qui a fait l’objet d’une

révision technique.

L’ISO 5667 comprend les parties suivantes, présentées sous le titre général Qualité de l’eau —

Échantillonnage :

— Partie 1 : Lignes directrices pour la conception des programmes et des techniques d’échantillonnage

— Partie 3 : Conservation et manipulation des échantillons d’eau

— Partie 4 : Guide pour l’échantillonnage des eaux des lacs naturels et des lacs artificiels

— Partie 5 : Lignes directrices pour l’échantillonnage de l’eau potable des usines de traitement et du réseau

de distribution

— Partie 6 : Lignes directrices pour l’échantillonnage des rivières et des cours d’eau

— Partie 7 : Guide général pour l’échantillonnage des eaux et des vapeurs dans les chaudières

— Partie 8 : Guide général pour l’échantillonnage des dépôts humides
— Partie 9 : Guide général pour l’échantillonnage des eaux marines
— Partie 10 : Guide pour l’échantillonnage des eaux résiduaires
— Partie 11 : Lignes directrices pour l’échantillonnage des eaux souterraines
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ISO 5667-14:2014(F)
— Partie 12 : Guide général pour l’échantillonnage des sédiments
— Partie 13 : Lignes directrices pour l’échantillonnage de boues

— Partie 14 : Lignes directrices sur l’assurance qualité et le contrôle qualité pour l’échantillonnage et la

manutention des eaux environnementales

— Partie 15 : Lignes directrices pour la conservation et le traitement des échantillons de boues et de

sédiments
— Partie 16 : Lignes directrices pour les essais biologiques des échantillons

— Partie 17 : Lignes directrices pour l’échantillonnage des matières solides en suspension

— Partie 19 : Lignes directrices pour l’échantillonnage des sédiments en milieu marin

— Partie 20 : Lignes directrices relatives à l’utilisation des données d’échantillonnage pour la prise de

décision — Conformité avec les limites et systèmes de classification

— Partie 21 : Lignes directrices pour l’échantillonnage de l’eau potable distribuée par camions-citernes ou

d’autres moyens que les tuyaux de distribution

— Partie 22 : Lignes directrices pour la conception et l’installation de points d’échantillonnage des eaux

souterraines

— Partie 23 : Lignes directrices pour l’échantillonnage passif dans les eaux de surface

vi © ISO 2014 – Tous droits réservés
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ISO 5667-14:2014(F)
Introduction

L’échantillonnage est la première étape en vue de la réalisation d’examens chimiques, physiques et

biologiques. Par conséquent, il convient que l’échantillon prélevé soit représentatif de l’objectif visé et

soit expédié au laboratoire de manière adaptée. Les erreurs dues à un prélèvement, un prétraitement,

un transport et un stockage incorrects des échantillons ne peuvent pas être corrigées.

La présente partie de l’ISO 5667 spécifie les modes opératoires d’assurance qualité et de contrôle

qualité et fournit des lignes directrices supplémentaires pour l’échantillonnage des différents types

d’eaux couverts dans les parties spécifiques de l’ISO 5667.

Les modes opératoires de contrôle qualité sont requis pour le prélèvement des échantillons d’eau

environnementale afin de :
a) contrôler l’efficacité de la méthodologie d’échantillonnage ;

b) démontrer que les différentes étapes du procédé de prélèvement d’échantillons sont correctement

contrôlées et adaptées à l’usage prévu, y compris le contrôle adéquat des sources d’erreur telles que

la contamination des échantillons, la perte de l’élément à doser et l’instabilité des échantillons. À

cet effet, il est recommandé que les modes opératoires de contrôle qualité permettent de détecter

les erreurs d’échantillonnage, et ainsi de rejeter les données non valides ou erronées résultant du

procédé d’échantillonnage ;

c) quantifier et contrôler les sources d’erreurs qui apparaissent lors de l’échantillonnage. La

quantification donne des indications sur l’importance que l’échantillonnage joue dans l’exactitude

globale des données ; et

d) fournir des informations sur les modes opératoires accélérés d’assurance qualité susceptibles

d’être utilisés pour les opérations d’échantillonnage rapides telles que les incidents de pollution ou

les analyses d’eaux souterraines.

La présente partie de l’ISO 5667 fait partie d’un groupe de Normes internationales relatives à

l’échantillonnage des eaux. Il convient de la lire conjointement avec les autres parties de l’ISO 5667, en

particulier avec les parties 1 et 3.
La terminologie générale est conforme à celle publiée.
© ISO 2014 – Tous droits réservés vii
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NORME INTERNATIONALE ISO 5667-14:2014(F)
Qualité de l’eau — Échantillonnage —
Partie 14:
Lignes directrices sur l’assurance qualité et le contrôle
qualité pour l’échantillonnage et la manutention des eaux
environnementales

AVERTISSEMENT — Tous les risques doivent être pris en compte et réduits le plus possible, et

les règles de sécurité doivent être appliquées. Se reporter à l’ISO 5667-1 pour les précautions de

sécurité spécifiques, y compris l’échantillonnage effectué à partir de bateaux et l’échantillonnage

d’eaux couvertes de glace.
1 Domaine d’application

La présente partie de l’ISO 5667 fournit des lignes directrices sur le choix et l’utilisation de différentes

techniques d’assurance qualité et de contrôle qualité liées à l’échantillonnage manuel des eaux de

surface, potables, résiduaires, marines et souterraines.

NOTE Dans certains cas, les principes généraux exposés dans la présente partie de l’ISO 5667 peuvent

s’appliquer à l’échantillonnage de boues et de sédiments.
2 Références normatives

Les documents ci-après, dans leur intégralité ou non, sont des références normatives indispensables à

l’application du présent document. Pour les références datées, seule l’édition citée s’applique. Pour les

références non datées, la dernière édition du document de référence s’applique (y compris les éventuels

amendements).

ISO 5667-1:2006, Qualité de l’eau — Échantillonnage — Partie 1: Lignes directrices pour la conception des

programmes et des techniques d’échantillonnage

ISO 5667-3:2012, Qualité de l’eau — Échantillonnage — Partie 3: Conservation et manipulation des

échantillons d’eau
3 Termes et définitions

Pour les besoins du présent document, les termes et définitions suivants s’appliquent.

3.1
exactitude

étroitesse de l’accord entre le résultat d’essai ou résultat de mesure et la valeur vraie

Note 1 à l’article: Dans la pratique, la valeur de référence acceptée remplace la valeur vraie.

Note 2 à l’article: Le terme « exactitude », appliqué à un ensemble de résultats d’essai ou de mesure, implique une

combinaison de composantes aléatoires et d’une erreur systématique commune ou d’une composante de biais.

Note 3 à l’article: L’exactitude fait référence à une combinaison de justesse et de fidélité.

[SOURCE: ISO 3534-2:2006, 3.3.1]
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ISO 5667-14:2014(F)
3.2
biais

différence entre l’espérance mathématique d’un résultat d’essai ou résultat de mesure et une valeur vraie

Note 1 à l’article: Le biais est une erreur systématique totale par opposition à l’erreur aléatoire. Il peut y avoir

une ou plusieurs composantes d’erreurs systématiques qui contribuent au biais. Une différence systématique

importante par rapport à la valeur vraie est reflétée par une grande valeur du biais.

Note 2 à l’article: Le biais (erreur de justesse) d’un instrument de mesure est normalement estimé en prenant

la moyenne de l’erreur d’indication sur un nombre approprié d’observations répétées. L’erreur d’indication est

«l’indication d’un instrument de mesure moins une valeur vraie de la grandeur d’entrée correspondante».

Note 3 à l’article: Dans la pratique, la valeur de référence acceptée remplace la valeur vraie.

[SOURCE: ISO 3534-2:2006, 3.3.2]
3.3
fidélité

étroitesse d’accord entre des résultats d’essai/de mesure indépendants obtenus sous des conditions

stipulées

Note 1 à l’article: La fidélité dépend uniquement de la distribution des erreurs aléatoires et n’a aucune relation

avec la valeur vraie ou la valeur spécifiée.

Note 2 à l’article: La mesure de la fidélité est généralement exprimée en termes d’infidélité et est calculée à

partir de l’écart-type des résultats d’essai ou des résultats de mesure. Une fidélité faible est reflétée par un grand

écart-type.

Note 3 à l’article: Les mesures quantitatives de la fidélité dépendent de façon critique des conditions stipulées.

Les conditions de répétabilité et de reproductibilité sont des ensembles particuliers de conditions extrêmes

stipulées.
[SOURCE: ISO 3534-2:2006, 3.3.4]
3.4
représentativité

situation dans laquelle l’état de tous les échantillons prélevés dans la masse d’eau reflète celui de l’eau

analysée
3.5
blanc

valeur observée lorsque le mesurage est réalisé sur un échantillon identique à l’échantillon étudié, mais

en l’absence de l’élément à doser

Note 1 à l’article: L’eau désionisée ou distillée peut être utilisée pour les échantillons à blanc qui sont préparés au

laboratoire avant l’échantillonnage.
3.6
blanc de terrain

récipient préparé dans le laboratoire, utilisant comme réactif de l’eau ou toute autre matrice de

blanc, et destiné à être emporté par le personnel d’échantillonnage sur le terrain, pour être exposé à

l’environnement dans lequel l’échantillonnage est effectué afin de vérifier l’absence de contamination

au cours de l’échantillonnage
[SOURCE: ISO 11074:2005, 4.5.3]
3.7
échantillon dopé

quantité connue d’élément à doser ajoutée à un échantillon, en général pour les besoins de l’estimation

de l’erreur systématique d’un système analytique au moyen d’une récupération
2 © ISO 2014 – Tous droits réservés
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ISO 5667-14:2014(F)
3.8
récupération

opération au moyen de laquelle un système analytique peut mesurer une quantité ajoutée, connue, d’un

élément à doser dans un échantillon

Note 1 à l’article: La récupération est calculée à partir la différence entre les résultats obtenus à partir d’un

échantillon dopé (3.7) et une aliquote non dopée de l’échantillon, généralement exprimée en pourcentage.

3.9
carte de contrôle

graphique sur lequel sont reportées les valeurs d’une mesure statistique faite sur une série

d‘échantillons dans un ordre particulier pour orienter le processus en fonction de cette mesure et pour

contrôler et réduire la variation

Note 1 à l’article: L’ordre particulier est généralement fondé sur un ordre chronologique ou de numéro

d’échantillon.

Note 2 à l’article: La carte de contrôle est plus efficace lorsque la mesure concerne une variable du processus

corrélée à un produit final ou à une caractéristique de service.
[SOURCE: ISO 3534-2:2006, 2.3.1]
3.10
carte de contrôle de Shewhart

carte de contrôle avec des limites de contrôle de Shewart principalement utilisée pour différencier une

variation sur la mesure reportée due à des causes aléatoires et celle due à des causes spéciales

Note 1 à l’article: Cette carte pourrait utiliser des attributs (par exemple, une proportion de non-conformités) ou

des variables (par exemple, une moyenne et une étendue) pour évaluer un processus. Exemples :

a) carte X barre — les moyennes des échantillons sont reportées afin de contrôler la valeur moyenne d’une

variable ;

b) carte R — les étendues des échantillons sont reportées afin de contrôler la variabilité d’une variable ;

c) carte s — les écarts-types des échantillons sont reportés afin de contrôler la variabilité d’une variable ;

d) carte s — les variances des échantillons sont reportées afin de contrôler la variabilité d’une variable ;

e) carte C — le nombre d’individus défectueux (par lot, par jour, par machine, etc.) est représenté.

[SOURCE: ISO 3534-2:2006, 2.3.2, modifiée — La Note 1 à l’article a été ajoutée]
3.11
limites d’action

limites de contrôle entre lesquelles la valeur statistique considérée se situe avec une probabilité très

élevée quand le processus est en état de maîtrise statistique

Note 1 à l’article: Les lignes d’action sont tracées sur une carte de contrôle pour représenter les limites d’action.

Note 2 à l’article: Quand la mesure reportée est au-delà d’une limite d’action, une action corrective appropriée est

réalisée sur le processus.

Note 3 à l’article: Ces limites sont fondées sur l’hypothèse que seul 0,3 % des résultats suivant une distribution

normale seront en dehors de ces limites. Une telle occurrence suggèrerait l’existence très probable de causes de

variation systématiques, supplémentaires, nécessitant une action visant à les identifier et les réduire.

[SOURCE: ISO 3534-2:2006, 2.4.4, modifiée — La Note 3 à l’article a été ajoutée]
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ISO 5667-14:2014(F)
3.12
limites de surveillance

limites de contrôle entre lesquelles la valeur statistique considérée se situe avec une probabilité élevée

quand le processus est en état de maîtrise statistique

Note 1 à l’article: Les lignes de surveillance sont tracées sur une carte de contrôle pour représenter les limites de

surveillance.

Note 2 à l’article: Quand la valeur statistique reportée est en dehors des limites de surveillance mais à l’intérieur

des limites d’action (3.11), une surveillance accrue du processus, conforme à des règles pré-spécifiées, est

généralement nécessaire.

Note 3 à l’article: Les limites sont calculées à partir de l’écart-type de la valeur statistique considérée d’au

moins 10 échantillons. Les limites de surveillance et d’action sont appliquées aux résultats d’échantillonnage

individuels.
[SOURCE: ISO 3534-2:2006, 2.4.3, modifiée — La Note 3 à l’article a été ajoutée]
3.13
incertitude
incertitude de mesure

paramètre non négatif qui caractérise la dispersion des valeurs attribuées à un mesurande, à partir des

informations utilisées

[SOURCE: Guide ISO/IEC 99:2007, 2.26, modifiée — Les notes à l’article ne sont pas incluses ici]

3.14
valeur vraie

valeur qui caractérise une grandeur ou une caractéristique quantitative parfaitement définie dans les

conditions qui existent lorsque cette grandeur ou caractéristique quantitative est considérée

Note 1 à l’article: La valeur vraie d’une grandeur ou d’une caractéristique quantitative est une notion théorique

et, en général, ne peut pas être connue exactement.

[SOURCE: ISO 3534-2:2006, 3.2.5, modifiée — La Note 2 à l’article n’est pas incluse ici]

3.15
valeur de référence acceptée
valeur qui sert de référence, selon un agrément pour une comparaison
Note 1 à l’article: La valeur de référence acceptée résulte :
a) d’une valeur théorique ou établie, fondée sur des principes scientifiques ;

b) d’une valeur assignée ou certifiée, fondée sur les travaux d’une organisation nationale ou internationale ;

c) d’une valeur de consensus ou certifiée, fondée sur un travail expérimental en collaboration et placé sous les

auspices d’un groupe scientifique ou technique ;

d) de l’espérance, c’est-à-dire la moyenne de la population spécifiée de mesures, dans les cas où a), b) et c) ne

sont pas applicables.
[SOURCE: ISO 3534-2:2006, 3.2.7]
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ISO 5667-14:2014(F)
4 Sources d’erreurs d’échantillonnage
Les erreurs d’échantillonnage peuvent provenir des sources suivantes :
a) contamination ;

La contamination peut être due aux matériaux constituant l’équipement d’échantillonnage (matériel

d’échantillonnage et flacons), à la contamination croisée entre échantillons, à la conservation des

échantillons et à des mesures de stockage et de transport inadaptées.
b) instabilité des échantillons ;

Le type de flacons et de matériel d’échantillonnage utilisés peut affecter la stabilité de l’élément à

doser entre l’échantillonnage et l’analyse en raison de l’instabilité inhérente de l’échantillon ainsi

que de ses conditions de stockage et de transport.
c) conservation incorrecte ;

Le choix des flacons et du matériel d’échantillonnage a un impact sur l’intégrité de l’élément à doser

ainsi que les conditions de conservation. Se référer à l’ISO 5667-3.
d) échantillonnage incorrect ;

Tout écart par rapport au mode opératoire d’échantillonnage, ou le mode opératoire en lui-même,

peut être source d’erreurs.
e) échantillonnage à partir de masses d’eau non homogénéisées ;
f) transport des échantillons.

La Figure 1 illustre différentes sources d’erreurs d’échantillonnage : environnement, personnel,

matériaux, méthodes, conservation et transport. L’Annexe A donne d’autres exemples de sources

d’erreurs courantes lors de l’échantillonnage.
Figure 1 — Sources d’erreurs d’échantillonnage
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ISO 5667-14:2014(F)
5 Qualité de l’échantillonnage
5.1 Généralités

Il convient d’élaborer un programme permettant d’établir la qualité de chaque série d’échantillonnages

afin de s’assurer que les données résultant des programmes d’échantillonnage soient fiables et

scientifiquement crédibles. Toute erreur commise à une étape quelconque du
...