DRAFT FOR DEVELOPMENT

Lead and lead alloys

Analysis by flame
atomic absorption
spectrometry (FAAS) or
inductively coupled
plasma emissions
spectrometry (ICP-ES),
after separation by
co-precipitation

ICS 77.120.60

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

DD ENV
14138:2001

DD ENV 14138:2001

National foreword
This Draft for Development is the English language version of
ENV 14138:2001.
This publication is not to be regarded as a British Standard.
It is being issued in the Draft for Development series of publications and is of
a provisional nature because, although the analytical procedures in the method
are generally recognized, the evaluation of the method via Round-Robin
analyses, together with the resultant statistical validation, as required by
CEN, has not yet been carried out. It should be applied on this provisional
basis, so that information and experience of its practical application may be
obtained.
Comments arising from the use if this Draft for Development are requested so
that UK experience can be reported to the European organization responsible
for its conversion into a European Standard. A review of this publication will
be initiated 2 years after its publication by the European organization so that
a decision can be taken on its status at the end of its three-year life. The
commencement of the review period will be notified by an announcement in
Update Standards.
According to the replies received by the end of the review period, the
responsible BSI Committee will decide whether to support the conversion into
a European Standard, to extend the life of the prestandard or to withdraw it.
Comments should be sent in writing to the Secretary of BSI Technical
Committee NFE/22, Lead and lead alloys, at 389 Chiswick High Road, London
W4 4AL, giving the document reference and clause number and proposing,
where possible, an appropriate revision of the text.
A list of organizations represented on this committee can be obtained on
request to its secretary.
Cross-references
The British Standards which implement international or European
publications referred to in this document may be found in the BSI Standards
Catalogue under the section entitled International Standards Correspondence
Index, or by using the Find facility of the BSI Standards Electronic
Catalogue.

This Draft for Development,

having been prepared under
the direction of the Engineering
Sector Policy and Strategy
Committee, was published
under the authority of the
Standards Policy and Strategy
Committee on
21 December 2001

Summary of pages
This document comprises a front cover, an inside front cover, the ENV title
page, pages 2 to 14, an inside back cover and a back cover.
The BSI copyright date displayed in this document indicates when the
document was last issued.

Amendments issued since publication

Amd. No.
BSI 21 December 2001

ISBN 0 580 38084 X

Date

Comments

EUROPEAN PRESTANDARD

ENV 14138

PRNORME EUROPENNE
EUROPISCHE VORNORM

December 2001

ICS 77.120.60

English version

Lead and lead alloys - Analysis by flame atomic absorption

spectrometry (FAAS) or inductively coupled plasma emission
spectrometry (ICP-ES), after separation by co-precipitation
Plomb et alliages de plomb - Analyse par spectromtrie
d'absorption atomique dans la flamme (FAAS) ou par
spectromtrie d'mission plasma inductif coupl (ICPES), aprs sparation par co-prcipitation

Blei und Bleilegierungen - Analyse durch FlammenAtomabsorptionsspektrometrie (FAAS) oder EmissionSpektrometrie mit induktiv gekoppeltem Plasma (ICP-ES),
nach Abtrennung durch Mitfllung

This European Prestandard (ENV) was approved by CEN on 18 November 2001 as a prospective standard for provisional application.
The period of validity of this ENV is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the ENV can be converted into a European Standard.
CEN members are required to announce the existence of this ENV in the same way as for an EN and to make the ENV available promptly
at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the final
decision about the possible conversion of the ENV into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMIT EUROPEN DE NORMALISATION
EUROPISCHES KOMITEE FR NORMUNG

Management Centre: rue de Stassart, 36

2001 CEN

All rights of exploitation in any form and by any means reserved

worldwide for CEN national Members.

B-1050 Brussels

Ref. No. ENV 14138:2001 E

ENV 14138:2001 (E)

Contents
page
Foreword......................................................................................................................................................................4
1

Scope ..............................................................................................................................................................5

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

3
3.1
3.2
3.2.1
3.2.2

Principle ..........................................................................................................................................................5
Preparation of the test solution....................................................................................................................5
Instrumental techniques ...............................................................................................................................6
Flame atomic absorption spectrometry (FAAS) .........................................................................................6
Inductively coupled plasma emission spectrometry (ICP-ES)..................................................................6

4
4.1
4.2
4.3
4.4
4.4.1
4.4.2

Apparatus .......................................................................................................................................................6
General............................................................................................................................................................6
Volumetric glassware ....................................................................................................................................6
Filtration system ............................................................................................................................................6
Instruments.....................................................................................................................................................6
Flame atomic absorption spectrometer ......................................................................................................6
Inductively coupled plasma emission spectrometer .................................................................................7

5
5.1
5.2
5.2.1
5.2.2
5.2.3
5.3
5.3.1
5.3.2
5.4
5.5
5.6
5.7
5.8
5.8.1
5.8.2
5.8.3
5.8.4

Reagents .........................................................................................................................................................7
General............................................................................................................................................................7
Nitric acid (HNO3) ..........................................................................................................................................7
Concentrated nitric acid................................................................................................................................7
Nitric acid 1:1 (V/V) ........................................................................................................................................7
Nitric acid 1:2 (V/V) ........................................................................................................................................7
Hydrochloric acid (HCl) .................................................................................................................................7
Concentrated hydrochloric acid...................................................................................................................7
Hydrochloric acid 1:1 (V/V) ...........................................................................................................................7
Ammonia solution..........................................................................................................................................7
Pure lead .........................................................................................................................................................7
Manganese nitrate solution ..........................................................................................................................8
Potassium permanganate solution ..............................................................................................................8
Standard solutions ........................................................................................................................................8
Standard solutions (1g/l)...............................................................................................................................8
Standard solutions (100 mg/l).......................................................................................................................8
Standard solutions (10 mg/l).........................................................................................................................9
Multi-element solutions (either 10 mg/l or 100 mg/l) ..................................................................................9

Sampling and sample preparation ...............................................................................................................9

7
7.1
7.1.1
7.1.2
7.1.3
7.2
7.3
7.4

Procedure .......................................................................................................................................................9
Preparation of the test solution....................................................................................................................9
Dissolution......................................................................................................................................................9
Co-precipitation with manganese dioxide...................................................................................................9
Test solution...................................................................................................................................................9
Preparation of the synthetic test solution...................................................................................................9
Preparation of the blank test solution .......................................................................................................10
Preparation of calibration solutions ..........................................................................................................10

8
8.1
8.2
8.3
8.3.1
8.3.2

Determination of elements by FAAS..........................................................................................................10

General..........................................................................................................................................................10
Calibration and measurement of the test solution ...................................................................................11
Expression of results ..................................................................................................................................11
Analyte recovery rate ..................................................................................................................................11
Analyte content in the sample ....................................................................................................................11

9
9.1
9.2

Determination of elements by ICP-ES .......................................................................................................12

General..........................................................................................................................................................12
Calibration and measurement of the test solution ...................................................................................12

ENV 14138:2001 (E)

9.3
9.3.1
9.3.2

Expression of results ..................................................................................................................................13

Analyte recovery rate ..................................................................................................................................13
Analyte content in the sample....................................................................................................................13

10

Test report ....................................................................................................................................................13

Bibliography ..............................................................................................................................................................14

ENV 14138:2001 (E)

Foreword
This European Prestandard has been prepared by Technical Committee CEN /TC 306, "Lead and lead alloys", the
secretariat of which is held by AFNOR.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this European Prestandard: Austria, Belgium, Czech Republic, Denmark, Finland,
France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden,
Switzerland and the United Kingdom.
CAUTION FOR SAFETY AND TRAINING
The methods in this Prestandard are recommended for the certification of reference materials and as umpire
methods in cases of a dispute. The importance of either application, and the paramount issue of safety, requires
that they should only be carried out by fully-trained analysts who are experienced in all relevant techniques and the
precautions necessary in the inherently hazardous environs of a laboratory, especially those required when using
particularly hazardous apparatus and reagents used in some of these methods.
Where a particular hazard exists, this is given as a DANGER adjacent to the point in the text where the apparatus
or reagent is referenced.

ENV 14138:2001 (E)

Scope

This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively
coupled plasma emission spectrometry (ICP-ES) for the determination of elements at low content in lead for the
ranges given in Table 1.
Higher contents than those listed in Table 1 should be determined according to ENV 13800.
Table 1 Ranges of application for the determination of elements
Element

Ranges of applications
(% m/m)
FAAS

ICP-ES

As

0,0002

0,005

0,00005

0,005

Sb

0,0002

0,0025

0,0002

0,0025

Se

0,0002

0,005

0,0002

0,005

Sn

0,0005

0,005

0,0002

0,005

Te

0,00002

0,0025

0,00002

0,0025

These methods are intended as the definitive methods in case of dispute for the determination of elements at low
content in lead. They are also recommended for the analysis of Certified Reference Materials (CRM) and
Reference Materials (RM) which are used in analysis according to ENV 12908.

Normative references

This European Prestandard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Prestandard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
EN 12402, Lead and lead alloys - Methods of sampling for analysis.
ENV 12908, Lead and lead alloys - Analysis by Optical Emission Spectrometry (OES) with spark excitation.
ENV 13800, Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively
coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrix.
ISO 648, Laboratory glassware One-mark pipettes.
EN ISO 1042, Laboratory glassware One-mark volumetric flasks (ISO 1042:1998).
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).

3
3.1

Principle
Preparation of the test solution

Dissolution of a test portion in nitric acid.

Separation of analyte by co-precipitation with manganese dioxide.
Dissolution of the precipitate, made up to a defined volume.
Determination of the analyte concentration using one of the two techniques described in 3.2.

ENV 14138:2001 (E)

3.2

Instrumental techniques

3.2.1

Flame atomic absorption spectrometry (FAAS)

The analyte concentration in the test solution is obtained by :

nebulization of the test solution into the flame of an atomic absorption spectrometer ;

measurement of the absorption of the resonance line energy of the spectrum from the element at the relevant
wavelength (absorbance) ;

comparison with that of calibration solutions of the same element.

3.2.2

Inductively coupled plasma emission spectrometry (ICP-ES)

The analyte concentration in the test solution is obtained by :

nebulization of the test solution into the plasma of an inductively coupled plasma optical emission
spectrometer ;

measurement of the intensity of the emission signal from the spectrum of the element to be determined at the
relevant wavelength ;

comparison with that of calibration solutions of the same element.

Apparatus

4.1

General

Use ordinary apparatus as available in a chemical laboratory.

All glassware to be used shall be cleaned with diluted hydrochloric acid (5.3.2) and thoroughly rinsed with water.

4.2

Volumetric glassware

4.2.1 One-mark volumetric flasks of capacities 25 ml, 100 ml, 500 ml and 1 000 ml in accordance with EN ISO
1042 class A.
4.2.2 One-mark pipettes of capacities 5 ml, 10 ml, 15 ml, 20 ml, 25 ml and 50 ml in accordance with ISO 648
class A.

4.3

Filtration system

Vacuum filtration system with a filter membrane of PTFE, or other material inert to nitric acid, of about 5 m
porosity (filtering diameter 20 mm to 50 mm).

4.4
4.4.1

Instruments
Flame atomic absorption spectrometer

Flame atomic absorption spectrometer (FAAS) equipped with laminar flow burners suitable for acetylene-air,
hydrogen-air or acetylene-nitrous oxide flames, and with radiation sources such as hollow cathode lamps (HCL) or
electrode-less discharge lamps (EDL) as appropriate to the element to be determined.
The instrument shall be used in accordance with the manufacturer's instructions and the performance checked (see
also ISO/DIS 13204-2 and ISO/DIS 13204-3).
DANGER
To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be
exhausted externally.

ENV 14138:2001 (E)

4.4.2

Inductively coupled plasma emission spectrometer

Inductively coupled plasma emission spectrometer (ICP-ES), either a simultaneous instrument with the relevant
wavelengths installed or a sequential instrument where a monochromator system allows the selection of
wavelengths (see also ISO/DIS 12235-1).
The instrument shall be used in accordance with the manufacturer's instructions and the performances checked
(see also ISO/DIS 12235-2).
DANGER
To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be
exhausted externally.

Reagents

5.1

General

For all stages of analysis, unless otherwise stated, use only reagents of recognised analytical grade, preferably
with an actual analysis, suitable for trace analysis and only water of at least grade 2, as specified in EN ISO 3696.
Prepare all solutions using the same container of each reagent.

5.2
5.2.1

Nitric acid (HNO3)

Concentrated nitric acid

Nitric acid of high purity, which
20 = 1,41 g/ml.

5.2.2

Nitric acid 1:1 (V/V)

Add to one volume of water, in a suitable container, the same volume of concentrated nitric acid (5.2.1) and mix
thoroughly.
5.2.3

Nitric acid 1:2 (V/V)

Add 200 ml concentrated nitric acid (5.2.1) to 400 ml water in a 1 000 ml beaker and mix thoroughly.

5.3
5.3.1

Hydrochloric acid (HCl)

Concentrated hydrochloric acid

Hydrochloric acid of high purity, which
20 = 1,18 g/ml.

5.3.2

Hydrochloric acid 1:1 (V/V)

Add 400 ml of concentrated hydrochloric acid (5.3.1) to 400 ml water in a 1 000 ml flask. This acid is used to clean
all glassware which should be soaked for at least 1 h prior to use, then rinsed thoroughly with water.

5.4

Ammonia solution

Ammonia solution of high purity which
20 = 0,88 g/ml.

5.5

Pure lead

For the determination of the recovery rate of the analyte (see 7.2), very pure lead (99,9999 % m/m) should be used.
However, lead of lower purity may be used provided that the analyte is not present in an amount that could be
significant to the determination required.

ENV 14138:2001 (E)

5.6

Manganese nitrate solution

Dissolve (7,00 0,01) g of hydrated manganese nitrate (Mn(NO3)24H2O) in water, transfer to a 100 ml volumetric
flask, make up to the mark with water and mix thoroughly.

5.7

Potassium permanganate solution

Weigh (3,20 0,01) g of potassium permanganate (KMnO4) into a 600 ml beaker, add 400 ml water and swirl until
dissolved. Transfer into a 1 000 ml volumetric flask, make up to the mark with water and mix thoroughly.

5.8

Standard solutions

5.8.1
5.8.1.1

Standard solutions (1g/l)

General

Either use commercially available certified standard solutions or prepare standard solutions as described in 5.8.1.2
to 5.8.1.6.
5.8.1.2

Solution for arsenic

Dry approximately 5 g of arsenic oxide (As2O3, 99,99 % m/m minimum purity) in an oven at (105  2) C for two
hours and allow to cool completely in a desiccator. Weigh (1,320  0,001) g of dried arsenic oxide and transfer into
a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a watch glass, and swirl until dissolution is complete.
Transfer into a 1 000 ml volumetric flask (4.2.1) then make up to the mark with water and mix thoroughly.
5.8.1.3

Solution for antimony

Dry approximately 5 g of antimony oxide (Sb2O3, 99,99% m/m minimum purity) in an oven at (105 2) C for two
hours and allow to cool completely in a desiccator. Weigh (1,197  0,001) g into a 250 ml beaker, add 25 ml of
water and 50 ml of concentrated hydrochloric acid (5.3.1), cover with a watch glass and swirl until dissolution is
complete. Transfer into a 1 000 ml volumetric flask (4.2.1) then make up to the mark with water and mix thoroughly.
5.8.1.4

Solution for selenium

Weigh (1,000  0,001) g of selenium (99,99 % m/m minimum purity) into a 250 ml beaker, add 100 ml of nitric acid
(5.2.2), cover with a watch glass, and heat gently to initiate the reaction of dissolution. Cool if the reaction proceeds
too vigorously. Allow to cool, transfer to a 1 000 ml volumetric flask (4.2.1) then make up to the mark with water and
mix thoroughly.
5.8.1.5

Solution for tin

Weigh (1,000  0,001) g of tin (99,99 % m/m minimum purity) into a 250 ml beaker, add 100 ml of concentrated
hydrochloric acid (5.3.1), cover with a watch glass and heat gently until dissolution is complete. Allow to cool, then
transfer to a 1 000 ml volumetric flask (4.2.1) then make up to the mark with water and mix thoroughly.
5.8.1.6

Solution for tellurium

Weigh (1,000  0,001) g of tellurium (99,99 % m/m minimum purity) into a 250 ml beaker, add 100 ml of nitric acid
(5.2.2), cover with a watch glass and swirl until dissolution is complete, transfer into a 1 000 ml volumetric flask
(4.2.1) then make up to the mark with water and mix thoroughly.
5.8.2

Standard solutions (100 mg/l)

Using a 50 ml pipette (4.2.2) transfer 50 ml of the relevant standard solution (5.8.1) into a 500 ml volumetric flask
(4.2.1). Add 50 ml of concentrated hydrochloric acid (5.3.1) then make up to the mark with water and mix
thoroughly.

ENV 14138:2001 (E)

5.8.3

Standard solutions (10 mg/l)

Using a 10 ml pipette (4.2.2), transfer 10 ml of the relevant standard solution (5.8.1) into a 1 000 ml volumetric flask
(4.2.1). Add 50 ml of concentrated hydrochloric acid (5.3.1), then make up to the mark with water and mix
thoroughly.
Each solution shall be prepared on the day of use.
5.8.4

Multi-element solutions (either 10 mg/l or 100 mg/l)

For preparing multi-element solutions, transfer either 10 ml or 100 ml of each relevant standard solution (5.8.1) of
the elements required into a 1 000 ml volumetric flask (4.2.1). Add the appropriate volume of acid, then make up to
the mark with water and mix thoroughly.
Each multi-element solution (10 mg/l) shall be prepared on the day of use.

Sampling and sample preparation

Sampling and preparation of the laboratory sample shall be carried out in accordance with EN 12402.

Procedure

7.1
7.1.1

Preparation of the test solution

Dissolution

Weigh (20,00  0,01) g of the laboratory sample and transfer this test portion into a 250 ml tall-form beaker. Add
60 ml of nitric acid (5.2.3), cover with a watch glass. Heat gently on a hot plate until dissolution of the test portion is
complete. Then make up to the volume to about 250 ml with water.
7.1.2

Co-precipitation with manganese dioxide

Add ammonia solution (5.4) dropwise to the beaker to adjust the pH of the solution to between 3 and 4
7.1.2.1
using a pH meter.
Add 2 ml manganese nitrate solution (5.6) and bring to the boil. While still boiling, add 12 ml of
7.1.2.2
potassium permanganate solution (5.7) in three approximately equal portions, boiling gently for 2 min to 3 min after
each addition. Cover the beaker with a watch glass and allow to settle for 2 h at 50 C to 60 C. Filter the solution
through the filter membrane, wash several times with warm water, then discard the filtrate.
7.1.3

Test solution

Place a clean receiver back under the filter. With the suction off, add 3 ml of concentrated hydrochloric acid (5.3.1)
onto the filter membrane and wait until the dissolution of the precipitate is complete. Apply suction until the solution
passes through. Repeat this operation using a further 2 ml of concentrated hydrochloric acid (5.3.1). Finally, rinse
the filter twice with water, using not more than 10 ml in total. Transfer the filtrate into a 20 ml volumetric flask, make
up to the mark with water and mix thoroughly.

7.2

Preparation of the synthetic test solution

This solution is used to determine the recovery rate of the analyte.

Weigh (20,00 0,01) g of pure lead (5.5) and transfer into a 400 ml beaker. Add the appropriate volume of the
relevant standard solution (5.8) to simulate the analyte content to be determined in the lead sample.
Add 60 ml of nitric acid (5.2.3), cover with a watch glass and heat gently until the dissolution is complete. Then
proceed according to 7.1.2 and 7.1.3.

ENV 14138:2001 (E)

EXAMPLE 1
Addition of 2 ml of the standard solution (10 mg/l) (5.8.3) corresponds to a simulated analyte content of
0,0001 % m/m in the sample.
EXAMPLE 2
Addition of 5 ml of the standard solution (100 mg/l) (5.8.2) corresponds to a simulated analyte content of
0,0025 % m/m in the sample.
NOTE

7.3

The recovery rate is normally over 0,9.

Preparation of the blank test solution

Carry out a blank test in parallel with the preparation of the test solution, following the same procedure (7.1), but
omitting the test portion.

7.4

Preparation of calibration solutions

To each of six 200 ml volumetric flasks (4.2.1), labelled 0 to 5, add 50 ml of concentrated hydrochloric acid (5.3.1).
Then, using one-mark pipettes, add to the flasks respectively the volumes of the relevant standard solution of the
analyte (5.8.1 to 5.8.4) given in Table 2 or Table 3. Make up to the mark with water and mix thoroughly.
Table 2 Calibration solutions - analyte concentration 0,25 mg/l to 5 mg/l
Calibration solution number

Volume of analyte standard solution (10 mg/l) in the 200 ml

flask (ml)

10

20

Volume of analyte standard solution (100 mg/l) in the

200 ml flask (ml)

10

Analyte concentration in the solution (mg/l)

0, 25

0,5

2,5

Corresponding analyte content in the sample (% m/m)

0,000025

0,00005

0,0001

0,00025

0,0005

Table 3 Calibration solutions - analyte concentration 2,5 mg/l to 50 mg/l

Calibration solution number

Volume of analyte standard solution (100 mg/l) in the

200 ml flask (ml)

10

20

Volume of analyte standard solution (1g/l) in the 200 ml

flask (ml)

10

Analyte concentration in the solution (mg/l)

2,5

10

25

50

Corresponding analyte content in the sample (% m/m)

0,00025

0,0005

0,001

0,0025

0,005

8
8.1

Determination of elements by FAAS

General

Optimise the spectrometer following the manufacturer's manual (see also ISO/DIS 13204-2 and ISO/DIS 13204-3),
using the wavelength and the type of flame listed for each analyte in Table 4. All the measurements shall be
repeated at least twice. The average of these replicate values is the absorbance of the solution.

Table 4 Wavelength and type of flame used for each analyte

10

Analyte

Wavelength
(nm)

Type of flame

As

193,7

nitrous oxide/acetylene, reducinga

Sb

206,8

air/acetylene, oxidising

ENV 14138:2001 (E)

Se

196,0

nitrous oxide/acetylene, highly reducinga

Sn

224,6

nitrous oxide/acetylene, highly reducinga

Te

214,3

air/acetylene, oxidising

Alternatively, an air/hydrogen flame may be used. In this case, follow all the special safety
precautions.

8.2

Calibration and measurement of the test solution

For computerised spectrometers, enter the relevant parameters for the calibration solutions (7.4), the
8.2.1
blank test solution (7.3), the test solution (7.1), and the synthetic test solution (7.2). Aspirate the calibration
solutions (7.4) in order of increasing concentration, the blank test solution (7.3), the test solution (7.1), and the
synthetic test solution (7.2). Read the average analyte concentration of each test solution.
8.2.2 For manual spectrometers, aspirate the calibration solutions (7.4) in order of increasing concentration, the
blank test solution (7.3), the test solution (7.1), and the synthetic test solution (7.2). Plot the calibration graph of
absorbance against concentration (mg/l). Convert the absorbance value of each test solution into analyte
concentration using this graph.

8.3

Expression of results

8.3.1

Analyte recovery rate

For computerised spectrometers, the analyte content (A % m/m) for the synthetic test solution (7.2) is given directly
by the computer, in percentage by mass.
For manual spectrometers, the analyte content measured for the synthetic test solution (7.2) is given by the
following formula :
A % (m/m) 

V(a  b)
m  10 4

where
A

is the measured analyte content, expressed in % (m/m) ;

is the volume of the synthetic test solution in millilitres (ml) ;

is the concentration of analyte in the synthetic test solution, in milligrams per litre (mg/l) ;

is the concentration of analyte in the blank test solution, in milligrams per litre (mg/l) ;

is the mass of the synthetic test portion (= 20 g).

Then the analyte recovery rate is : R 

A
c

where
c
8.3.2

is the simulated analyte content expressed in % (m/m).

Analyte content in the sample

a)

For computerised spectrometers, the analyte content for the test solution given directly by the computer, in
percentage by mass, shall be divided by the value of the analyte recovery rate (R) to give the analyte content
in the sample ;

b)

for manual spectrometers, the analyte content in the laboratory sample is given by the following formula :

11

ENV 14138:2001 (E)

A%(m/m) 

V(a  b)
m  10 4  R

where
A

is the analyte (element to be determined) ;

is the volume of the test solution in millilitres (ml) ;

is the concentration of analyte in the test solution, in milligrams per litre (mg/l) ;

is the concentration of analyte in the blank test solution, in milligrams per litre (mg/l) ;

is the mass of the test portion in grams (g) ;

is the analyte recovery rate.

NOTE
In accordance with the status of an European Standard, precision data will be included when the results of the
precision tests are available.

9
9.1

Determination of elements by ICP-ES

General

Optimise the spectrometer following the manufacturer's manual (see also ISO/DIS 12235-2). Table 5 lists the
recommended wavelengths for each analyte.
All the measurements shall be repeated at least twice.
Table 5 Recommended wavelengths for each analyte
Analyte

Wavelengths
(nm)
(n = optical order)

As

189,042
193,696

Sb

206,834 / n=2

Se

196,090 / n=2

Sn

242,949 / n=2
283,998

Te

9.2

214,282 / n=2

Calibration and measurement of the test solution

Enter the relevant parameters for the calibration solutions (7.4), the blank test solution (7.3), the test solution (7.1)
and the synthetic test solution (7.2). Aspirate the calibration solutions (7.4) in order of increasing concentration, the
blank test solution (7.3), the test solution (7.1) and the synthetic test solution (7.2). Read the average analyte
concentration of each test solution.

12

ENV 14138:2001 (E)

9.3

Expression of results

9.3.1

Analyte recovery rate

The analyte content (A % m/m) for the synthetic test solution is given directly by the computer, as an average of the
replicated measurements.
Then the analyte recovery rate R is :
R

A
c

where
A

is the measured analyte content, expressed in % (m/m) ;

is the simulated analyte content expressed in % (m/m).

9.3.2

Analyte content in the sample

The analyte content for the test solution given directly by the computer (A % m/m) shall be divided by the value of
the analyte recovery rate (R) to give the analyte content in the sample.
NOTE
In accordance with the status of an European Prestandard, precision data will be included when the results of the
precision tests are available.

10 Test report
The test report shall include the following information :
a)

name of the laboratory ;

b)

identification of the sample ;

c)

results of the analysis ;

d)

date of the analysis ;

e)

reference number of this European Standard (ENV 14138) ;

f)

signature of the laboratory manager or other responsible person.

However, if the certificates are prepared by a suitable data processing system, the signature may be replaced by
an indication of the name and the position of the person responsible for validating the document.

13

ENV 14138:2001 (E)

Bibliography

ENV 14029, Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively
coupled plasma emission spectrometry (ICP-ES), after separation of the lead matrix.

14

DD ENV
14138:2001

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