DD ENV 14138-2001

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DRAFT FOR DEVELOPMENT DD ENV14138:2001

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

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EUROPEAN PRESTANDARD

PRÉNORME EUROPÉENNE

EUROPÄISCHE VORNORM

ENV 14138

December 2001

ICS 77.120.60

English version

Lead and lead alloys - Analysis by flame atomic absorptionspectrometry (FAAS) or inductively coupled plasma emissionspectrometry (ICP-ES), after separation by co-precipitation

Plomb et alliages de plomb - Analyse par spectrométried'absorption atomique dans la flamme (FAAS) ou par

spectrométrie d'émission à plasma inductif couplé (ICP-ES), après séparation par co-précipitation

Blei und Bleilegierungen - Analyse durch Flammen-Atomabsorptionsspektrometrie (FAAS) oder Emission-

Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES),nach Abtrennung durch Mitfällung

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 theircomments, 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 promptlyat national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the finaldecision 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

C OM ITÉ EUR OPÉEN DE NOR M ALISATION

EUR OPÄISC HES KOM ITEE FÜR NOR M UNG

Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2001 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.

Ref. No. ENV 14138:2001 E

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Contents

pageForeword......................................................................................................................................................................4

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

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

3 Principle..........................................................................................................................................................53.1 Preparation of the test solution....................................................................................................................53.2 Instrumental techniques ...............................................................................................................................63.2.1 Flame atomic absorption spectrometry (FAAS) .........................................................................................63.2.2 Inductively coupled plasma emission spectrometry (ICP-ES)..................................................................6

4 Apparatus .......................................................................................................................................................64.1 General ............................................................................................................................................................6

4.2 Volumetric glassware....................................................................................................................................64.3 Filtration system............................................................................................................................................64.4 Instruments.....................................................................................................................................................64.4.1 Flame atomic absorption spectrometer ......................................................................................................64.4.2 Inductively coupled plasma emission spectrometer .................................................................................7

5 Reagents.........................................................................................................................................................75.1 General ............................................................................................................................................................75.2 Nitric acid (HNO3) ..........................................................................................................................................7

5.2.1 Concentrated nitric acid................................................................................................................................75.2.2 Nitric acid 1:1 (V/V ) ........................................................................................................................................75.2.3 Nitric acid 1:2 (V/V ) ........................................................................................................................................75.3 Hydrochloric acid (HCl).................................................................................................................................7

5.3.1 Concentrated hydrochloric acid...................................................................................................................75.3.2 Hydrochloric acid 1:1 (V/V ) ...........................................................................................................................75.4 Ammonia solution..........................................................................................................................................75.5 Pure lead .........................................................................................................................................................75.6 Manganese nitrate solution ..........................................................................................................................85.7 Potassium permanganate solution ..............................................................................................................85.8 Standard solutions ........................................................................................................................................85.8.1 Standard solutions (1g/l)...............................................................................................................................85.8.2 Standard solutions (100 mg/l).......................................................................................................................85.8.3 Standard solutions (10 mg/l).........................................................................................................................95.8.4 Multi-element solutions (either 10 mg/l or 100 mg/l) ..................................................................................9

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

7 Procedure .......................................................................................................................................................97.1 Preparation of the test solution....................................................................................................................97.1.1 Dissolution......................................................................................................................................................97.1.2 Co-precipitation with manganese dioxide...................................................................................................97.1.3 Test solution...................................................................................................................................................97.2 Preparation of the synthetic test solution...................................................................................................97.3 Preparation of the blank test solution .......................................................................................................107.4 Preparation of calibration solutions ..........................................................................................................10

8 Determination of elements by FAAS..........................................................................................................108.1 General ..........................................................................................................................................................108.2 Calibration and measurement of the test solution...................................................................................118.3 Expression of results ..................................................................................................................................11

8.3.1 Analyte recovery rate ..................................................................................................................................118.3.2 Analyte content in the sample....................................................................................................................11

9 Determination of elements by ICP-ES .......................................................................................................129.1 General ..........................................................................................................................................................129.2 Calibration and measurement of the test solution...................................................................................12

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9.3 Expression of results ..................................................................................................................................139.3.1 Analyte recovery rate ..................................................................................................................................139.3.2 Analyte content in the sample....................................................................................................................13

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

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

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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 followingcountries 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 umpiremethods in cases of a dispute. The importance of either application, and the paramount issue of safety, requiresthat they should only be carried out by fully-trained analysts who are experienced in all relevant techniques and theprecautions 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 apparatusor reagent is referenced.

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1 Scope

This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductivelycoupled plasma emission spectrometry (ICP-ES) for the determination of elements at low content in lead for theranges 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

Ranges of applications(% m/m )

Element

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 lowcontent in lead. They are also recommended for the analysis of Certified Reference Materials (CRM) andReference Materials (RM) which are used in analysis according to ENV 12908.

2 Normative references

This European Prestandard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanPrestandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication 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 Principle

3.1 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.

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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 relevantwavelength (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 emissionspectrometer ;

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

comparison with that of calibration solutions of the same element.

4 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 ISO1042 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 648class A.

4.3 Filtration system

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

4.4 Instruments

4.4.1 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) orelectrode-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 (seealso 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 beexhausted externally.

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4.4.2 Inductively coupled plasma emission spectrometer

Inductively coupled plasma emission spectrometer (ICP-ES), either a simultaneous instrument with the relevantwavelengths installed or a sequential instrument where a monochromator system allows the selection ofwavelengths (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 beexhausted externally.

5 Reagents

5.1 General

For all stages of analysis, unless otherwise stated, use only reagents of recognised analytical grade, preferablywith 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 Nitric acid (HNO3)

5.2.1 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 Hydrochloric acid (HCl)

5.3.1 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 cleanall 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 besignificant to the determination required.


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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 untildissolved. 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 Standard solutions (1g/l)

5.8.1.1 General

Either use commercially available certified standard solutions or prepare standard solutions as described in 5.8.1.2to 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 intoa 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 iscomplete. 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 proceedstoo vigorously. Allow to cool, transfer to a 1 000 ml volumetric flask (4.2.1) then make up to the mark with water andmix 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 concentratedhydrochloric acid (5.3.1), cover with a watch glass and heat gently until dissolution is complete. Allow to cool, thentransfer 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 mixthoroughly.

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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 mixthoroughly.

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) ofthe elements required into a 1 000 ml volumetric flask (4.2.1). Add the appropriate volume of acid, then make up tothe mark with water and mix thoroughly.

Each multi-element solution (10 mg/l) shall be prepared on the day of use.

6 Sampling and sample preparation

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

7 Procedure

7.1 Preparation of the test solution

7.1.1 Dissolution

Weigh (20,00 0,01) g of the laboratory sample and transfer this test portion into a 250 ml tall-form beaker. Add60 ml of nitric acid (5.2.3), cover with a watch glass. Heat gently on a hot plate until dissolution of the test portion iscomplete. Then make up to the volume to about 250 ml with water.

7.1.2 Co-precipitation with manganese dioxide

7.1.2.1 Add ammonia solution (5.4) dropwise to the beaker to adjust the pH of the solution to between 3 and 4using a pH meter.

7.1.2.2 Add 2 ml manganese nitrate solution (5.6) and bring to the boil. While still boiling, add 12 ml ofpotassium permanganate solution (5.7) in three approximately equal portions, boiling gently for 2 min to 3 min aftereach addition. Cover the beaker with a watch glass and allow to settle for 2 h at 50 °C to 60 °C. Filter the solutionthrough 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 solutionpasses through. Repeat this operation using a further 2 ml of concentrated hydrochloric acid (5.3.1). Finally, rinsethe filter twice with water, using not more than 10 ml in total. Transfer the filtrate into a 20 ml volumetric flask, makeup 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 therelevant 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. Thenproceed according to 7.1.2 and 7.1.3.


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EXAMPLE 1 Addition of 2 ml of the standard solution (10 mg/l) (5.8.3) corresponds to a simulated analyte content of0,0001 % 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 of0,0025 % m/m in the sample.

NOTE The recovery rate is normally over 0,9.

7.3 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), butomitting 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 theanalyte (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 0 1 2 3 4 5

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

0 5 10 20 0 0

Volume of analyte standard solution (100 mg/l) in the200 ml flask (ml)

0 0 0 0 5 10

Analyte concentration in the solution (mg/l) 0 0, 25 0,5 1 2,5 5

Corresponding analyte content in the sample (% m/m) 0 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 0 1 2 3 4 5

Volume of analyte standard solution (100 mg/l) in the200 ml flask (ml)

0 5 10 20 0 0

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

0 0 0 0 5 10

Analyte concentration in the solution (mg/l) 0 2,5 5 10 25 50

Corresponding analyte content in the sample (% m/m) 0 0,00025 0,0005 0,001 0,0025 0,005

8 Determination of elements by FAAS

8.1 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 berepeated 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

Analyte Wavelength

(nm)

Type of flame

As 193,7 nitrous oxide/acetylene, reducinga

Sb 206,8 air/acetylene, oxidising

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Se 196,0 nitrous oxide/acetylene, highly reducinga

Sn 224,6 nitrous oxide/acetylene, highly reducinga

Te 214,3 air/acetylene, oxidising

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

8.2 Calibration and measurement of the test solution

8.2.1 For computerised spectrometers, enter the relevant parameters for the calibration solutions (7.4), theblank test solution (7.3), the test solution (7.1), and the synthetic test solution (7.2). Aspirate the calibrationsolutions (7.4) in order of increasing concentration, the blank test solution (7.3), the test solution (7.1), and thesynthetic 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, theblank test solution (7.3), the test solution (7.1), and the synthetic test solution (7.2). Plot the calibration graph ofabsorbance against concentration (mg/l). Convert the absorbance value of each test solution into analyteconcentration 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 directlyby the computer, in percentage by mass.

For manual spectrometers, the analyte content measured for the synthetic test solution (7.2) is given by thefollowing formula :

410

m

b)V(a A % (m/m)

where

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

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

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

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

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

Then the analyte recovery rate is : c

A R

where

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

8.3.2 Analyte content in the sample

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

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

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Rm

b)V(a A%(m/m)

410

where

A is the analyte (element to be determined) ;

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

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

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

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

R is the analyte recovery rate.

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

9 Determination of elements by ICP-ES

9.1 General

Optimise the spectrometer following the manufacturer's manual (see also ISO/DIS 12235-2). Table 5 lists therecommended 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 214,282 / n =2

9.2 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, theblank test solution (7.3), the test solution (7.1) and the synthetic test solution (7.2). Read the average analyteconcentration of each test solution.

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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 thereplicated measurements.

Then the analyte recovery rate R

is :

c

A R

where

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

c 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 ofthe 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 theprecision 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 byan indication of the name and the position of the person responsible for validating the document.


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ENV 14138:2001 (E)

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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.


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DD ENV14138:2001

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DD ENV 14138-2001