Textiles and textile products - Determination of biocide additives – Part 2, Chlorophenol-based preservatives, method using gas chromatography

This document specifies a test method for the determination of the content of chlorophenol-based preservative agents in textile materials and articles composed of textile products, by chromatography.

Textilien und textile Erzeugnisse - Bestimmung von Biozid-Zusatzstoffen - Teil 2: Konservierungsmittel auf Chlorphenolbasis, Verfahren mittels Gaschromatographie

Dieses Dokument legt ein Verfahren zur Bestimmung des Gehaltes an freiem Pentachlorphenol (PCP) und Tetrachlorphenol- (TeCP), Trichlorphenol- (TriCP), Dichlorphenol- (DiCP) und Monochlorphenol- (MoCP) Iso
meren fest. Mit dem Verfahren werden darüber hinaus Chlorphenole aus Salzen und Estern freigesetzt. Das Verfahren ist anwendbar auf Textilien aus natürlichen und synthetischen Fasern, einschließlich beschichteter Gewebe und Kleidungsbestanteile (z.B. Knöpfe, Reißverschlüsse usw.).

Textiles et produits textiles - Détermination des additifs biocides - Partie 2 : Conservateurs à base de chlorophénol, méthode par chromatographie en phase gazeuse

Le présent document spécifie une méthode pour déterminer la teneur en pentachlorophénol (PCP) libre, et en isomères de tétrachlorophénol (TeCP), trichlorophénol (TriCP), dichlorophénol (DiCP) et monochlorophénol (MoCP). Le mode opératoire libère aussi des chlorophénols à partir de sels et d’esters. La méthode est applicable aux textiles naturels et synthétiques, y compris les étoffes enduites et les articles d’habillement (par exemple boutons, fermetures à glissière, etc.).

Tekstilije in tekstilni izdelki - Določevanje biocidnega dodatka - 2. del: Konzervansi na osnovi klorofenola, metoda z uporabo plinske kromatografije

General Information

Status
Not Published
Public Enquiry End Date
18-Oct-2022
Current Stage
4020 - Public enquire (PE) (Adopted Project)
Start Date
03-Aug-2022
Due Date
21-Dec-2022
Completion Date
24-Oct-2022

Relations

Buy Standard

Draft
oSIST prEN 17134-2:2022
English language
42 pages
sale 10% off
Preview
sale 10% off
Preview
e-Library read for
1 day

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 17134-2:2022
01-september-2022

Tekstilije in tekstilni izdelki - Določevanje biocidnega dodatka - 2. del: Konzervansi

na osnovi klorofenola, metoda z uporabo plinske kromatografije

Textiles and textile products - Determination of biocide additives – Part 2, Chlorophenol-

based preservatives, method using gas chromatography

Textilien und textile Erzeugnisse - Bestimmung von Biozid-Zusatzstoffen - Teil 2:

Konservierungsmittel auf Chlorphenolbasis, Verfahren mittels Gaschromatographie
Textiles et produits textiles - Détermination des additifs biocides - Partie 2 :
Conservateurs à base de chlorophénol, méthode par chromatographie en phase
gazeuse
Ta slovenski standard je istoveten z: prEN 17134-2
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
oSIST prEN 17134-2:2022 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN 17134-2:2022
---------------------- Page: 2 ----------------------
oSIST prEN 17134-2:2022
DRAFT
EUROPEAN STANDARD
prEN 17134-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2022
ICS 59.080.01 Will supersede EN 17134:2019
English Version
Textiles and textile products - Determination of biocide
additives - Part 2, Chlorophenol-based preservatives,
method using gas chromatography
Textilien und textile Erzeugnisse - Bestimmung von
Biozid-Zusatzstoffen - Teil 2: Konservierungsmittel auf
Chlorphenolbasis, Verfahren mittels
Gaschromatographie

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 248.

If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations

which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other

language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC

Management Centre has the same status as the official versions.

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

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17134-2:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
Contents
Page

European foreword ............................................................................................................................................. 4

1 Scope .......................................................................................................................................................... 6

2 Normative references .......................................................................................................................... 6

3 Terms and definitions ......................................................................................................................... 6

4 Abbreviations ......................................................................................................................................... 6

5 Principle ................................................................................................................................................... 7

6 Apparatus ................................................................................................................................................. 7

6.1 Gas chromatograph (GC), with mass selective detector (MSD). ........................................... 7

6.2 Analytical balance, weighing with an accuracy of 0,1 mg. ...................................................... 7

6.3 Heating block, sand bath or drying cabinet, suitable for a temperature of 90 °C ± 1 °C

in the KOH solution............................................................................................................................... 7

6.4 Gas-tight glass vials, for example headspace vials, (20 ml) . ................................................. 7

6.5 GC vials, about 2 ml. .............................................................................................................................. 7

6.6 Pasteur pipettes, graduated pipettes, suitable autopipettes ................................................ 7

6.7 Vortex shaker ......................................................................................................................................... 7

6.8 Horizontal shaker, capable of at least 200 min ....................................................................... 7

7 Reagents ................................................................................................................................................... 7

7.1 General ...................................................................................................................................................... 7

7.2 Chlorophenol mixture Stock solution ............................................................................................ 7

7.3 Tetrachloroguaiacol (tetrachloro-o-methoxyphenol) CAS number: 2539-17-5 ............ 9

7.4 Isotope labelled internal standards ............................................................................................... 9

7.5 n-Hexane, for residue analysis. ........................................................................................................ 9

7.6 Potassium hydroxide solution (KOH), aqueous solution (1 mol/l). ................................... 9

7.7 Tetrachloroguiacol (TCG) solution, at a concentration of 1 μg/ml in acetonitrile

(internal standard for injection control)...................................................................................... 9

7.8 Stock solution isotope-labelled internal standards in KOH solution, each 0,1 mg/ml 9

7.9 Extraction solution (containing isotope-labelled internal standards).............................. 9

7.10 Potassium carbonate (K CO ), aqueous solution (0,1 mol/l). ............................................... 9

2 3

7.11 Acetic anhydride (C H O ), for analysis. .....................................................................................10

4 6 3

7.12 Water, grade 3, according to ISO 3696. .......................................................................................10

7.13 Acetone ...................................................................................................................................................10

7.14 Acetonitrile ............................................................................................................................................10

7.15 Working solution calibration level 1, for daily calibration .................................................10

7.16 Working solution calibration level 2, for daily calibration .................................................10

7.17 Working solution calibration level 3, for daily calibration .................................................10

7.18 Working solution calibration level 4, for daily calibration .................................................10

7.19 Working solution calibration level 5, for daily calibration. ................................................10

8 Sampling .................................................................................................................................................10

9 Procedure...............................................................................................................................................10

9.1 General ....................................................................................................................................................10

9.2 Extraction with KOH ...........................................................................................................................10

9.3 Extractive acetylation ........................................................................................................................11

9.4 Derivatization of the chlorophenol mixtures and the TCG standards (calibration for

daily use) ................................................................................................................................................11

---------------------- Page: 4 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)

9.5 Gas chromatography (GC)................................................................................................................ 11

10 Expression of results ......................................................................................................................... 12

10.1 General ................................................................................................................................................... 12

10.2 Calculation of the individual chlorphenols in the test specimen ...................................... 12

10.3 Reliability of the procedure ............................................................................................................ 12

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

Annex A (informative) Chromatographic test conditions ................................................................. 14

A.1 Preliminary remarks ......................................................................................................................... 14

A.2 Gas chromatography with mass selective detector (GC-MSD) ........................................... 14

Annex B (informative) Procedure characteristics ............................................................................... 16

B.1 General ................................................................................................................................................... 16

B.2 Ring test results ................................................................................................................................... 16

B.2.1 Results of the first ring test ............................................................................................................. 16

B.2.2 Results of the second ring test from one real test specimen and two spikes of the real

test specimen, with 4 laboratories ............................................................................................... 17

B.3 Influence of standard solutions ..................................................................................................... 25

B.4 Influence of internal standards on contents of pentachlorophenol and other

chlorophenols ...................................................................................................................................... 31

Annex C (informative) Verification method for free mono- and dichlorophenol .................... 41

C.1 General ................................................................................................................................................... 41

C.2 Procedure .............................................................................................................................................. 41

---------------------- Page: 5 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
European foreword

This document (prEN 17134-2:2021) has been prepared by Technical Committee CEN/TC 248 “Textiles

and textile products”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 17134:2019.
---------------------- Page: 6 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
Introduction

In Europe, according to REGULATION (EU) 2019/1021[1] of the European Parliament and of the Council

of 20 June 2019 on persistent organic pollutants pentachlorophenol (PCP) and its salts and esters as

constituents of articles are prohibited. According to COMMISSION DELEGATED REGULATION (EU)

2021/277 of 16 December 2020 amending Annex I to Regulation (EU) 2019/1021 of the European

Parliament and of the Council on persistent organic pollutants as regards pentachlorophenol and its salts

and esters, articles containing PCP in concentrations equal or lower than 5 mg/kg are allowed.

Further chlorinated phenols are restricted by voluntary specifications (ecolabel criteria, industry

initiatives and standards).

This document specifies a method in which chlorophenols (CP) are acetylated before chromatographic

detection and the amount of detected chlorophenol acetate is quantified by a correction with an internal

standard.

WARNING - The use of this document involves hazardous materials. It does not purport to address all of

the safety or environmental problems associated with its use. It is the responsibility of users of this

document to take appropriate measures to ensure the safety and health of personnel and the

environment prior to application of the document, and fulfil statutory and regulatory requirements for

this purpose.
---------------------- Page: 7 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
1 Scope

This document specifies a method to determine the content of free pentachlorophenol (PCP), and

tetrachlorophenol- (TeCP), trichlorophenol- (TriCP), dichlorophenol- (DiCP), monochlorophenol-

(MoCP) isomers. The procedure also releases chlorophenols from salts and esters. The method is

applicable to natural and synthetic textiles, including coated fabrics and clothing components (e.g.

buttons, zippers, etc.).
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

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

ISO 3696, Water for analytical laboratory use — Specification and test methods

3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Abbreviations
The following abbreviations are used in this document for chlorophenols:
CP chlorophenols
MoCP monochlorophenol
DiCP dichlorophenol
TriCP trichlorophenol
TeCP tetrachlorophenol
PCP pentachlorophenol
2-MoCP-d4 2-chlorophenol-d
2,3-DiCP-d3 2,3-dichlorophenol-d
TeCP-13C6 2,3,4,6-tetrachlorophenol- C
PCP-C13 pentachlorophenol- C
TCG tetrachloroguaiacol (= tetrachloro-o-methoxyphenol)

The following abbreviations are used in this document for the designation of textile fibres:

---------------------- Page: 8 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
CO cotton
PES polyester
CV viscose
EL elastane
LI linen
PA polyamide
5 Principle

The sample is extracted with a potassium hydroxide solution (KOH solution) for 16 h at 90 ° C.

During subsequent extractive derivatization with n-hexane and acetic acid anhydride, CPs are acetylated

and the chlorinated acetates are analyzed using gas chromatography with a mass-selective detector

13 2

(MSD). The quantitative determination is made by correction with C and H labelled internal standards.

13 13

For pentachlorophenol, the C derivative of PCP is used, for tetrachlorophenols the C derivative of

2,3,4,6-tetrachlorophenol, for tri- and dichlorophenols 2,3-dichlorophenol-d and for

monochlorophenols 2-chlorophenol-d . TCG serves as an internal standard for injection control.

6 Apparatus
6.1 Gas chromatograph (GC), with mass selective detector (MSD).
6.2 Analytical balance, weighing with an accuracy of 0,1 mg.

6.3 Heating block, sand bath or drying cabinet, suitable for a temperature of 90 °C ± 1 °C in the KOH

solution.
6.4 Gas-tight glass vials, for example headspace vials, (20 ml) .
6.5 GC vials, about 2 ml.
6.6 Pasteur pipettes, graduated pipettes, suitable autopipettes
6.7 Vortex shaker
6.8 Horizontal shaker, capable of at least 200 min
7 Reagents
7.1 General
Unless otherwise stated, chemicals of analytical grade shall be used.
7.2 Chlorophenol mixture Stock solution

A mixture of chlorophenols which, at a concentration of 50 μg/ml in a suitable solvent (for example

---------------------- Page: 9 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
Acetonitrile) contains the following isomers:
2-chlorophenol CAS number: 95-57-8
3-chlorophenol CAS number: 108-43-0
4-chlorophenol CAS number: 106-48-9
2,3-dichlorophenol CAS number: 576-24-9
2,4-dichlorophenol CAS number: 120-83-2
2,5-dichlorophenol CAS number: 583-78-8
2,6-dichlorophenol CAS number: 87-65-0
3,4-dichlorophenol CAS number: 95-77-2
3,5-dichlorophenol CAS number: 591-35-5
2,3,4-trichlorophenol CAS number: 15950-66-0
2,3,5-trichlorophenol CAS number: 933-78-8
2,3,6-trichlorophenol CAS number: 933-75-5
2,4,5-trichlorophenol CAS number: 95-95-4
2,4,6-trichlorophenol CAS number: 88-06-2
3,4,5-trichlorophenol CAS number 609-19-8
2,3,4,5-tetrachlorophenol CAS number 4901-51-3
2,3,4,6-tetrachlorophenol CAS number: 58-90-2
2,3,5,6-tetrachlorphenol CAS number: 935-95-5
pentachlorophenol CAS number: 87-86-5

NOTE This mixture of chlorophenols is available from laboratory chemical suppliers.

---------------------- Page: 10 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
7.3 Tetrachloroguaiacol (tetrachloro-o-methoxyphenol) CAS number: 2539-17-5
7.4 Isotope labelled internal standards
2-chlorophenol-d CAS number: 93951-73-6
2,3-dichlorophenol-d CAS number: 93951-74-7
2,3,4,6-tetrachlorophenol- C CAS number:1246820-81-4
pentachlorophenol- C CAS number: 85380-74-1

Instead of the isotope-labelled derivatives of tetra-, di- and monochlorophenol mentioned, other isotope-

labelled analogues of the same chlorination levels, e.g. 4-chlorophenol-d , may also be used as internal

standards.
7.5 n-Hexane, for residue analysis.
7.6 Potassium hydroxide solution (KOH), aqueous solution (1 mol/l).

Weigh 56,1 g KOH into a 1 l volumetric flask and dissolve with 100 ml water (7.12) (caution: heat

generation!). After cooling, fill up to 1 l with water (7.12).

7.7 Tetrachloroguiacol (TCG) solution, at a concentration of 1 μg/ml in acetonitrile

(internal standard for injection control)

Dissolve 10 mg TCG in 100 ml acetonitrile (7.14). Take 1,0 ml from this stock solution and dilute to 100 ml

with acetonitrile (7.14).

7.8 Stock solution isotope-labelled internal standards in KOH solution, each 0,1 mg/ml

Dissolve 10 mg of each isotope-labelled internal standard (7.4) in 100 ml KOH solution (7.6).

7.9 Extraction solution (containing isotope-labelled internal standards)

1,0 ml stock solution isotope-labelled internal standards (7.8) is filled up with KOH solution (7.6) in a 1 l

volumetric flask, the concentration of each of the isotope-labelled internal standards (7.4) is 0,1 µg/ml .

The concentration of isotope-labelled internal standards shall be adapted to the respective calibration

range of the chlorophenols (see solutions 7.15 to 7.19). If a more sensitive measuring instrument is used

and the calibration is lowered, then the concentration of isotope-labelled internal standards in the KOH

solution should also be reduced.
7.10 Potassium carbonate (K CO ), aqueous solution (0,1 mol/l).
2 3

Weigh 13,82 g K CO into a 1 l volumetric flask, dissolve with water (7.12) and fill up to 1 l.

2 3
---------------------- Page: 11 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
7.11 Acetic anhydride (C4H6O3), for analysis.
7.12 Water, grade 3, according to ISO 3696.
7.13 Acetone
7.14 Acetonitrile
7.15 Working solution calibration level 1, for daily calibration

30 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 10 ml volumetric

flask; the concentration of chlorophenols is 0,15 μg/ml.
7.16 Working solution calibration level 2, for daily calibration

400 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 10 ml volumetric

flask; the concentration of chlorophenols is 2,0 μg/ml.
7.17 Working solution calibration level 3, for daily calibration

800 μl stock solution chlorophenol mixture (7.2) are filled up with acetonitrile (7.14) in a 10 ml

volumetric flask; the concentration of chlorophenols is 4 μg/ml.
7.18 Working solution calibration level 4, for daily calibration

600 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 2 ml volumetric

flask; the concentration of chlorophenols is 15 μg/ml.
7.19 Working solution calibration level 5, for daily calibration.

1 000 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 2 ml volumetric

flask; the concentration of chlorophenols is 25 μg/ml.

The concentrations of the calibration solutions (7.15 to 7.19) are examples and should be adjusted

according to the specified limit values and the linearity of the device.
8 Sampling

From the material to be examined, a representative test specimen shall be taken and cut into pieces of

about 0,5 cm × 0,5 cm.
9 Procedure
9.1 General

If it is only required to test for free mono- and dichlorophenols, the procedure described in Annex C shall

be applied.
9.2 Extraction with KOH

Place approximately 1 g (minimum sample weight 0,2 g) of the cut test specimen (to the nearest 0,01 g)

in the reaction vessel (6.4). Add 10 ml extraction solution (7.9). After closing, the vessel is transferred to

a heating apparatus (6.3) and left for 16 h ± 15 min at (90 ± 1) °C. The temperature in the reaction vessel

is checked with extraction solution. If the test specimen to be examined is too voluminous to be

---------------------- Page: 12 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)

completely covered with KOH solution for the period of extraction, the test specimen shall be weighed

down with glass balls or a comparable inert object to ensure complete wetting, or a suitable larger

amount of extraction solution shall be added (take into account the different specimen weight to liquor

ratio in the calculation).

NOTE Deviations from the specified extraction time and temperature can lead to significant deviations in the

result.
9.3 Extractive acetylation

After extraction, the test specimen shall be cooled down to room temperature and shaken vigorously

(1 min vortex shaker (6.7) or 10 min horizontal shaker (6.8)). Transfer 4 ml of the KOH extraction

solution into a new reaction vessel (6.4) and add 6 ml potassium carbonate solution (7.10), 2 ml n-hexane

(7.5), 250 μl TCG solution (7.7) and 1 ml acetic acid anhydride (7.11).

After closing the vessel, shake it for 30 min at a shaking rate of at least 200 min on a horizontal shaker

(6.8). An efficient mixing of the phases shall be ensured.

After shaking, centrifugation may improve phase separation. The vessel is then opened carefully (caution:

overpressure!). Transfer an aliquot (for example 1 ml) from the upper phase to a GC vial (6.5) for analysis.

Take 4 ml of extraction solution and add 2 ml of n-hexane to reliably detect a value of 0,05 mg/kg

chlorophenols. For device configurations that allow lower limits of detection, the volume of extraction

solution used for acetylation may be reduced or the amount of n-hexane added may be increased. The

same volumes shall be used for calibration and test specimens. A validation with the changed conditions

shall be executed.
By reducing the weight of the test specimen higher limit values can be covered.

9.4 Derivatization of the chlorophenol mixtures and the TCG standards (calibration for

daily use)

100 μl of each chlorophenol working solution (7.15 to 7.19), 4 ml extraction solution (7.9), 6 ml

potassium carbonate solution (7.10), 2 ml n-hexane (7.5), 250 μl TCG solution (7.7) and 1 ml of acetic

acid anhydride (7.11) shall be added into a separate reaction vessel (6.4). After closing the vessel, shake

it for 30 min at a shaking rate of at least 200 min on a horizontal shaker (6.8). The vessel is centrifuged

after shaking and then carefully opened (caution: overpressure!). Transfer an aliquot (for example 1 ml)

from the upper phase from each reaction vessel to a GC vial (6.5) for analysis. Depending on the device, a

basic calibration is carried out for detection and determination and for the linear working area.

9.5 Gas chromatography (GC)

Various types of gas chromatographic equipment may be used. The chromatography conditions specified

in Annex A are an example of parameters that have been successfully applied in the analysis.

---------------------- Page: 13 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
10 Expression of results
10.1 General

The quantitative determination is made using multi-point calibration with at least three points.

The calibration curve is constructed by plotting the area units against the known standard concentrations

and correcting for the isotope-labelled internal standards. Pentachlorophenol- C is used as an internal

standard for pentachlorophenol, 2,3,4,6-tetrachlorophenol- C for tetrachlorophenols, 2,3-

dichlorophenol-d for tri- und dichlorophenols and 2-chlorophenol-d for monochlorophenols. From the

3 4

calibration curve, the concentration of chlorophenol, in μg/ml (ρ ), is interpolated.

If the recovery of the isotope-labelled internal standards due to matrix effects is lower than the specified

recovery of the laboratory's quality guideline, other valid methods, such as addition procedures, may be

used to determine the quantitative result. In exceptional cases, at the discretion of the person responsible

for the laboratory, a value may also be calculated against TCG. However, if possible, the calculation against

isotope-labelled chlorophenols should always be preferred. For materials with very low recoveries of the

isotope-labelled internal standards, 5 ml n-hexane (7.5), 625 μl TCG solution (7.7) and 2,5 ml acetic

anhydride (7.11) may be added to the total extraction solution containing the specimen in the same vessel

and then proceed as described above. For the following instrumental analysis according to 9.5 and

Annex A, the n-hexane phase obtained here is significantly more matrix-loaded than the phase according

to 9.3, but empirically the recoveries of the isotope-labelled internal standards improve.

Values calculated via TCG shall be reported separately in the test report.
10.2 Calculation of the individual chlorphenols in the test specimen

The content of chlorophenol is calculated as a mass portion w, in mg/kg, of the test specimen according

to equation (1):
𝜌𝜌 ×𝑉𝑉 ×𝑉𝑉
s KOH n-hexane
𝑤𝑤= (1)
𝐴𝐴 ×𝑚𝑚
KOH E
where
w the concentration of chlorophenol found, in mg/kg;
ρ the interpolated chlorophenol concentration, in μg/ml measured solution;

V the volume of the KOH extraction solution according to 9.2, in ml (here 10 ml);

KOH
A aliquot of the KOH extraction solution according to 9.2, in ml (here 4 ml);
KOH
V the volume of the added amount of n-hexane, in ml (here 2 ml);
n-hexane
m the mass of the test specimen, in g.
10.3 Reliability of the procedure
For the reliability (precision) of the procedure, see Annex B.
---------------------- Page: 14 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
11 Test report
The test report shall include at least the following information:
a) reference to this document, i.e. EN 17134-2:202X;
b) kind, origin and designation of the sample;

c) the result for each CP, in mg/kg, rounded to a maximum of 2 significant figures with a maximum of 2

decimal points;
d) any deviations from the given procedure;
e) an indication whether values were calculated via TCG and, if so, which;
f) date of analysis.
---------------------- Page: 15 ----------------------
oSIST prEN 17134-2:2022
prEN 17134-2:2022 (E)
Annex A
(informative)
Chromatographic test conditions
A.1 Preliminary remarks

Due to possible differences in the instrumental equipment (6.1) of the laboratories, no general

requirements for gas chromatographic analyses can be made. The following chromatographic conditions

are an example of the parameters that have been successfully applied in this method.

A.2 Gas chromatography with mass
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.