oSIST prEN 17137:2023
(Main)Textiles - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes
Textiles - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes
This document specifies a test method (using gas chromatography with mass selective detector for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in textile materials (fibres, yarns, fabrics), coated fabrics and plastics.
Textilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzolen und Chlortoluolen
Dieses Dokument legt ein auf Gaschromatographie mit massenselektivem Detektor (GC-MSD) beruhendes Prüfverfahren für den Nachweis und die quantitative Bestimmung von Chlorbenzolen, Chlortoluolen und α-chlorierten Toluolen in Fasern, Garnen, textilen Flächengebilden, beschichteten Geweben und Kunststoffen fest.
ANMERKUNG1 CEN/TR16741 legt fest, welche Materialien für dieses Prüfverfahren anwendbar sind.
Textiles et produits textiles - Détermination de la teneur de composés à base de chlorobenzènes et chlorotoluènes
Le présent document spécifie une méthode d’essai utilisant la chromatographie en phase gazeuse avec détecteur sélectif de masse (GC-MSD) pour la détection et la quantification des chlorobenzènes, des chlorotoluènes et des toluènes α-chlorés dans les fibres, les fils, les supports textiles, les supports textiles revêtus et les matières plastiques.
NOTE 1 Le CEN/TR 16741 définit les matériaux applicables à cette méthode d’essai.
Tekstilije - Določevanje spojin na osnovi klorobenzenov in klorotoluenov
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN 17137:2023
01-september-2023
Tekstilije - Določevanje spojin na osnovi klorobenzenov in klorotoluenov
Textiles - Determination of the content of compounds based on chlorobenzenes and
chlorotoluenes
Textilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von
Chlorbenzolen und Chlortoluolen
Textiles et produits textiles - Détermination de la teneur de composés à base de
chlorobenzènes et chlorotoluènes
Ta slovenski standard je istoveten z: prEN 17137
ICS:
59.080.01 Tekstilije na splošno Textiles in general
oSIST prEN 17137:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 17137:2023
DRAFT
EUROPEAN STANDARD
prEN 17137
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2023
ICS Will supersede EN 17137:2018
English Version
Textiles - Determination of the content of compounds
based on chlorobenzenes and chlorotoluenes
Textiles - Détermination de la teneur de composés à Textilien - Bestimmung des Gehaltes von
base de chlorobenzènes et chlorotoluènes Verbindungen auf der Basis von Chlorbenzol und
Chlortoluol
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, Türkiye 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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17137:2023 E
worldwide for CEN national Members.
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Contents Page
European foreword . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Reagents . 5
6 Apparatus . 7
7 Sampling . 7
8 Procedure . 8
8.1 Extraction . 8
8.2 Determination by GC-MS or GC-MS/MS . 8
9 Expression of results . 8
9.1 Calculation . 8
9.2 Sum of chlorobenzenes and chlorotoluenes . 9
9.3 Reliability of the method . 9
10 Test report . 9
Annex A (informative) False positives . 10
A.1 False positives . 10
A.2 Occurrences of chlorobenzenes and chlorotoluenes . 10
A.3 Examples of false positives (not exhaustive) . 10
A.3.1 α-Chlorotoluene (benzyl chloride) as a degradation product of quaternary
ammonium salts . 10
[2]
A.3.2 1,2-Dichlorobenzene findings from synthesis residues . 10
A.3.3 Chlorobenzenes and chlorotoluenes released by dyestuff as degradation products . 11
Annex B (informative) Test procedures if false positive results of benzyl chloride derived
from benzalkonium chloride are suspected . 12
B.1 Confirmation of benzyl chloride derived from benzalkonium chloride by LC-DAD . 12
B.1.1 Principle . 12
B.1.2 Reagents . 12
B.1.2.1 Water, grade 3 according to EN ISO 3696 or LC-MS grade. . 12
B.1.2.2 Methanol, LC-MS grade, CAS number 67-56-1 . 12
B.1.2.3 Ammonium formate, CAS number 540-69-2 . 12
B.1.2.4 Benzyl chloride, CAS number 100-44-7 . 12
B.1.2.5 Benzalkonium Chloride, CAS number 63449-41-2 (for qualitative screening) . 12
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B.1.3 Apparatus . 12
B.1.3.1 Liquid Chromatograph with Diode-Array Detection (LC-DAD). . 12
B.1.4 Procedure . 12
B.1.4.1 Sampling Procedure . 12
B.1.4.2 Extraction . 12
B.1.4.3 Calculation . 13
B.1.4.4 Chromatography parameters (example) . 13
B.2 Removal of benzalkonium chloride by water extraction with subsequent GC-MS
analysis . 14
Annex C (informative) Parameter for instrumental analyses . 15
C.1 Gas chromatograph/single quad mass spectrometer (GC-MS) . 15
C.2 Gas chromatograph/triple quad mass spectrometer (GC-MS/MS) . 17
Annex D (informative) Reliability of the method . 19
D.1 General . 19
D.2 Accuracy . 19
D.3 Detection Limit (LOD) and Quantification Limit (LOQ) . 20
D.4 Repeatability . 21
D.5 Reproducibility . 22
D.6 Robustness . 23
D.7 Selectivity . 24
D.8 Extraction Efficiency . 25
Bibliography . 26
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European foreword
This document (prEN 17137:2023) 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 17137:2018.
prEN 17137:2023 includes the following significant technical changes with respect to EN 17137:2018:
– The clauses have been reorganised and renamed according to CEN/CENELEC Internal Regulations
Part 3:2019;
– Clause 1: The scope has been extended to α-chlorinated toluenes and rephrased;
– Clause 2: EN ISO 4787 has been added;
– Subclauses 3.1 and 3.2 have been deleted;
– Clause 4 has been rephrased;
– Clause 5 has been reorganised and rephrased;
– Subclause 5.2: Several α-chlorinated toluenes have been added in Table 1, and Table 1 has been
reorganised.
– Clause 6 has been reorganised and rephrased;
– Subclause 6.6: Triple-quadrupole mass spectrometer has been added as a suitable detector;
– Clause 7 has been reorganised and rephrased;
– Clause 8 has been reorganised and rephrased;
– Subclause 9.2: A clause on how to calculate the sum of chlorobenzenes and chlorotoluenes has been
added;
– Subclause 9.3: The limit of quantification of the test method is given;
– Clause 10 has been reorganised and rephrased;
– Annex A: A description on the occurrence of false positives has been added;
– Annex B: Test procedure if false positives are suspected has been added;
– Annex C: Former Annex A has become Annex C,
– Annex C.2: Instrumental Conditions and characteristic masses for quantification with mass
chromatograph/triple quad mass spectrometer (GC-MS/MS) have been added;
– Annex D: Former Annex B has become Annex D;
– Bibliography: Further references have been added.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Republic of North Macedonia, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands,
Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
the United Kingdom.
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1 Scope
This document specifies a test method using gas chromatography with mass selective detector (GC-
MSD) for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in
fibres, yarns, fabrics, coated fabrics and plastics.
NOTE 1 CEN/TR 16741 defines which materials are applicable to this test method.
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.
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987)
EN ISO 4787, Laboratory glass and plastic ware - Volumetric instruments - Methods for testing of capacity
and for use (ISO 4787:2021)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology 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 Principle
The sample is cut into small pieces and extracted with dichloromethane in a sealed vial at a defined
temperature in an ultrasonic bath. An aliquot of the extract is analysed for the substances listed in
Table 1 using a GC-MSD.
5 Reagents
Unless otherwise specified, all reagents shall be of a recognised analytical grade.
®1 ®
5.1 Dichloromethane, CAS Registry Number (CAS RN ): 75-09-2
1
CAS Registry Number® (CAS RN®) is a trademark of CAS corporation. This information is given for the
convenience of users of this document and does not constitute an endorsement by CEN of the product named.
Equivalent products may be used if they can be shown to lead to the same results.
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5.2 Reference substances
Reference substances are listed in Table 1.
Table 1 — Reference substances
Substance
®
Substance CAS RN
number
Chlorobenzenes
1 Chlorobenzene 108-90-7
2 1,2-Dichlorobenzene 95–50–1
3 1,3-Dichlorobenzene 541–73–1
4 1,4-Dichlorobenzene 106–46–7
5 1,2,3-Trichlorobenzene 87–61–6
6 1,2,4-Trichlorobenzene 120–82–1
7 1,3,5-Trichlorobenzene 108–70–3
8 1,2,3,4-Tetrachlorobenzene 634–66–2
9 1,2,3,5-Tetrachlorobenzene 634–90–2
10 1,2,4,5-Tetrachlorobenzene 95–94–3
11 Pentachlorobenzene 608–93–5
12 Hexachlorobenzene 118–74–1
Chlorotoluenes
13 2-Chlorotoluene 95–49–8
14 3-Chlorotoluene 108–41–8
15 4-Chlorotoluene 106–43–4
16 2,3-Dichlorotoluene 32768–54–0
17 2,4-Dichlorotoluene 95–73–8
18 2,5-Dichlorotoluene 19398–61–9
19 2,6-Dichlorotoluene 118–69–4
20 3,4-Dichlorotoluene 95–75–0
21 3,5-Dichlorotoluene 25186-47-4
22 2,3,4-Trichlorotoluene 7359-72-0
23 2,3,5-Trichlorotoluene 56961-86-5
24 2,3,6-Trichlorotoluene 2077–46–5
25 2,4,5-Trichlorotoluene 6639–30–1
26 3,4,5-Trichlorotoluene 21472-86-6
27 2,3,4,5-Tetrachlorotoluene 1006-32-2
28 2,3,4,6-Tetrachlorotoluene 875-40-1
29 2,3,5,6-Tetrachlorotoluene 1006-31-1
30 Pentachlorotoluene 877–11–2
α-chlorinated toluenes
α-Chlorotoluene
31 100-44-7
α,α-Dichlorotoluene
32 98-87-3
33 α,α,α-Trichlorotoluene 98-07-7
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Substance
®
Substance CAS RN
number
34 α,α,2,6-Tetrachlorotoluene 81-19-6
35 α,α,α,2-Tetrachlorotoluene 2136-89-2
36 α,α,α,4-Tetrachlorotoluene 5216-25-1
Internal standard
37 2,4,5,6-Tetrachloro-m-xylene 877–09–8
5.3 Standard solutions
5.3.1 Target compound stock solutions
Based on its tasks, a laboratory shall decide which substances from Table 1 need to be determined.
Based on this decision, standard stock solutions for each substance (e.g., c = 100 μg/ml for each
substance) shall be available either as commercially available certified mixes or individual components
in solution or as self-prepared individual or mixed standard stock solutions of each substance (Table 1)
in dichloromethane (5.1).
EXAMPLE For standard stock solutions with concentrations of 100 μg/ml, weigh 25,0 mg of each
substance (Table 1) into a 250 ml volumetric flask, fill it up to the mark with dichloromethane (5.1.1)
and mix thoroughly to dissolve the substance completely.
5.4.2 Target compound working solution
Prepare a mixed working solution containing all required substances in a suitable concentration for
your GC-MSD system (e.g., c = 10 µg/ml).
5.4.3 Internal standard solution
Prepare an IS solution of a suitable concentration for your GC-MSD system (e.g., c = 1 µg/ml) by
dissolving 2,4,5,6-Tetrachloro-m-Xylene (Table 1, item 37) in dichloromethane (5.1).
6 Apparatus
The usual laboratory apparatus and laboratory glassware, according to EN ISO 4787, shall be used, in
addition to the following:
6.1 Analytical balance, with a precision of at least 0,1 mg.
6.2 Glass vials with tight closure, e.g., 40 ml.
6.3 Ultrasonic bath.
6.4 Polytetrafluoroethylene (PTFE) filter, at maximum 0,45 μm pore size.
6.5 GC vial with cap, e.g., 2 ml
6.6 Gas chromatograph (GC), coupled with single-quadrupole mass spectrometer (MS) or triple-
quadrupole mass spectrometer (MS/MS).
7 Sampling
7.1 Preparation of test specimens
The test specimen shall consist of a single material type (fibres, yarns, fabrics, coated fabrics or
plastics). Up to three test specimens (of equal mass) of the same material type can be tested together
taking into consideration the limits of quantification. Since different colours can contain different
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concentrations of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes, each coloured material
shall be considered as one test specimen. Multicoloured material with small pattern shall only be tested
as a single test specimen.
Cut the test specimen into pieces of about 0,3 cm to 0,5 cm edge length and store them in a sealed glass
vial (6.2) until further processing.
8 Procedure
8.1 Extraction
Weigh (2,0 ± 0,1) g of the specimen (7.1) in a glass vial (6.2), record the mass to the nearest 10 mg, add
20 ml internal standard solution (5.4.3) appropriate for your GC-MSD (6.6) system, and seal the vial. If
less than 2 g of test specimen is available, the test specimen mass shall be more than 0,5 g, and the
volume of the internal standard solution (5.4.3) shall be reduced proportionately. Extract the test
specimen for (30 ± 1) min in an ultrasonic bath (6.3) initially at laboratory ambient temperature.
After the extraction, let the solution cool down to nearly room temperature before opening the vial.
Filter the solution through a PTFE filter (6.4). Transfer an aliquot of the extract into a GC-MS vial (6.5)
and seal with a cap.
8.2 Determination by GC-MS or GC-MS/MS
8.2.1 Preparation of calibration solutions
Prepare at least 5 calibration solutions of a mixture of the required substances listed in Table 1,
including internal standard, from the working solutions 5.4.2, in dichloromethane (5.1), at suitable
concentrations for the analysis. Each solution shall contain the internal standard in a concentration that
matches the internal standard concentration in the extract (8.1).
8.2.2 Determination by GC-MS or GC-MS/MS
Determine the compounds listed in table 1 extracted in 8.1 by GC-MS or GC MS/MS (6.6) as required.
Examples of chromatographic conditions GC-MS and GC-MS/MS are given in Annex C.
It is known that particular substances used for textile finishing may degrade at temperatures above
150 °C in a GC inlet and release α-chlorinated toluenes (see Annex A). Take quality measures to avoid
false positive results (Annex A). Examples of suitable instrumental parameters to avoid the formation of
α-chlorinated toluenes are shown in Annex A and Annex B.
9 Expression of results
9.1 Calculation
The concentrations of chlorobenzenes, chlorotoluenes and α-chlorinated toluenes arise as a mass
fraction in µg/ml from the following Formula 1:
𝐹𝐹
𝑐𝑐
sample
ISTD
𝑐𝑐 = × (1)
sample
𝐹𝐹 𝑚𝑚
ISTD
where
F is the measured value of the substance (area value);
sample
F is the measured value of the internal standard (area value);
IS
c is the mass concentration of the substance in the extract (µg/ml);
sample
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c is the mass concentration of the internal standard in the extract (µg/ml);
IS
m is the slope of the calibration graph.
The concentrations of the analytes are calculated as mass fraction w in mg/kg using the following
Formula 2:
�𝑐𝑐 ×V�
sample
𝑤𝑤 = (2)
𝐸𝐸
where
w is the mass fraction (mg/kg);
V is the extraction volume (ml);
E is the initial mass (g).
9.2 Sum of chlorobenzenes and chlorotoluenes
In certain cases, the sum of different chlorobenzenes and chlorotoluenes (chlorinated organic carriers)
is requested as a final result. Only chlorobenzenes and chlorotoluenes that have been clearly identified
shall be included in the sum.
The results of the identified chlorobenzenes and chlorotoluenes (as obtained in 9.1) are added to give
the result of the sum. If the result for a single chlorobenzene or chlorotoluene is lower than 0,3 mg/kg
(9.3), this result is considered as zero and shall not be included in the sum.
9.3 Reliability of the method
This method is able to determine the concentrations of the substances listed in Table 1 with a limit of
quantification (LOQ) of 0,3 mg/kg or lower.
For the reliability of the method, see Annex C.
10 Test report
The test report shall include at least the following particulars:
a) reference to this document (including year of publication);
b) identification of the submitted sample;
c) description of the sampling of individual components;
d) date of test;
e) mass fraction for each chlorobenzene, chlorotoluene and α-chlorinated toluene, in mg/kg (9.1);
f) if requested, sum of certain chlorobenzenes and chlorotoluenes, in mg/kg (9.2);
g) any deviation from the given procedure;
h) any unusual features observed.
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Annex A
(informative)
False positives
A.1 False positives
"False positives" are analytical results that appear to be derived from target substances but actually
come from other sources than the target substance in the sample. For example, degradation products of
other chemicals in the product that have undergone chemical reactions during the analysis leads to
false positives.
Detection of traces of target substances, for example chlorobenzenes as residues from the production of
dyestuffs, are not considered as "false positives".
A temperature above 150 °C in the GC injector can cause false positive results.
A.2 Occurrences of chlorobenzenes and chlorotoluenes
Chlorobenzenes and chlorotoluenes have diverse applications in several industries. Within the apparel
and footwear supply chains, they are found in textile applications. Chlorobenzenes and chlorotoluenes
(with the exception of α-chlorotoluenes) can be used as carriers (named as chlorinated organic carriers
– COC) during the dyeing process of synthetic fibres, especially for polyester and polyester blends.
Chlorobenzenes and chlorotoluenes are also used as intermediates in the synthesis of other chemicals,
as well as solvents for dyestuffs and other chemical formulations with high melting temperatures.
Certain chlorobenzenes can be used to make deodorisers or degreasers for metal, leather and wool,
where 1,2-dichlorobenzene is used. There are known cases where 1,4-dichlorobenzene is used in air
fresheners and moth repellents. Therefore, chlorobenzenes and chlorotoluenes can also be present as
[2],[3], [4]
impurities .
A.3 Examples of false positives (not exhaustive)
A.3.1 α-Chlorotoluene (benzyl chloride) as a degradation product of quaternary
ammonium salts
Quaternary ammonium salts are often used in disinfectants, surfactants, fabric softeners and other
textile applications.
Quaternary ammonium salts, containing benzyl groups at the quaternary nitrogen can degrade in the
GC inlet due to the high inlet temperature and form α-chlorotoluene (benzyl chloride)[3]. For example,
this is known for benzalkoniumchloride: some safety data sheets report the decomposition of this
compound at ~150 °C (see Annex B).
[2]
A.3.2 1,2-Dichlorobenzene findings from synthesis residues
In dyestuffs, residues of 1,2-dichlorobenzene in the range of 0,5 mg/kg up to 5 mg/kg are common and
are not to be classified as false positives. These are (often) contamination/residues out of the synthesis
process of these dyestuffs. However, during extraction with dichloromethane some of the dyestuff is
extracted as well and can decompose in the GC inlet system and show significant results of
1,2-dichlorobenzene.
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A.3.3 Chlorobenzenes and chlorotoluenes released by dyestuff as degradation products
Some dyestuffs can decompose in a GC injector and release chlorinated benzenes and toluenes, see
Table A.1.
Table A.1 — Examples of dyestuff that can release chlorinated benzenes in GC injectors
Released substance Dyestuff
®
1,2-Dichlorobenzene Disperse Red 153 (CAS RN 78564-87-1)
®
Disperse Yellow 241 (CAS RN 83249-52-9)
®
C.I. Pigment Brown 41 (CAS RN 211502-16-8)
®
1,3-Dichlorobenzene Pigment Yellow 16 (CAS RN 5979-28-2)
®
Vat Blue 36 (CAS RN 6424-69-7)
®
1,4-Dichlorobenzene Pigment Red 2 (CAS RN 6041-94-7)
®
Pigment Red 9 (CAS RN 6410-38-4)
®
Pigment Red 166 (CAS RN 3905-19-9)
®
Pigment Red 214 (CAS RN 82643-43-4)
®
Pigment Brown 1 (CAS RN 6410-40-8)
®
Pigment Brown 25 (CAS RN 6992-11-6)
®
1,2,4-Trichlorobenzene Pigment Red 112 (CAS RN 6535-46-2)
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Annex B
(informative)
Test procedures if false positive results of benzyl chloride derived from
benzalkonium chloride are suspected
B.1 Confirmation of benzyl chloride derived from benzalkonium chloride by LC-
DAD
B.1.1 Principle
A sample is extracted with methanol for 1 hour, in an ultrasonic bath at room temperature. Afterwards,
the extract is analysed with Liquid Chromatography with Diode-Array Detection (LC-DAD).
B.1.2 Reagents
B.1.2.1 Water, grade 3 according to EN ISO 3696 or LC-MS grade.
B.1.2.2 Methanol, LC-MS grade, CAS number 67-56-1
B.1.2.3 Ammonium formate, CAS number 540-69-2
B.1.2.4 Benzyl chloride, CAS number 100-44-7
B.1.2.5 Benzalkonium Chloride, CAS number 63449-41-2 (for qualitative screening)
B.1.3 Apparatus
B.1.3.1 Liquid Chromatograph with Diode-Array Detection (LC-DAD).
B.1.4 Procedure
B.1.4.1 Sampling Procedure
Follow clause 7.1
B.1.4.2 Extraction
Weigh (2,0 ± 0,1) g of the specimen (B.1.4.1) in a glass vial (6.2), record the mass to the nearest 10 mg,
add 20 ml methanol (B.1.2.2) and seal the vial. If less than 2 g of test specimen is available, use at least
0,5 g of the test specimen, and reduce the volume of the internal standard solution (5.4.3)
proportionately. Extract the test specimen for (60 ± 1) min in an ultrasonic bath (6.3) initially at
laboratory ambient temperature.
Evaporate the solvent under nitrogen flow or other suitable solvent evaporator down to 1 ml final
volume. Adjust the evaporation syste
...
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