FprCEN/TS 17847
(Main)Characterization of waste - Determination of selected low boiling point alcohols using gas chromatography with flame ionization detection after static head-space extraction (HS-GC-FID)
Characterization of waste - Determination of selected low boiling point alcohols using gas chromatography with flame ionization detection after static head-space extraction (HS-GC-FID)
This document specifies a method for quantitative determination of the concentration of selected alcohols with low boiling point in liquid waste and pasty waste by gas chromatography with flame ionization detection after static headspace extraction.
Under the conditions specified in this document, a limit of application of 20 mg/kg, expressed on dry matter for pasty waste and expressed on raw waste for liquid waste, can be achieved.
Charakterisierung von Abfällen - Bestimmung von ausgewählten, niedrigsiedenden Alkoholen mittels Gaschromatographie mit Flammenionisationsdetektor nach statischer Headspace Extraktion (HS-GC-FID)
Dieses Dokument legt ein Verfahren für die quantitative Bestimmung der Konzentration von ausgewählten, niedrigsiedenden Alkoholen in flüssigem Abfall und pastösem Abfall mittels Gaschromatographie mit Flammenionisationsdetektor nach statischer Dampfraumanalyse fest.
Unter den in diesem Dokument festgelegten Bedingungen kann eine untere Grenze des Anwendungsbereichs von 20 mg/kg, angegeben bezogen auf die Trockenmasse für pastösen Abfall bzw. bezogen auf Rohabfall für flüssigen Abfall, erreicht werden.
Caractérisation des déchets - Détermination d'une sélection d'alcools à bas point d’ébullition par chromatographie en phase gazeuse avec détection par ionisation de flamme après extraction statique par espace de tête (HS-GC-FID)
Le présent document spécifie une méthode de détermination quantitative de la concentration d'une sélection d’alcools à bas point d’ébullition dans des déchets liquides et pâteux, par chromatographie en phase gazeuse avec détection par ionisation de flamme après extraction statique par espace de tête.
Dans les conditions spécifiées dans le présent document, une limite d’application de 20 mg/kg, exprimée par rapport à la matière sèche pour les déchets pâteux et par rapport aux déchets bruts pour les déchets liquides, peut être atteinte.
[Not translated]
General Information
Standards Content (sample)
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17847:2022
01-junij-2022
[Not translated]
Characterization of waste - Determination of selected low boiling point alcohols using
gas chromatography with flame ionization detection after static head-space extraction
(HS-GC-FID)Charakterisierung von Abfällen - Bestimmung von ausgewählten, niedrigsiedenden
Alkoholen mittels Gaschromatographie mit Flammenionisationsdetektor nach statischer
Headspace Extraktion (HS-GC-FID)Caractérisation des déchets - Détermination d'une sélection d'alcools à bas point
d’ébullition par chromatographie en phase gazeuse avec détection par ionisation de
flamme après extraction statique par espace de tête (HS-GC-FID)Ta slovenski standard je istoveten z: FprCEN/TS 17847
ICS:
13.030.01 Odpadki na splošno Wastes in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
kSIST-TS FprCEN/TS 17847:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TS FprCEN/TS 17847:2022
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17847
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
April 2022
ICS 13.030.01
English Version
Characterization of waste - Determination of selected low
boiling point alcohols using gas chromatography with
flame ionization detection after static head-space
extraction (HS-GC-FID)
Caractérisation des déchets - Détermination d'une Charakterisierung von Abfällen - Bestimmung von
sélection d'alcools à bas point d'ébullition par ausgewählten, niedrigsiedenden Alkoholen mittels
chromatographie en phase gazeuse avec détection par Gaschromatographie mit Flammenionisationsdetektor
ionisation de flamme après extraction statique par nach statischer Headspace Extraktion (HS-GC-FID)
espace de tête (HS-GC-FID)This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee
CEN/TC 444.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 Technical Specification. It is distributed for review and comments. It is subject to change
without notice and shall not be referred to as a Technical Specification.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. FprCEN/TS 17847:2022 E
worldwide for CEN national Members.---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17847:2022
FprCEN/TS 17847:2022 (E)
Contents Page
European foreword ............................................................................................................................................. 3
Introduction .......................................................................................................................................................... 4
1 Scope .......................................................................................................................................................... 5
2 Normative references .......................................................................................................................... 5
3 Terms and definitions ......................................................................................................................... 5
4 Principle ................................................................................................................................................... 5
5 Interferences .......................................................................................................................................... 6
5.1 Interferences with sampling and extraction ............................................................................... 6
5.2 Interferences with GC .......................................................................................................................... 6
6 Apparatus and reagents ...................................................................................................................... 6
6.1 Apparatus ................................................................................................................................................. 6
6.2 Reagents ................................................................................................................................................... 7
6.3 Sampling, storage and pretreatment ............................................................................................. 7
6.3.1 Sampling ................................................................................................................................................... 7
6.3.2 Storage ...................................................................................................................................................... 8
6.3.3 Preatreatment ........................................................................................................................................ 8
7 Procedure................................................................................................................................................. 8
7.1 Determination of dry matter via water content for pasty waste ......................................... 8
7.2 Calibration ............................................................................................................................................... 8
7.3 Mass of sample ....................................................................................................................................... 8
7.4 Analysis ..................................................................................................................................................... 9
7.4.1 Identification of selected alcohols by retention times on the chromatogram obtained
by GC-FID .................................................................................................................................................. 9
7.4.2 Confirmation criteria for the identification of selected alcohol .......................................... 9
7.4.3 Procedure................................................................................................................................................. 9
8 Calculation .............................................................................................................................................10
8.1 Calibration function ...........................................................................................................................10
8.2 Calculation of selected alcohol concentration in the sample ..............................................10
9 Expression of results ..........................................................................................................................11
10 Test report .............................................................................................................................................11
Annex A (informative) Examples of gas chromatographic conditions ............................................12
A.1 Examples of head-space sampler conditions ............................................................................12
A.2 Examples of suitable chromatographic columns .....................................................................12
A.3 Examples of GC settings ....................................................................................................................12
Bibliography ........................................................................................................................................................14
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European foreword
This document (FprCEN/TS 17847:2022) has been prepared by Technical Committee CEN/TC 444
“Environmental characterization of solid matrices”, the secretariat of which is held by NEN.
This document is currently submitted to the Vote on TS.---------------------- Page: 5 ----------------------
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FprCEN/TS 17847:2022 (E)
Introduction
Directive 96/82/EC, as amended, requires transit/sorting/regrouping or waste treatment facilities to
assess the hazardous nature of their waste, in particular, from the point of view of the following categories
of hazards:— very toxic or toxic to humans if swallowed, for example contact with the skin or by inhalation,
— very toxic or toxic to the aquatic environment.Based on knowledge of the composition of elements and substances of a waste, its hazard potential can
then be determined from the classification rules established for mixtures in waste legislation.
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FprCEN/TS 17847:2022 (E)
1 Scope
This document specifies a method for quantitative determination of the concentration of selected
alcohols with low boiling point in liquid waste and pasty waste by gas chromatography with flame
ionization detection after static headspace extraction.Under the conditions specified in this document, a limit of application of 20 mg/kg, expressed on dry
matter for pasty waste and expressed on raw waste for liquid waste, can be achieved.
2 Normative referencesThe 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 15934:2012, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after
determination of dry residue or water contentEN 16179:2012, Sludge, treated biowaste and soil — Guidance for sample pretreatment
EN 15002:2015, Characterization of waste — Preparation of test portions from the laboratory sample
3 Terms and definitionsNo 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 Principle
This method describes a gas chromatography (GC) method using a flame ionization detection (FID) after
an equilibrium-based static headspace preparation.A specified quantity of extractant solution is added to a test portion of raw sample before any
pretreatment in a hermetically sealed vial with sufficient space for desorption of analytes into the gas
phase. The vial is heated in a thermostat at 80 °C until desorption equilibrium is reached.
A defined portion of the gas phase is injected into the gas chromatograph using two analytical columns
with different stationary phases, and the analytes are detected by a flame ionization detector. The amount
of each analyte is calculated using a calibration function established with external standards. An internal
standard is added in the extractant solution, for the retention time verification.
The list of analytes is given in Table 1.---------------------- Page: 7 ----------------------
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FprCEN/TS 17847:2022 (E)
Table 1 — Analytes, with CAS RN and boiling point
Substance CAS RN Boiling point
(°C)
Methanol (Me-OH) 67–56–1 64,5
Ethanol (Et-OH) 64–17–5 78,5
Iso-Propanol (i-Pr-OH) 67–63–0 82,4
Tert-Butanol (t-Pr-OH) 75–65–0 83
n-Propanol (Pr-OH) 71–23–8 97,1
Iso-Butanol (i-Bu-OH) 78–83–1 108
n-Butanol (Bu-OH) 71–36–3 118
NOTE The method can be applied to other low boiling point analytes not specified in the scope provided
suitability is proven by proper in-house validation.5 Interferences
5.1 Interferences with sampling and extraction
Use sampling glass containers. During storage of the samples, losses of alcohols may occur due to
volatilization. Sampling directly in head-space vials minimizes handling of samples and analytes loss.
Samples can be contaminated by diffusion of volatile organic compounds through the septum seal of the
sample vial during shipment and storage. A transport blank, prepared from extractant solution and
sample container and carried through sampling and handling protocols, serves as a check on such
contamination.5.2 Interferences with GC
Substances that co-elute with analytes may interfere with the determination. These interferences may
lead to insufficient signal resolution and may, depending on their magnitude, affect accuracy and
precision of the analytical results. Two analytical columns with different stationay phases (6.1.5) are used
to confirm the identification of the selected alcohols.6 Apparatus and reagents
6.1 Apparatus
Usual laboratory glassware.
All glassware and material that come into contact with the sample or extract shall be thoroughly cleaned.
6.1.1 Analytical balance, with a weighing accuracy of 0,1 mg.6.1.2 Gas chromatograph, with head-space autosampler.
6.1.3 Flame ionization detector.
6.1.4 Glass head-space vials, 10 to 20 ml, according to the type of headspace equipment, with
hermetic crimp or screw cap and septum (silicone /polytetrafluoroethylene (PTFE)).
6.1.5 Chromatographic columns, e.g. DB-Wax 60 m × 0,25 mm × 0,25 µm, CP-SIL8-CB (see Annex A).
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6.1.6 Automatic syringe or bottle
...
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