EN 15192:2006

Characterisation of waste and soil - Determination of Chromium(VI) in solid material by alkaline digestion and ion chromatography with spectrophotometric detection

This standard describes the determination of Cr(VI) in solid waste material and soil by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,1 mg/kg.

Charakterisierung von Abfällen und Boden - Bestimmung von sechswertigem Chrom in Feststoffen durch alkalischen Aufschluss und lonenchromatographie mit photometrischer Detektion

Diese Norm beschreibt die Bestimmung von Cr(VI) in festen Abfallmaterialien und Boden durch basischen Aufschluss und Ionenchromatographie mit photometrischer Detektion. Das Verfahren kann zum Bestimmen von Cr(VI)-Massenanteilen in Feststoffen ab 0,1 mg/kg angewendet werden.

Caractérisation des déchets et des sols - Dosage du chrome (VI) dans les matériaux solides par digestion alcaline et chromatographie ionique avec détection spectrophotométrique

La présente norme décrit le dosage du Cr(VI) dans les déchets solides et les sols par digestion alcaline et chromatographie ionique avec détection spectrophotométrique. Cette méthode peut être utilisée pour déterminer les fractions massiques de Cr(VI) dans les solides supérieures à 0,1 mg/kg.
NOTE   Il n’est pas possible d’indiquer dans un rapport une teneur valable en Cr(VI) lorsque la matrice de déchets est réductrice ou oxydante.

Karakterizacija odpadkov in zemljine - Določevanje šestvalentnega kroma Cr (VI) v trdnem mediju z alkalnim razklopom in ionsko kromatografijo s spektrofotometrično detekcijo

General Information

• Status: Withdrawn
• Publication Date: 14-Nov-2006
• Withdrawal Date: 06-Jul-2021
• ICS: 13.030.10 - Solid wastes
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: CEN/TC 444 - Environmental characterization
• Drafting Committee: CEN/TC 444/WG 3 - Inorganic analysis
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 07-Jul-2021
• Ref Project: SIST EN 15192:2007 - Characterisation of waste and soil - Determination of Chromium(VI) in solid material by alkaline digestion and ion chromatography with spectrophotometric detection

Relations

• Replaced By: EN ISO 15192:2021 - Soil and waste - Determination of Chromium(VI) in solid material by alkaline digestion and ion chromatography with spectrophotometric detection (ISO 15192:2021)
• Effective Date: 14-Jul-2021

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Characterisation of waste and soil - Determination of Chromium(VI) in solid material by alkaline digestion and ion chromatography with spectrophotometric detectionCaractérisation des déchets et des sols - Dosage du chrome (VI) dans les matériaux solides par digestion alcaline et chromatographie ionique avec détection spectrophotométriqueCharakterisierung von Abfällen und Boden - Bestimmung von sechswertigem Chrom in Feststoffen durch alkalischen Aufschluss und lonenchromatographie mit photometrischer DetektionTa slovenski standard je istoveten z:EN 15192:2006SIST EN 15192:2007en13.080.10Chemical characteristics of soils13.030.10Trdni odpadkiSolid wastesICS:SLOVENSKI
STANDARDSIST EN 15192:200701-april-2007

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15192November 2006ICS 13.030.10; 13.080.10 English VersionCharacterisation of waste and soil - Determination ofChromium(VI) in solid material by alkaline digestion and ionchromatography with spectrophotometric detectionCaractérisation des déchets et des sols - Dosage duchrome VI dans les matériaux solides par digestion alcalineet chromatographie ionique avec détectionspectrophotométriqueCharakterisierung von Abfällen und Boden - Bestimmungvon sechswertigem Chrom in Feststoffen durch alkalischenAufschluss und lonenchromatographie mit photometrischerDetektionThis European Standard was approved by CEN on 6 October 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15192:2006: E

Alternative methods for direct determination of Cr(VI) in the alkaline digestion solution.16 Annex B Ion chromatographic system.17 Annex C (informative)
Requirements for test portion preparation.18 Annex D (informative)
Background on methods for the determination of Cr(VI) in solid samples.19 D.1 Summary of literature methods for Cr (VI) determinations in solids [6].19 D.2 Theoretical kinetic background for Cr(III)-Cr(VI) inter-conversions [6].19 D.3 Special needs for Cr(VI) determination in soil extracts [7].20 D.4 Determination of Cr(VI) in glass.21 D.5 Determination of Cr(VI) in air particulate matter.21 Annex E (informative)
Validation.22 Bibliography.26

3 Terms and Definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 alkaline digestion process of obtaining a solution containing the analyte of interest from a sample under alkaline conditions. Alkaline digestion may or may not involve complete dissolution of the sample 3.2 speciation analysis activities of measuring the quantity of one or more individual chemical species in a sample, e.g. Cr(VI) in a particular sample or matrix 4 Safety remarks Anyone dealing with waste and soil analysis has to be aware of the typical risks of the material irrespective of the parameters determined. Waste and soil samples may contain hazardous (e.g. toxic, reactive, flammable, infectious) substances, which can be liable to biological and/or chemical reaction. Consequently, it is recommended that these samples should be handled with special care. The gases which may be produced by microbiological or chemical activity are potentially flammable and can pressurise sealed bottles. Bursting bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. Avoid any contact with the skin, ingestion or inhalation of Cr(VI) compounds. Cr(VI) compounds are genotoxic and potentially carcinogenic to humans.

3) method must not cause oxidation of native Cr(III) contained in the sample to Cr(VI).
The alkaline digestion described in this standard meets these criteria for a wide spectrum of solid matrices. Under the alkaline conditions of the digestion, neglectable reduction of Cr(VI) or oxidation of native Cr(III) is expected. The additon of Mg2+ in a phosphate buffer to the alkaline solution prevents air oxidation of trivalent chromium [1], [6], [32]. NOTE Background on methods for the determination of Cr(VI) in solid samples is given in Annex D and [4], [5], [6]. 5.2 Determination Quantification of Cr(VI) in the alkaline digestion solution should be performed using a suitable technique with appropriate accuracy. For this purpose ion chromatography is used to separate Cr(VI) from interferences. Following this ion chromatographic separation, Cr(VI) is measured spectrophotometrically either at 365 nm (direct UV detection) or after post-column derivatisation with 1,5-diphenylcarbazide in acid solution at 540 nm. Post-column derivatisation involves reaction of 1,5-diphenylcarbazide with Cr(VI) to produce trivalent chromium and diphenylcarbazone. These then combine to form a trivalent chromium-diphenylcarbazone complex containing the characteristic magenta chromagen (λmax= 540 nm). NOTE 1 The choice of detection method is based upon the required sensitivity. Direct UV detection is less sensitive than detection after post-column derivatisation with 1,5-diphenylcarbazide. NOTE 2 Hyphenated methods with ion chromatographic separation and detection techniques, such as inductively coupled plasma mass spectrometry (ICP-MS) or inductively coupled plasma atomic emission spectroscopy (ICP-AES), may be used once validation of the chosen analytical method has been performed. 5.3 Interferences and sources of error  Use of ion chromatography is necessary for the separation of Cr(VI) from possible interferences in the alkaline digestion solution from solid material [7] (see also Annex D.3).  For waste materials or soils, where the Cr(III)/Cr(VI) ratio is expected to be high, Cr(VI) results may be biased due to method induced oxidation. This can be particularly expected in soils high in Mn content and amended with soluble Cr(III) salts or freshly precipitated Cr(OH)3 [4] (see also Annex D.2).
 Cr(VI) can be reduced to Cr(III) during digestion from the sample due to reaction with reducing agents such as e.g. divalent iron. This problem is minimised in the described procedure using alkaline digestion solution [6] (see also Annex D.2).  Cr(III) can be oxidised to Cr(VI) in hot alkaline solutions. This problem is minimised in the described procedure by adding magnesium to the alkaline digestion solution [3], [4], [6], [32] (see also Annex D.2).
 Overloading the analytical column capacity with high concentrations of anionic species (e.g. chloride) may cause underestimation of Cr(VI) [43].

suitable for using 0,45-µm membrane filters. 6.3 Membrane filters, 0,45 µm pore size, chemically inert. 6.4 Ion chromatographic system,
all components which come into contact with the sample or eluent stream shall be comprised of inert materials, e.g. polyetherether ketone (PEEK), as shall all connecting tubing (see Annex B). 6.5 Ion chromatographic column, suitable for chromate separation with a sufficient ion exchange capacity. 6.6 Detection system  UV-VIS spectrophotometer at 365 nm; or  VIS spectrophotometer at 540 nm after post column derivatisation.
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