Characterization of waste - Halogen and sulfur content - Oxygen combustion in closed systems and determination methods

This standard specifies a combustion method for the determination of halogen and sulfur contents in materials by combustion in a closed system containing oxygen (calorimetric bomb), and the subsequent analysis of the combustion product using different analytical techniques.
This method is applicable to solid, pasty and liquid samples containing more than 0,025 g/kg of halogen and/or 0,025 g/kg of sulfur content. The limit of detection depends on the element, the matrix and the determination technique used.
Insoluble halides and sulphate present in the sample or produced during the combustion step are not completely determined by these methods.

Charakterisierung von Abfällen - Halogen- und Schwefelgehalt - Sauerstoffverbrennung in geschlossenen Systemen und Bestimmungsmethoden

Diese Norm legt ein Verbrennungsverfahren für die Bestimmung des Halogen  und Schwefelgehalts in Materialien durch Verbrennung in einem geschlossenen, Sauerstoff enthaltenden System (kalorimetrische Bombe) fest und die anschließende Analyse des Verbrennungsprodukts nach unterschiedlichen analytischen Verfahren.
Dieses Verfahren ist anwendbar bei festen, pastösen und flüssigen Proben mit mehr als 0,025 g/kg Halogengehalt und/oder 0,025 g/kg Schwefelgehalt. Die Nachweisgrenze hängt vom Element, von der Matrix und vom angewendeten Bestimmungsverfahren ab.
In der Probe vorhandene oder beim Verbrennungsschritt erzeugte unlösliche Halogenide und Sulfate werden mit diesen Verfahren nicht vollständig bestimmt.

Caractérisation des déchets - Teneur en halogènes et en soufre - Combustion sous oxygène en systèmes fermés et méthodes de dosage

La présente norme spécifie une méthode par combustion permettant de déterminer la teneur en halogènes et en soufre des matériaux par combustion dans un système fermé contenant de l’oxygène (bombe calorimétrique). Elle spécifie également l’analyse des produits de combustion à l’aide de différentes techniques analytiques.
Cette méthode est applicable aux échantillons solides, pâteux et liquides contenant une teneur en halogènes et/ou en soufre supérieure à 0,025 g/kg. La limite de détection dépend de l’élément, de la matrice et de la technique de dosage employée.
Les halogénures et le sulfate insolubles présents dans l’échantillon ou produits au cours de la phase de combustion ne sont pas complètement dosés par ces méthodes.

Karakterizacija odpadkov - Vsebnost halogena in žvepla - Sežig s kisikom v zaprtem sistemu in metode za določevanje

Ta standard določa metodo s sežiganjem za določanje vsebnosti halogena in žvepla s sežigom v zaprtem sistemu, ki vsebuje kisik (kalorimetrična bomba), in naknadno analizo sežganega izdelka z različnimi tehnikami analize. Ta metoda se uporablja za trdne vzorce, vzorce v pasti ali tekoče vzorce.

General Information

Status
Published
Public Enquiry End Date
07-Jul-2015
Publication Date
11-Apr-2017
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Feb-2017
Due Date
09-Apr-2017
Completion Date
12-Apr-2017

Relations

Standard
SIST EN 14582:2017
English language
35 pages
sale 10% off
Preview
sale 10% off
Preview
e-Library read for
1 day

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Charakterisierung von Abfällen - Halogen- und Schwefelgehalt - Sauerstoffverbrennung in geschlossenen Systemen und BestimmungsmethodenCaractérisation des déchets - Teneur en halogènes et en soufre - Combustion sous oxygène en systèmes fermés et méthodes de dosageCharacterization of waste - Halogen and sulfur content - Oxygen combustion in closed systems and determination methods13.030.40Naprave in oprema za odstranjevanje in obdelavo odpadkovInstallations and equipment for waste disposal and treatmentICS:Ta slovenski standard je istoveten z:EN 14582:2016SIST EN 14582:2017en,fr,de01-maj-2017SIST EN 14582:2017SLOVENSKI
STANDARDSIST EN 14582:20071DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14582
August
t r s x ICS
s uä r u rä v r Supersedes EN
s v w z tã t r r yEnglish Version
Characterization of waste æ Halogen and sulfur content æ Oxygen combustion in closed systems and determination methods Caractérisation des déchets æ Teneur en halogènes et en soufre æ Combustion sous oxygène en systèmes fermés et méthodes de dosage
Charakterisierung von Abfällen æ Halogenæ und Schwefelgehalt æ Sauerstoffverbrennung in geschlossenen Systemen und BestimmungsmethodenThis European Standard was approved by CEN on
s y June
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s v w z tã t r s x ESIST EN 14582:2017

Performance characteristics . 15 Annex B (informative)
Oxygen flask combustion by Schoeniger . 18 B.1 General . 18 B.2 Principle . 18 B.3 Interferences and hazards . 18 B.4 Reagents and control mixtures . 18 B.5 Equipment . 18 B.6 Safety precautions . 19 B.7 Procedure. 19 B.7.1 General . 19 B.7.2 Choice of the absorption solution . 19 SIST EN 14582:2017

Recovery yields obtained for control mixtures with different absorption solutions and analytical techniques . 24 Annex D (informative)
Examples of possible control substances . 27 Annex E (informative)
Additional results of inter-laboratory tests . 29 Annex F (informative)
Summary of general requirements and recommendations . 31 Annex G (informative)
Additional validation data . 32 G.1 General . 32 G.2 Samples . 32 G.3 Homogeneity and stability . 33
Control mixture 1 Control mixture 2 Amount of control substances 0,50 g of 4-fluoro-benzoic acid 2,0 g of 4-chloro-benzoic acid 2,0 g sulfanilic acid 55,0 g cellulose 0,25 g 4-bromo-benzoic acid 0,25g 4-iodo-benzoic acid 59,5 g cellulose Content of halogens and sulfur 1,130 g/kg fluorine 7,547 g/kg chlorine 6,170 g/kg sulfur 1,656 g/kg bromine 2,132 g/kg iodine 8 Sample conservation and pretreatment of test portion Biological active laboratory samples should be stored at 4 °C and the analyses of halogen and sulfur should be carried out within seven days after sampling. If this is not possible, the samples should be further preserved by e.g. freezing, if possible, to minimize biodegradation and loss of volatile halogenated and sulfur compounds. The test sample is prepared according to EN 15002. For solid materials, the particle size should be less than 200 µm. During preparation of the test sample, the use of halogenated polymers, e.g. PVC gloves, should be avoided. Drying the laboratory sample may be carried out for homogenization purposes if the sample, according to the accuracy of the method, contains only negligible amounts of halogen and sulfur compounds volatile at the temperature intended for the drying process. Dry matter is determined according to EN 14346 on a separate sub sample (the result will be used for calculation). Heterogeneous moist or paste like samples may be mixed with aluminium oxide (7.1.10) until granular material is obtained and then reduced to a granular powder, preferably with a particle size less than 200 µm. In this case, the ratio of aluminium oxide to sample should be incorporated into the calculation of the halogen and sulfur content and combustion enhancer should be added if necessary. SIST EN 14582:2017

X X 2 X X X X X X
X X 3 X X X X X
X
4 X
X
X
X
5 X X X
X
X X X
6 X X X X X X X X X
NOTE 2 The ascorbic acid and large amount of nitrate may interfere with early eluting halogens (fluoride, chloride and bromide) if detected by ion chromatography. The determination of recoveries of halogen and sulfur from control mixtures mentioned in Table 1 is presented in Annex C, in order to show the possible use and combination between absorption solutions and different analytical methods. 10.3 Preparation of the bomb The bomb is prepared according to the manufacturer’s instructions and the free ends of the firing wire (9.3) attached to the electric terminals of the ignition circuit (9.4). If using an absorption solution inside the bomb, add 10 ml of the chosen absorption solution (see 10.2), wetting the sides of the bomb (9.1). The sample cup should not be in contact with the absorption solution. Depending on the bomb design and/or the expected concentration range of the analytes of interest, it may be necessary to adapt the amount of the absorption solution or trap the combustion gases in an external absorption flask (see 9.5). 10.4 Combustion 0,05 g to 1 g of sample, depending on its calorific value, the amount of element present and on the determination method, is weighed (to the nearest 0,1 mg) into the sample cup (9.2). Samples that burn with difficulty (e.g. mineral samples or samples with high water content), may require the addition of a combustion enhancer (7.1.9). Liquid samples may be weighed in a capsule (7.1.11). To avoid swirling up of the sample when filling the bomb with oxygen, powdery samples may be covered with inert material (e.g. aluminium oxide (7.1.10)) or soaked with combustion enhancer (7.1.9), depending of their calorific value. Powdery samples with low density and that burn very readily may be pressed into a pellet before combustion, to avoid material to be flung out of the crucible. Depending on the type of the bomb, the total sample mass plus enhancer should not exceed 1 g to 1,5 g to avoid dangerous high pressure and possible rupturing the bomb. NOTE 1 The combined energy from sample and enhancer is not important to recover halogens and sulfur from the sample compounds. Hence it may be necessary to optimize the enhancer/sample amount ratio. Place the sample cup in position and arrange the firing wire (9.3) so that it will be just in contact with the sample but not touching the sample cup (9.2). SIST EN 14582:2017

F Cl Br I S Ion chromatography X X X X X ICP-OES
X X ICP-MS
X X X Potentiometry (Ion selective electrode) X
Potentiometry (AgNO3 titration)
X X X
Gravimetry with BaCl2
X 12 Control measurements A blank test shall be carried out for each series of determinations under the same conditions as the samples: absorption solution, combustion enhancer, capsule, reactants, oxygen purges, etc. If the value of this blank test is sign
...

Questions, Comments and Discussion

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

Loading comments...