SIST EN 14582:2017
(Main)Characterization of waste - Halogen and sulfur content - Oxygen combustion in closed systems and determination methods
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.
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
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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
SIST EN 14582:2017
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
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9
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
EN 14582:2016 (E) 2 Contents Page European foreword . 4 Introduction . 5 1 Scope . 6 2 Normative references . 6 3 Terms and definitions . 6 4 Principle . 6 5 Interferences . 7 6 Hazards . 7 7 Reagents and control mixtures . 7 7.1 Reagents . 7 7.2 Control mixtures. 7 8 Sample conservation and pretreatment of test portion . 8 9 Equipment . 9 10 Procedure. 9 10.1 General . 9 10.2 Choice of the absorption solution . 10 10.3 Preparation of the bomb . 11 10.4 Combustion . 11 10.5 Collection of the halides and sulphate . 12 10.6 Cleaning procedure . 12 11 Recommended methods of determination . 13 12 Control measurements . 13 13 Evaluation . 13 14 Test report . 14 Annex A (informative)
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
EN 14582:2016 (E) 3 B.7.3 Sample preparation . 20 B.7.4 Combustion . 20 B.8 Determination methods; control measurements; data evaluation and test report . 20 B.9 Performance characteristics . 21 Annex C (informative)
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
SIST EN 14582:2017
EN 14582:2016 (E) 4 European foreword This document (EN 14582:2016) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2017, and conflicting national standards shall be withdrawn at the latest by February 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 14582:2007. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 14582:2017
EN 14582:2016 (E) 5 Introduction Sulfur and halogens (fluorine, chlorine, bromine and iodine) may be found in materials in various forms. During the combustion of these materials, corrosive and harmful compounds may be released. The determination of sulfur and halogens by oxygen combustion may be used to assess the suitability of waste for incineration. The determination of the resultant halides and sulphate can be achieved by many different techniques, e.g. using atomic emission spectrometry, titrimetry or ion chromatography. Validation data of these different techniques are given in Annex A (informative). Another method, oxygen flask combustion by Schoeniger, did not pass the method validation due to lack of participants. This method is described in Annex B (informative). Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material irrespective of the parameter to be determined. Waste and sludge samples may contain hazardous (e.g. toxic, reactive, flammable, infectious) substances, which can be liable to biological and/or chemical reaction. Consequently these samples should be handled with special care. Gases which may be produced by microbiological or chemical activity are potentially flammable and will pressurize sealed containers. 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. SIST EN 14582:2017
EN 14582:2016 (E) 6 1 Scope 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. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 14346, Characterization of waste - Calculation of dry matter by determination of dry residue or water content EN 15002, Characterization of waste - Preparation of test portions from the laboratory sample EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. NOTE Be aware that the above definitions are valid for this empirical EN only and do not comply with scientific definitions of sulfur and halogen content. 3.1 sulfur content sum of sulfur contained as organic and inorganic compounds that can be converted to sulphate by combustion and then absorbed or dissolved in an aqueous solution 3.2 halogen content sum of halogens contained as organic and inorganic compounds that can be converted to halides (fluoride, chloride, bromide, iodide) by combustion and then absorbed or dissolved in an aqueous solution 4 Principle The sample is oxidized by combustion in a closed system (a bomb containing oxygen under pressure). Halogenated and sulfur containing compounds are converted to fluoride, chloride, bromide, iodide and sulphate, which are absorbed and/or dissolved in an absorption solution. Several methods may be used for the determination of halides and sulphate concentrations in the absorption solution. The method may be used for samples that burn with difficulty, which involves the use of a combustion enhancer. SIST EN 14582:2017
EN 14582:2016 (E) 7 5 Interferences There are no interferences in the combustion step described in this standard but interferences may occur during the subsequent determination of sulphate and halides (see corresponding standards). Insoluble halides and sulphate present in the sample or produced during the combustion step are not completely determined by these methods. The choice of absorption solutions may introduce interferences depending on the analytical technique used. 6 Hazards Hydrogen peroxide is very caustic; potassium and sodium hydroxide are corrosive and hydrazine hydrate is harmful, toxic and carcinogenic. Thus the operator shall wear goggles and gloves and shall work under a fume hood when handling this reagent. As this method uses a gas (oxygen) at a high temperature and a high pressure, precautions shall be taken by the operator. 7 Reagents and control mixtures 7.1 Reagents 7.1.1 General All reagents shall be at least of analytical grade and suitable for their specific purposes. Particularly, they shall be free of sulfur and halogens. The reagents correspond to the chemical compounds used for the preparation of the absorption solutions; they are not all necessary depending on the choice of the solutions made by the laboratory for the determination of halides and sulfur (see Annex C). 7.1.2 Water of grade 1 as specified in EN ISO 3696. 7.1.3 Sodium hydroxide (NaOH) or potassium hydroxide (KOH) pellets. 7.1.4 Sodium bicarbonate NaHCO3 and sodium carbonate Na2CO3. 7.1.5 Hydrogen peroxide (about 30 %) (H2O2). 7.1.6 Hydrazine hydrate (H2N-NH2·H2O), reagent grade about 50 % – 60 %. 7.1.7 Ascorbic acid (C6H8O6). 7.1.8 Oxygen, free of combustible material, available at a pressure of 3 MPa to 4 MPa (30 atm to 40 atm) (e.g. medical grade). 7.1.9 Combustion enhancer (e.g. paraffin). 7.1.10 Aluminium oxide, Al2O3, neutral, particle size < 200 µm, pre-heated to 600 °C. 7.1.11 Gelatine or aceto-butyrate capsules. 7.2 Control mixtures Select a certified reference material (CRM) or create an appropriate control mixture by choosing the control substances in combination so all elements that shall be determined in the samples are SIST EN 14582:2017
EN 14582:2016 (E) 8 represented. The amount of halogen and sulfur contents shall be in the same range of the element contents of the samples and approximately in the middle of the working range of the determination techniques. If necessary, dilute with cellulose or aluminium oxide to get a suitable element content. The mixture of the control substances and the cellulose or aluminium oxide needs to be homogenized, e.g. using a pestle with mortar or ball mill. Table D.1 lists examples of control substances that give complete (90 % to 110 %) recoveries of halogen and sulfur. NOTE Combined combustion of iodine and sulfur may interact to improve the reduction of iodine to iodide and the oxidation of sulfur to sulphate. If the actual samples only contain one of the elements, a combined control mixture may give false assurance of the method capacity. Examples of composition for a control mixture to determine fluorine, chlorine and sulfur (control mixture 1) and another control mixture for bromine and iodine (control mixture 2) are detailed in Table 1. Table 1 — Examples of control mixture to test the recoveries of halogens and sulfur with a defined analytical method
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
EN 14582:2016 (E) 9 9 Equipment 9.1 Calorimetric bomb, with a capacity of not less than 200 ml and equipped with a purging system This bomb shall not leak during testing and shall permit a quantitative recovery of the liquid. Its inner surface may be made of stainless steel or any other material that will not be affected by combustion gases. Materials used for the bomb assembly, such as the head gasket and wire insulation, shall be heat and chemical action resistant and shall not undergo any reaction that will affect the results. Bombs with pitted surfaces should never be used because of their tendency to retain halides and sulphate. After repeated use of the bomb, a film may build up on the inner surface. This dullness should be removed by periodically polishing the bomb according to the manufacturer’s instructions. The internal surface of some calorimetric bombs may have a ceramic coating or platinum buckets, which have better resistance to corrosion. 9.2 Sample cup, platinum or stainless steel or quartz. 9.3 Firing wire, platinum or stainless steel or nickel/chromium alloy or an equivalent. 9.4 Ignition circuit, capable of supplying a sufficient current to ignite the sample without melting the wire. 9.5 Absorption flask (e.g. a 200 ml test tube equipped with a glass frit dip-tube for bubbling the combustion gases). 9.6 Usual laboratory equipment, as homogenization devices (e.g. mixers, stirrers, grinders, mills), analytical balance (accurate at least to 0,1 mg), etc. 9.7 Safety precautions The bomb shall not contain any organic residue (vapours of organic solvents, grease, etc.). Respect shall be given to the manufacturer's instructions, especially to the oxygen pressure inside the bomb and the maximum allowable calorific value of the test portion. NOTE Combustion of 1 g of hydrocarbons such as lubricating oil produces about 40 kJ (the calorific values of benzoic acid and isooctane are about 26 MJ/kg and 48 MJ/kg). 10 Procedure 10.1 General Before each series of determinations, a blank and quality check shall be carried out on a control mixture (7.2), according to Clause 12. Alternately running samples high and low in halogen or sulfur content should be avoided whenever possible as it is difficult to rinse the last traces of ions from the internal surfaces of the apparatus and a tendency for residual elements to carry over from sample to sample has been observed. When a sample high in halogen or sulfur content has preceded a sample low in concentration, the test on the second sample should be repeated and one or both of the low values thus obtained should be considered suspect if they do not fall within the limits of repeatability of this method. It is good practice to insert a blank between each sample, unless the series of samples being analysed has similar expected concentrations. SIST EN 14582:2017
EN 14582:2016 (E) 10 When the composition or homogeneity of the sample is unknown, it is better to carry out the analysis in duplicate or triplicate and report the mean result from all determinations with the associated standard deviation. In case of significant carry over it is recommended to collect the exhaustion gases of the sample and the following blank sample in one absorption liquid. 10.2 Choice of the absorption solution The combustion gases can be collected inside and/or outside the bomb in an absorption solution. Water is generally used when low concentrations of halogens and sulfur are expected (usually, less than 10 g/kg). Alkaline solution should be used for high contents of halogens and sulfur, to ensure neutralization of the acid compounds produced. The composition of absorption solutions depend on the determination technique and on the expected content of halogens and sulfur. Applicable examples are: — Solution 1: Water (7.1.2); — Solution 2: 0,3 mol/l potassium or sodium hydroxide solution: dissolve 16,8 g of KOH or 12,0 g of NaOH pellets (7.1.3) in water (7.1.2) and dilute to 1 l; — Solution 3: Carbonate/bicarbonate solution: dissolve 2,52 g sodium bicarbonate NaHCO3 and 2,54 g sodium carbonate Na2CO3 (7.1.4) in water (7.1.2) and dilute to 1 l; — Solution 4: 0,25 mol/l sodium hydroxide solution (dissolve 10,0 g NaOH pellets (7.1.3) in water (7.1.2) and dilute to 1 l) + 50 µl of hydrogen peroxide solution at 3 % (dilute 5 ml H2O2 (7.1.5) into 50 ml); — Solution 5: 0,25 mol/l sodium hydroxide solution (dissolve 10,0 g NaOH pellets (7.1.3) in water (7.1.2) and dilute to 1 l) + 0,5 ml of hydrazine hydrate (7.1.6); — Solution 6: Ascorbic acid-solution at 1 % or at 5 % prepared with pure reagent (7.1.7) in water (7.1.2). NOTE 1 More details regarding these solutions and there performances in terms of halogens and sulfur recovery are available in Annex C. When ion chromatography is used for the determination of halides and sulphate, the absorption solution may have the composition of the mobile phase, e.g. carbonate/bicarbonate solution. It is recommended to add 0,5 ml of hydrogen peroxide solution (7.1.5) to the absorption solution before combustion to improve the oxidation of sulfur. However, hydrogen peroxide may oxidize iodide leading to an underestimation. When sulfur and iodine are to be determined in the same sample, it is recommended to carry out two different combustion operations. For iodine and bromine use 10 ml of 1 % ascorbic acid (solution 6) as an absorption solution to improve the reduction to iodide or bromide before opening of the bomb. The most suitable combinations of absorption solutions with determination techniques for the expected halogens or sulfur are presented in Table 2. SIST EN 14582:2017
EN 14582:2016 (E) 11 Table 2 — Suitable combinations of absorption solution and determination technique for halogens and sulfur Absorption solution Analytical techniques for halogens and sulfur content determination Fluorine Chlorine Bromine Iodine Sulfur IC Ion selective electrode IC Potentiometry IC Potentiometry IC Potentiometry IC Gravimetry 1 X X X X X X
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
EN 14582:2016 (E) 12 NOTE 2 Some operators use nylon thread or cotton wick and loop it around the wire so that its ends immerse directly in the liquid sample or are in contact with the solid sample. Assemble the bomb and tighten the cover securely. Admit oxygen (7.1.8) carefully (to avoid blowing the sample from the cup) to a pressure below the safety pressure specified by the manufacturer. In case nitrates produced during the oxidation of the nitrogen of the air contained in the bomb interfere during the analytical determination, this ambient air should be eliminated by vacuum depletion or by flushing the bomb with oxygen. Connect the terminals to the open electrical circuit. Close the circuit to ignite the sample. After the combustion is complete, let the bomb cool to ambient temperature, e.g. in a water bath. 10.5 Collection of the halides and sulphate When relatively high levels of halogens and sulfur (e.g. over 20 g/kg) are expected, and/or when there is no absorption solution inside the bomb, connect the exit of the bomb to an absorption flask (9.
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