BS EN 14582 pdf free download
BS EN 14582-2016 pdf free download.Characterization of waste — Halogen and sulfur content — Oxygen combustion in closed systems and determination methods.
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 NaHCO 3 and sodium carbonate Na 2 CO 3 .
7.1.5 Hydrogen peroxide (about 30 %) (H 2 O 2 ).
7.1.6 Hydrazine hydrate (H 2 N-NH 2 ·H 2 O), reagent grade about 50 % – 60 %.
7.1.7 Ascorbic acid (C 6 H 8 O 6 ).
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, Al 2 O 3 , 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 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.
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.BS EN 14582 pdf download.
