BS EN 15290:2011 pdf download
BS EN 15290:2011 pdf download.Solid biofuels- Determination of major elements—Al,Ca, Fe,Mg,P, K,Si,Na and Ti.
For the digestion of the ash similar working steps, as for the digestion of the fuel, are evident:
C) Mix 50 mg of ground and homogenised ash, weighed to the nearest 0,1 mg, with 2.0 ml H202 (30 %), 3.0 ml HNO3 (65 %) and 2,0 ml HF (40 %) in a dosed decomposition vessel. A reaction time of minimum
5 mm shall be kept before dosing the vessel.
d) Digest the sample following one of the heating programmes described in 9.1.1 for digestion.
NOTE 3 If the maxnum pressure hm.t of the vessel Is exceeded durmg the digestion and by that an opening of the relief valve has occurred, the digestion should be discarded due 10 possible loss of Si (In form of gaseous SIF4).
a) After cooling to room temperature, the HF is neutralized by adding 20 ml l48O (4 %) and 10 ml deionised water.
NOTE 4 The water is neceswy to keep K in solution for bio-asfles with high KCI content.
I) Reheat the sample according to the healing programmes for neutralisation described in 9.1.1.
g) After cooling, transfer the digest to a volumetric flask. Rinse the digestion vessel carefully and transfer the rinse solution to the volumetric flask. Add desonised water to the digest to an appropnate volume, depending on the detection method to be used.
9.2 Detection methods
For the defection of the concentrations of Al, Ca. Fe, Mg. P. K, Si, Na. Ti in the digests, the following methods can be used:
— ICP-OES according 10 the pnnclples of EN ISO 11885:
— ICP-MS according to the princles of EN ISO 17294-2;
— MS according to the principles of EN ISO 7980, ISO 9964-1 and ISO 9964-2;
— FES according to the principles of ISO 9964-3.
9.3 CalIbration of the apparatus
When the analytical system is evaluated for the first time for this application, establish a calibration function for the measurement in accordance with the manufacturers instructions. Adjust the established calibration function during the analysis if necessary. Check the performance of the instrument using the accepted standard procedures like replicate analysis, use of SRM andlor CRM, control samples and control charts. The calibration and quality control scheme shall be organized and maintained in such a way that the required uncertainly of measurement can be obtained. The results of the validation study of BioNorm2 (Annex B) demonstrates what is achievable with commercial instruments that are used by experienced laboratories.
9.4 Analysis of digests
Analyse test portions of the digests in accordance with the manufacture?s instructions,
9.5 Blank test
Carry out a blank test, using the same procedure and methods as described in 9.1.1, 9.1.2, 9.2, 9.3 and 9.4 but omitting the test portion. This assesses both the contents of the elements in the reagents and any contamination from equipment and the laboratory atmosphere. This contribution shall not be quantitatively significant.
The round robin was carTled out by laboratories in Austria, Belgium. Denmark. Finland. Germany. Ireland. Italy. the Netherlands. Spain. Sweden and the United Kingdom. The variety of instruments and other analytical conditions were used in accordance with the quality paramefers specified in the method.
The tests wee carried out using two samples, wood chips and exhausted olive residues produced in the EUprqect BioNorm in 2008 in accordance with CEN?TS 14780 The sample ‘wood chips’ was made of German coniferous wood chs: the Chips were dried and mdled to 1 mm by means of cutting mill. The sample exhausted olive residues’ was obtained from olive ow industry wt Spa4n from a typ.cal outdoor storage facilrty. In the original sample stones and other natural impurities were present. These impurities and stones were removed manually and the sample was prepared from the residues in two steps using a coarse cutting mill equipped with a 10mm sieve and a laboratory cutting mill equipped with WC cutting tools and a 1 mm sieve.
The performance data acco’ding to ISO 5725-2 [1] are presented in Tables Bi to B.9
NOTE 1 S. Table B I for definition of the symbols used in Tables 8,1 to B 9
NOTE 2 A guideline can be found i EN 15296 on how to use these validation parameiers.