This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead. The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic matter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method was successfully tested for: – calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material (phosphate), 1 mineral premixture and 2 complementary feeds (2 mineral feeds), – lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed) The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg\/kg or lower. This method also applies for the determination in products with high element content (>5 %). For this purpose the accuracy of the method has to be checked individually. NOTE 1 EN 15621 uses the pressure digestion mode, therefore lower results may be obtained with the described method in this standard.<\/p>\n
| PDF Pages<\/th>\n | PDF Title<\/th>\n<\/tr>\n | ||||||
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| 44<\/td>\n | National foreword <\/td>\n<\/tr>\n | ||||||
| 49<\/td>\n | 1 Scope 2 Normative references 3 Terms and definitions <\/td>\n<\/tr>\n | ||||||
| 50<\/td>\n | 4 Principle 5 Reagents <\/td>\n<\/tr>\n | ||||||
| 52<\/td>\n | 6 Apparatus 7 Sampling <\/td>\n<\/tr>\n | ||||||
| 53<\/td>\n | 8 Sample preparation 8.1 General 8.2 Animal feeding stuffs, which can be ground as such 8.3 Liquid animal feeding stuffs 8.3.1 General 8.3.2 Pre-drying 8.3.3 Freeze-drying 8.4 Mineral matrices 9 Procedure 9.1 Digestion 9.1.1 Selection of the procedure 9.1.1.1 Determination of Ca, Na, P, Mg, K, Fe, Zn, Cu, Mn, Co, Mo, Pb <\/td>\n<\/tr>\n | ||||||
| 54<\/td>\n | 9.1.1.2 Determination of extractable Pb 9.1.2 Extraction with HCl 9.1.3 Dry ashing and extraction with HCl <\/td>\n<\/tr>\n | ||||||
| 55<\/td>\n | 9.1.4 Wet digestion with HNO3 9.2 Calibration 9.2.1 General 9.2.2 External calibration 9.2.3 Standard addition technique 9.2.4 Example of calibration with one addition after dry ashing \u2013HCl 9.2.4.1 Preparation of the test solution 9.2.4.2 Preparation of the blank solution <\/td>\n<\/tr>\n | ||||||
| 56<\/td>\n | 9.2.4.3 Preparation of the addition 9.2.5 Example of calibration with one addition after wet digestion \u2013 1\u00a0% HCl 9.2.5.1 Preparation of the test solution 9.2.5.2 Preparation of the blank solution 9.2.5.3 Preparation of the addition 9.2.6 Example of calibration with one addition after wet digestion with HNO3 9.2.6.1 Preparation of the test solution 9.2.6.2 Preparation of the blank solution 9.2.6.3 Preparation of the addition 9.3 Determination 9.3.1 General 9.3.2 Determination by inductively coupled plasma \u2013 atomic emission spectrometry 9.3.2.1 General <\/td>\n<\/tr>\n | ||||||
| 57<\/td>\n | 9.3.2.2 External calibration method 9.3.2.3 Standard addition technique 10 Calculation and expression of the result 10.1 General <\/td>\n<\/tr>\n | ||||||
| 58<\/td>\n | 10.2 External calibration 10.3 Standard addition method with only one addition 10.4 Standard addition method with several additions <\/td>\n<\/tr>\n | ||||||
| 59<\/td>\n | 10.5 Calculation of the element content in the sample <\/td>\n<\/tr>\n | ||||||
| 60<\/td>\n | 10.6 Example of calculation after standard addition technique with one addition 11 Precision 11.1 Inter-laboratory test 11.2 Repeatability 11.3 Reproducibility <\/td>\n<\/tr>\n | ||||||
| 64<\/td>\n | 12 Test report <\/td>\n<\/tr>\n | ||||||
| 65<\/td>\n | Annex\u00a0A (informative)Results of the inter-laboratory test <\/td>\n<\/tr>\n | ||||||
| 71<\/td>\n | Annex\u00a0B (informative)Notes on the detection technique, interferences and quantification B.1 General B.2 Interferences B.2.1 General B.2.2 Spectral interferences B.2.3 Ionization interferences B.2.4 Physical interferences B.3 Quantification and matrix matching B.3.1 General <\/td>\n<\/tr>\n | ||||||
| 72<\/td>\n | B.3.2 Calibration curve B.3.3 Matrix matching B.3.4 Standard addition <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" Tracked Changes. Animal feeding stuffs. Methods of sampling and analysis. Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead by ICP-AES<\/b><\/p>\n |