Comparación de procedimientos para analizar fertilizantes potásicos

2011 
Se compararon cinco metodos analiticos para determinar potasio en fertilizantes inorganicos. Dos contemplaron la extraccion con una mezcla de acidos minerales y su determinacion por dos tecnicas: espectrofotometria de absorcion atomica y fotometria de llama, y dos metodos se basaron en la extraccion con agua y la determinacion por las dos tecnicas mencionadas. En el quinto metodo se extrajo el potasio con oxalato de amonio, y su cuantificacion se realizo por volumetria. Se establecio un diseno estadistico de bloques al azar con cinco tratamientos (metodos) y cuatro repeticiones (laboratorios). Cada analisis se realizo por triplicado. Los procedimientos se aplicaron a cinco fertilizantes y un reactivo estandar (KH 2 PO 4 ). Este ultimo se utilizo para la determinacion de la exactitud. Se obtuvieron resultados equivalentes, independientemente del extractante usado y de la forma de determinacion aplicada, lo cual es favorable, ya que permitiria a los laboratorios decidir el procedimiento mas conveniente de acuerdo a su disponibilidad de equipos y reactivos. La exactitud resulto aceptable segun los criterios considerados, y fluctuo entre 97,70 %  y  99,75 % de recuperacion de K 2 O. Los valores de repetibilidad variaron entre 0,207 y 3,896,  y estuvieron asociados a los niveles de K 2 O en los casos que involucraron solamente las determinaciones por absorcion atomica (extraccion con acido y agua) y fotometria de llama (extraccion en acido). La reproducibilidad no presento esta asociacion en ninguno de los procedimientos evaluados, y sus valores oscilaron entre 1,979 y 2,7891.  Palabras Clave: absorcion atomica, fotometria de llama, estudios interlaboratorios, precision, exactitud. Abstract Five analytical methods for determining potassium in inorganic fertilizers were compared. In two methods the potassium was extracted with a mixture of mineral acids and determined by two techniques: atomic absorption spectrophotometry and flame photometry. Two other methods were based on water extraction and determination by the two techniques referred to above. In the fifth method the potassium was extracted with ammonium oxalate and measured by titration. A statistical design of randomized blocks with five treatments (methods) and four repetitions (laboratories) was established. Each analysis was performed by triplicate. The procedures were applied to five different fertilizers and a standard reagent (KH 2 PO 4 ). The latter was used to determine the accuracy of the compared methods. Equivalent results were obtained regardless of the extractant used and the method of determining applied. This is favorable because it allows individual laboratories to decide the most appropriate procedure, according to their availability of equipment and reagents. The accuracy ranged between 97.70% and 99.75% of K 2 O recovery. The repeatability values ranged from 0.207  to  3.896 and were associated with levels of K 2 O in the methods based on determinations with atomic absorption (extraction with acid and water) or flame photometry (acid extraction). The reproducibility did not show this association in any of the procedures evaluated and their values varied between 1.978 and 2.7891. Key words: Atomic absorption, flame photometry, inter-laboratory study
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