Soils are complex matrices and their geochemical investigation necessarily needs reliable Certified Reference Materials (CRMs), i.e. standards, to support analytical precision and accuracy. In particular, the definition of soil multi-element CRMs is particularly complex and involves an inter-laboratory program that employs numerous analytical techniques. In this study, we present the results of the inter-calibration experiment focused on the certification of two new soil standards named AMS-ML1 and AMS-MO1. The two soils developed on sandstone and serpentinite parent materials, respectively. The experiment involved numerous laboratories and focused on the evaluation of soil physicochemical parameters and geochemical analyses of major and trace elements by X-ray fluorescence (XRF) and Inductive Coupled Plasma techniques (ICP-OES and ICP-MS). The data was statistically elaborated. Three levels of repeatability and accuracy in function of the different analytical methods and instrumentation equipment was observed. The statistical evaluation of the results obtained by ICP-OES on Aqua Regia extracts (i.e., Lilliefors test for normally, Grubbs test for outliers, Cochran test for outliers in variances and ANOVA) allowed to computed some certified values for the two proposed soil standards. This preliminary study will represent the first step of a more thorough intercalibration ring-test involving a higher number of laboratories, in order to propose the investigated matrices as CRMs.

I suoli sono matrici complesse e la loro indagine geochimica ha bisogno di materiali certificati di riferimento (CRM) per valutarne la precisione analitica e l'accuratezza. In particolare la preparazione di materiali di riferimento idonei al controllo di determinazioni analitiche effettuate sul suolo richiede un programma interlaboratorio con l’impiego di metodologie e strumentazioni differenti. In questo studio vengono presentati i risultati dell'esperimento di intercalibrazione incentrato sulla certificazione di due nuovi standard di suoli denominati AMS-ML1 e AMS-MO1 originatisi rispettivamente su rocce arenacee e serpentinose. L'attività sperimentale ha coinvolto numerosi laboratori e, oltre alla valutazione di parametri chimico-fisici del suolo, si è concentrata sull’affinamento delle tecniche analitiche mediante fluorescenza a raggi X (XRF) e spettrometria di massa (ICP-OES, ICP-MS). L’elaborazione statistica ha permesso di evidenziare tre livelli di ripetibilità e precisione in funzione dei differenti metodi di analisi e della strumentazione utilizzata. Nel caso specifico dell’estrazione in Aqua Regia e determinazione in ICP-OES i risultati, elaborati mediante test di Lilliefors, di Grubbs, di Cochran e ANOVA, hanno permesso di definire il livello di certificazione per alcuni elementi riferiti ai due standard proposti. Lo studio rappresenta un primo livello di intercalibrazione e verranno effettuati ulteriori ring test con il contributo di più laboratori specializzati, in modo da conseguire una certificazione internazionale.

Critical evaluation of an intercalibration project focused on the definition of new multi-element soil reference materials (AMS-MO1 and AMS-ML1)

BIANCHINI, Gianluca
Secondo
;
TASSINARI, Renzo
Penultimo
;
2014

Abstract

Soils are complex matrices and their geochemical investigation necessarily needs reliable Certified Reference Materials (CRMs), i.e. standards, to support analytical precision and accuracy. In particular, the definition of soil multi-element CRMs is particularly complex and involves an inter-laboratory program that employs numerous analytical techniques. In this study, we present the results of the inter-calibration experiment focused on the certification of two new soil standards named AMS-ML1 and AMS-MO1. The two soils developed on sandstone and serpentinite parent materials, respectively. The experiment involved numerous laboratories and focused on the evaluation of soil physicochemical parameters and geochemical analyses of major and trace elements by X-ray fluorescence (XRF) and Inductive Coupled Plasma techniques (ICP-OES and ICP-MS). The data was statistically elaborated. Three levels of repeatability and accuracy in function of the different analytical methods and instrumentation equipment was observed. The statistical evaluation of the results obtained by ICP-OES on Aqua Regia extracts (i.e., Lilliefors test for normally, Grubbs test for outliers, Cochran test for outliers in variances and ANOVA) allowed to computed some certified values for the two proposed soil standards. This preliminary study will represent the first step of a more thorough intercalibration ring-test involving a higher number of laboratories, in order to propose the investigated matrices as CRMs.
2014
EQA
Livia Vittori, Antisari; Bianchini, Gianluca; Enrico, Dinelli; Gloria, Falsone; Aldo, Gardini; Andrea, Simoni; Tassinari, Renzo; Gilmo, Vianello...espandi
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11392/2273014
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