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Direct determination of calcium and phosphorus in mineral supplements for cattle by wavelength dispersive X-ray fluorescence (WD-XRF)
Microchemical Journal ( IF 4.9 ) Pub Date : 2018-03-01 , DOI: 10.1016/j.microc.2017.11.002
Diego Victor Babos , Vinícius Câmara Costa , Marco Aurelio Sperança , Edenir Rodrigues Pereira-Filho

Abstract The current study describes a simple and rapid method for the direct determination of Ca and P in mineral supplements for cattle by wavelength dispersive - X-ray fluorescence (WD-XRF). For calibration, solid standards obtained through a set of reference materials (RMs) of mineral supplements for cattle with concentrations of Ca ranged from 120 to 223 g kg− 1 (r = 0.9809) and P ranged from 29 to 95 g kg− 1 (r = 0.9957) were used. For Ca, the matrix-matching using the RM 18/03 diluted in Na2CO3: NaCl (1:1 w/w) in the range of 0–204 g kg− 1 (r = 0.9975) was also used as calibration strategy. The proposed method presented limits of detection of 47 mg kg− 1 for Ca and 36 mg kg− 1 for P using calibrations with RMs and 61 mg kg− 1 to Ca using matrix-matching calibration strategy. Accuracy was assessed by the analysis of four RM of mineral supplements for cattle. A statistical evaluation using student's t-test showed that there is no significant difference between the value obtained with the proposed method and the certified value, at 95% confidence level. The method was successfully applied and is a good alternative to conventional acid digestion routine analysis for determination of Ca and P in mineral supplements for cattle.

中文翻译:

波长色散 X 射线荧光 (WD-XRF) 直接测定牛用矿物质补充剂中的钙和磷

摘要 本研究描述了一种通过波长色散 X 射线荧光 (WD-XRF) 直接测定牛用矿物质补充剂中 Ca 和 P 的简单快速方法。对于校准,通过一组牛用矿物质补充剂的参考材料 (RM) 获得的固体标准品的 Ca 浓度范围为 120 至 223 g kg−1 (r = 0.9809),P 浓度范围为 29 到 95 g kg−1 r = 0.9957) 被使用。对于 Ca,使用在 0–204 g kg− 1 (r = 0.9975) 范围内的 Na2CO3: NaCl (1:1 w/w) 稀释的 RM 18/03 的基质匹配也用作校准策略。所提出的方法提出了使用 RM 校准的 Ca 检测限为 47 mg kg-1,P 检测限为 36 mg kg-1,使用基质匹配校准策略对 Ca 的检测限为 61 mg kg-1。通过分析四种牛用矿物质补充剂来评估准确性。使用学生 t 检验的统计评估表明,在 95% 的置信水平下,使用建议方法获得的值与认证值之间没有显着差异。该方法已成功应用,是用于测定牛用矿物质补充剂中 Ca 和 P 的常规酸消解常规分析的良好替代方法。
更新日期:2018-03-01
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