Determination of Arsenic and Lead in Earth and Sand Using EDXRF [JIS K 0470]

Significance of the Topic

The determination of arsenic and lead in soil and sand is essential to monitor environmental contamination, protect public health, and ensure compliance with regulatory standards such as JIS K0470.

Objectives and Study Overview

The goal of this application note is to demonstrate the rapid and accurate quantification of arsenic, lead, and other selected toxic elements in soil samples using an energy dispersive X-ray fluorescence (EDXRF) spectrometer, following the JIS K0470 method.

Methodology and Instrumentation

Sample preparation was conducted according to JIS K0470: soils were dried at 110°C, crushed, sieved to 106 µm, and finely powdered. Two grams of powder were mounted in sample cups lined with 5 µm polypropylene film. Calibration curves were established using JIS standard reference materials and NIST SRM 2711. A Shimadzu EDX-720 (and EDX-GP) with a Rh target X-ray tube, specific filters, and a 10 mm measurement diameter was employed. Analytical lines included As Kα and Pb Lβ1, with overlap correction and lower limits of detection and quantitation determined.

Main Results and Discussion

Calibration demonstrated linear response for arsenic and lead, with detection limits of 1.9 ppm (As) and 4.3 ppm (Pb), and quantitation limits of 6.5 ppm (As) and 14.6 ppm (Pb). Repeatability tests on a soil sample (Soil A) yielded average concentrations of 42.1 ppm As (CV 3.8%) and 53.9 ppm Pb (CV 4.1%). Qualitative analysis identified multiple elements, and quantitative FP-based analysis revealed major oxides (SiO2 57.8%, Al2O3 24.1%, Fe2O3 10.5%) along with trace As (0.005%) and Pb (0.005%).

Benefits and Practical Applications

• Non-destructive, multi-element simultaneous analysis
• Fast sample preparation and measurement (300 s)
• Compliance with JIS regulatory requirements
• Suitable for routine monitoring in factory, environmental, and quality control laboratories

Future Trends and Applications

Advances may include portable EDXRF for in-field testing, enhanced sensitivity through optimized detectors, automated data processing with chemometric models, and integration into real-time environmental monitoring networks.

Conclusion

The EDXRF method per JIS K0470 effectively quantifies arsenic and lead in soils with reliable detection limits and repeatability, offering a rapid and robust solution for environmental surveillance.

Reference

• JIS K 0470: Energy Dispersive X-Ray Fluorescence Spectrometric Method for Arsenic and Lead in Earth and Sand, Japanese Industrial Standard, 2008
• NIST SRM 2711: Montana II Soil Standard Reference Material
• Shimadzu Application News No. X238A, Determination of Arsenic and Lead in Earth and Sand Using EDXRF, Second Edition, Mar. 2015