Loose‐powder technique for X‐ray fluorescence analysis of ancient pottery using a small (100 mg) powdered sample

Abstract

A molded-loose-powder technique using a small powdered sample (100 mg) was developed for the X-ray fluorescence analysis of 22 components () in ancient pottery. This loose powder specimen was prepared by pressing the small powdered sample into a sample holder, formed from a stainless steel disk (48-mm diameter  0.8-mm height) with a hole (11-mm diameter), by hand. Calibration standards were prepared by homogenizing chemical reagents containing these 22 analytes using the concentration ranges of 166 ancient potteries and three clay materials from Japan. The calibration curves of these benchmark mixtures exhibited a good linearity (correlation coefficient, r = 0.990-1.000), accuracy, and reproducibility compared with those of other synthesized specimens and three reference standards. The lower limits of detection were less than tens of mg kg À1 (e.g., 94 mg kg À1 for Na 2 O, 11 mg kg À1 for P 2 O 5 , 1.1 mg kg À1 for Rb, and 0.9 mg kg À1 for Y). Using the present method, we determined 22 components in two prehistoric potteries from Japan. The advantage of this method is that only a small amount of sample is required, which can be prepared easily and rapidly and reused for other analyses. Hodogaya, Yokohama, Japan) and Yayoi pottery (from Daikata, Chiba, Japan), were used to evaluate the molded-loose-powder Loose-powder technique for X-ray fluorescence analysis of pottery

Preparation of arsenic‐containing white rice grains as calibration standards for X‐ray fluorescence analysis of total arsenic in cereals

“…Sample thickness is an important parameter for XRF analysis . Samples with sufficient thickness are desirable to avoid analytical errors resulting from a difference in the absorption effects.…”

Development of undersized (12.5 mm diameter) low‐dilution glass beads for X‐ray fluorescence determination of 34 components in 200 mg of igneous rock for applications with geochemical and archeological silicic samples

“…The intervals optimized evenness for ten major oxides and bias toward low concentration for 24 minor elements. The composition of the calibration standard set was constructed by reference to recommended values of Geological Survey of Japan geochemical references and calibration ranges of igneous rock and ancient pottery …”

Crystalline Phase Quantitation of Sintered Ore with Powder X-ray Diffractometry with Rietveld Refinement

“…These reagents all exhibited particle sizes less than 10 μm, as reported elsewhere. 22) All reagents were dried under the appropriate conditions 23) using an electric furnace (FUM312PA; Toyo Seisakusho Kaisha, Ltd., Japan).…”

“…A measurement chamber in the spectrometer was regulated at a vacuum of several Pascals to analyze the molded loose powder specimens. 22) The measurement diameter was 10 mm. Two collimators, arranged between a sample and a dispersive crystal, were used for the present measurements: a coarse collimator (450 μm slits) for Al, Si, Ca, and Fe, which is regular size, and a fine collimator (150 μm slits) for Mg to prevent overlap with Ca Kα (n = 3).…”

“…Molded loose powder 22) was prepared for the XRF analyses of sintered ore samples and calibration standard powders. 33,34) A powdered sample (1.5 g) was placed into a sample holder with an acrylic disk (48 mm diameter × 5 mm height) with a hole (11 mm diameter) in the center.…”