Research on grain size effect in XRF analysis of pelletized samples

Mzyk, Zofia; Baranowska, Irena; Mzyk, Jan

doi:10.1002/xrs.534

Cited by 29 publications

(25 citation statements)

References 14 publications

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“…Samples of identical composition, but different thicknesses, can thus yield apparently different measured compositions if no correction is applied. This is similar to the particle size effect in powders, 4 though powders have the additional complication of geometric effects related to particle shape and orientation. A method for determining compositions for transmitting samples is the transmission emission method, 5,6 in which separate measurements are made of the transmitting sample, a standard of semi-infinite thickness and containing the element being assayed in the sample, and the transmitting sample in front of the standard.…”

Section: Introductionmentioning

confidence: 60%

Composition determination for complex and transmitting samples in x‐ray quantitative analysis

Vasquez

2008

X-Ray Spectrometry

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In this work, quantitative analysis of x-ray fluorescence measurements of transmitting samples with complex chemical composition is considered. A method is presented for analytical solution of sample composition including matrix effects, independent of sample thickness and requiring no standards. The method uses fundamental parameters and measured fluorescence signal intensities, and is applicable to transmission geometry measurements for which standard analyses are not applicable. Limitations of the analysis presented here are discussed.

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Section: Introductionmentioning

confidence: 60%

Composition determination for complex and transmitting samples in x‐ray quantitative analysis

Vasquez

2008

X-Ray Spectrometry

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“…The reagents, same as those used for the glass bead method and ), were used as calibration standards. These reagents had a particle size less than 10 mm [24] to attain adequate repeatability and avoid the effects of microabsorption [23] (Table 3). These standards were prepared by mixing 13 g of a mixture of these reagents using the V-type mixing machine for 90 min.…”

Section: Calibration Standards For Molded Loose Powdermentioning

confidence: 99%

“…However, it is difficult to obtain precise and accurate XRF analysis with a powder specimen (e.g., a pressed powder pellet or loose powder) because of micro-absorption and mineral effects. [23] In particular, it is difficult to prepare the specimen of powder samples using a mixture of chemicals owing to low homogeneity and particle size effects. Therefore, the precision and accuracy of the results obtained from the XRF analysis of loose powder are poorer than those obtained from the XRF analysis of glass beads.…”

Section: Introductionmentioning

confidence: 99%

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

2012

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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 Â 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

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“…Powder pellet production is simple and easy but prone to poor accuracy and reproducibility because of microabsorption and/or mineral effects. [11] Glass bead production is performed by mixing and fusing a powdered sample and an alkali flux. The XRF analysis of glass bead rock samples consisting of silicatelike earthenware is accurate, reproducible, and free from microabsorption effects.…”

Section: Introductionmentioning

confidence: 99%

Glass‐bead/X‐ray fluorescence analysis of earthenware body – sampling from heterogeneous earthenware

2011

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Samples of ancient earthenware were prepared in 1 : 10 glass beads for the X-ray fluorescence quantitation of 10 major elements (Na, Mg, Al, Si, P, K, Ca, Ti, Mn, and Fe). Calibration standards of the glass beads were used with a mixture of reagents in an arbitrary ratio instead of rock standards. The calibration curves were constructed using the reported values of Japanese wares and clay materials. The adequacy of conventional sampling methods was statistically evaluated by examining the homogeneities of two shards (112 g of Jomon ware and 92 g of Yayoi ware) with respect to their crystalline phases and 10 major constituents. Both shards were found to be heterogeneous. An important finding is that in the sampling from a shard, unless at least half of the shard is homogenized, small sampling cannot represent the whole shard. The sampling was found to be only marginally reliable because the K/Ca scatter diagram for determination of provenance showed regional characteristics, and the measured analytical values showed normal (or Gaussian) distributions. Furthermore, taking eight samples or above from a shard enhances the reliability of small sampling.

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Research on grain size effect in XRF analysis of pelletized samples

Cited by 29 publications

References 14 publications

Composition determination for complex and transmitting samples in x‐ray quantitative analysis

Composition determination for complex and transmitting samples in x‐ray quantitative analysis

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

Glass‐bead/X‐ray fluorescence analysis of earthenware body – sampling from heterogeneous earthenware

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