The Rapid Determination of Gold on Activated Carbon by X-Ray-Fluorescence Spectrometry Using Radioactive Isotopes

1986 ◽  
Vol 40 (8) ◽  
pp. 1190-1194 ◽  
Author(s):  
A. M. E. Balaes

A method is presented for the rapid (15 to 20 min) analysis of activated carbon from carbon-in-pulp (CIP) plants for its gold content. The method involves the use of microprocessor-controlled energy-dispersive x-ray-fluorescence spectrometer, using excitation by the radioactive isotope 218Pu, and a background-ratio technique to correct for small variations in the matrix. The gold can be determined in dried granular carbon and milled carbon, provided that the calibration standards and samples are in the same physical form. It is shown that, because of the large differences in composition of the matrices of loaded and eluted carbon, two calibration curves need to be established, one for gold concentrations lower than 200 μg/g, the other for gold concentrations higher than 200 μg/g. The calibration curves for milled carbon showed less scattering of the calibration points than those for granular carbon, and the relative standard deviation of the results for milled carbon was 1% as against 2% for granular carbon.

2021 ◽  
Author(s):  
Tao Lin ◽  
Xinglian Chen ◽  
Li Wang ◽  
Haixian Fang ◽  
Maoxuan Li ◽  
...  

Abstract The simultaneous determination method of 8 amide pesticides by multi-walled carbon nanotubes (MWCNs) cleanup, combined with QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry has been developed and successfully applied in complex matrix such as green onions, celery, leeks, citrus, lychees, avocado. The matric effect of MWCNs is optimized and compared with QuEChERS materials. The results show that MWCNs can effectively reduce the matrix effect in sample extraction. The mass spectrometry is optimized, through their chemical structure skeletons, the ESI+ and ESI- mode are simultaneously scanned in the method. The coefficient (r) is greater than 0.9990, the limit of quantification ranges from 0.03 to 0.80 μg/kg, the recovery rate ranges from 71.2% to 120%, and the relative standard deviation (RSD) ranges from 3.8% to 9.4%. The method is fast, simple, sensitive, and has good purification effect. It is suitable for the rapid determination of amide pesticides in complex matrix agri-food.


2017 ◽  
Vol 726 ◽  
pp. 85-89
Author(s):  
Lei Zhang ◽  
Man Li ◽  
Hai Jian Li ◽  
Xin Song

Energy dispersive X-ray fluorescence spectrometry (EDXRF) allows a rapid determination of the concentration of elemental constituents or the thickness of thin film, it has been widely used in the industry of thin film thickness. But for multilayer film, especially the middle layer, with the absorption and enhance effect of other layers, the thickness and intensity of the middle layer is not a linear relationship. This paper reports a quantitative analysis of multilayer film thicknesses based on the use of EDXRF and fundamental parameters method. The thickness of multilayer film can be easily determined with the CTCFP software because it requires a minimum number of pure elementals only. Analysis of double-layer thin films using the CTCFP software shows that the inter-element and inter-layer X-ray absorptions and enhancements in a specimen have been determined properly. Results obtained on the standards confirmed the accuracy of the method.


2002 ◽  
Vol 56 (1) ◽  
pp. 58-61
Author(s):  
F. Bosch-Reig ◽  
J. V. Gimeno-Adelantado ◽  
S. Sánchez-Ramos ◽  
D. J. Yusá-Marco ◽  
F. Bosch-Mossi ◽  
...  

This paper is an analytical study of the possibility of applying the linear range of the substitution-dilution method to correct the matrix effect in quantitative analysis by X-ray fluorescence (XRF) spectroscopy. The analytical range is obtained from a series of samples prepared in the form of glass discs by substituting the unknown sample with a standard sample (substitution factor, h) including a diluent-melt. In general, the substitution-dilution method is hyperbolic in character and therefore the diluent is required to ensure linear behavior between If vs. h in the experimental range. The linear range is located between the concentrations of standard and unknown for each element analyzed. This linear model makes it possible to correct the matrix effect in quantitative analysis by XRF using a single multi-elemental standard for different types of samples with a complex matrix, such as geologicals and cements. The results found for Si, Ti, Al, Fe, Mn, Ca, K, and P in soil and sediment samples and Si, Fe, Al, Ca, and K in cements (white and gray) are statistically satisfactory. Thus, the mean relative standard deviation calculated for all analytes in each sample was: ±4.0% and ±5.0% in soils; ±5.0% in sediments; and ±6.0% or ±3.0% in cements, white and gray, respectively.


Heritage ◽  
2020 ◽  
Vol 3 (4) ◽  
pp. 1302-1329
Author(s):  
Belgin Demirsar Arli ◽  
Gulsu Simsek Franci ◽  
Sennur Kaya ◽  
Hakan Arli ◽  
Philippe Colomban

The aim of this study is to estimate the uncertainty of a portable X-ray fluorescence (p-XRF) instrument for the (semi-quantitative) analyses of tiles with underglaze decoration. Before starting the campaign of on-site measurements, the optimum acquisition time and the most accurate calibration mode were selected. For this purpose, the elemental composition of two glass standards of NIST (SRM610 and SRM612) and a Corning A standard were measured with varied times (5–360 s) and in different calibration modes (Mining, Mining Light Elements, Soil, and Rare Earth Elements). Afterwards, a set of blue-and-white tiles that was unearthed at Iznik Tile Kilns Excavation between the dig seasons of 2015 and 2019 was examined with p-XRF by selecting ten points of measure from each layer (body, transparent glaze, and blue coloured areas). The elemental composition of different layers was evaluated by means of the intragroup and intergroup data. They were also compared to the previous studies and found that the corrosion-free, homogeneous, and non-porous surfaces decrease the relative standard deviation (RSD) by increasing the consistency of the compositional data. The major elements found in the matrix of each layer (Al and Si for the body, Pb and Sn for the glaze) have the lowest value of RSD, as expected. However, the comparison of the data with the analysis of the reference materials showed that the content of Mg and also Si, which belong to the low-Z elements group, is shifted relatively towards the higher compositional values. The impossibility of measuring the elemental composition of sodium does not hinder the classification of the samples. Although the transition metals have very low concentrations, p-XRF measurements appear rather consistent and the intrinsic scattering of the data observed for a single artefact is largely smaller than those observed for the tiles of different historical buildings. Thus, it allows the classification to be made related to the different techniques used.


2000 ◽  
Vol 83 (3) ◽  
pp. 762-770 ◽  
Author(s):  
Holger Hartmann ◽  
Jürgen Burhenne ◽  
Karin Müller ◽  
Hans G Frede ◽  
Michael Spiteller

Abstract The applicability of online trace enrichment with custom-made coated capillaries combined with tandem mass spectrometry was demonstrated for the target analysis of selected pesticides (mainly herbicides, e.g., triazines, phenylureas, and acetanilides) in water. The developed method allows rapid determination of several widely used plant protectants within a total analysis time of 11 min. Good linearity (r ≥ 0.995) was obtained for the selected pesticides in the range of 0.050–50 μg/L. The relative standard deviations (RSDs) of the peak areas were ≤3.8% for spiked Milli-Q water (5 μg/L). The RSDs obtained in analyses of spiked (1 μg/L) water samples (brook water, river water, sewage plant effluent) ranged from 2.9 to 6.8%, indicating low influence of the matrix on enrichment and detection. The detection limits, which ranged from 10 to 90 ng/L, fulfilled the requirements of the European regulations for drinking water. The polyacrylate coating of the extraction capillary showed good stability in the presence of water and acetonitrile and allowed ≥100 extractions with 1 capillary.


2005 ◽  
Vol 59 (12) ◽  
pp. 1465-1469 ◽  
Author(s):  
Z. Spolnik ◽  
K. Belikov ◽  
K. Van Meel ◽  
E. Adriaenssens ◽  
F. De Roeck ◽  
...  

A new commercial energy dispersive X-ray fluorescence spectrometer (EDXRF), applying a three-dimensional geometry and high-energy excitation, was optimized for the quantitative analysis of aerosols deposited on filters. The preliminary results are presented here. First-order calibration curves were obtained for 20 elements deposited on the filters. The accuracy of the applied method and of the obtained calibration curves was checked by the measurement of a standard reference material from NIST. The precision of the analysis for the majority of the analytes was better than 10%. Due to the obtained low detection limits, it is possible to determine the analytes usually present at very low concentrations in ambient air, such as, e.g., Cd, Sb, Cr, and V. It is also possible to decrease significantly the time of analysis or the time of the sampling.


2013 ◽  
Vol 781-784 ◽  
pp. 2336-2339
Author(s):  
Jia Lin Qi ◽  
Jia Rui Qi ◽  
Zhao Kun Wang ◽  
Gui Peng Yang ◽  
Chong Lin Wang

Recently determination of harmful elements in fertilizer has been paid growing attention. The determination method of cobalt in fertilizer by Wavelength Dispersive X-ray Fluorescence Spectrometry (WD-XRF) is developed. The calibration samples are made of blank compound fertilizer to simulate the matrix. The sample covered with microcrystalline cellulose is pressed at 35t for 60s, and cobalt content is determined by WD-XRF. This method has a good repeatability and accuracy with the linearity in the ranges of 0-2000mg/kg. The relative standard deviation is not more than 2.0%. The results obtained from WD-XRF and ICP-AES showed an acceptable agreement. 43 fertilizer samples are collected from 18 countries and determined. The cobalt contents are all not more than 13mg/kg.


Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S


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