X-ray Fluorescence Analysis of High-Density Brines Using a Compton Scattering Ratio Technique

1990 ◽  
Vol 34 ◽  
pp. 285-292
Author(s):  
Michael L. Samuelson ◽  
Stanley B. McCormell

AbstractHigh-density brines are used to control high pressure during oil and gas well operations. These dense brines (15 to 20 lb/gal) are solutions prepared from sale such as calcium chloride, calcium bromide, zinc bromide and/or combinations. During stages of completion, excessive losses of these expensive brines to the production zone can occur. Before the brine is reused in other oil and/or gas well operations, the brine may need to be reweighted. An analysis of the brine composition must be obtained to properly add the correct amount of salts.Standard addition or internal standardization methods are commonly used in X-ray fluorescence (XRF) applications but negate one of the advantages of XRF-elimination of tedious sample preparation. Scattered X-ray intensity has been used successfully to correct matrix effects in XRF applications. A Compton scatter ratio method is very advantageous for samples having a low atomic number, for which the scattered intensity is high. This paper describes an XRF method for determining Ca, CI, and Zn in high-density brines as well as the matrix correction for Br using a scattered X-ray ratio technique.

1973 ◽  
Vol 27 (5) ◽  
pp. 352-355 ◽  
Author(s):  
D. L. Taylor ◽  
G. Andermann

The “degree of internal standardization” for the scattered radiation method of compensation for matrix effects in x-ray fluorescence analysis is defined as the closeness of agreement between the results of analyses of specimens containing identical concentrations of analyte but with differing over-all elemental constituencies. The definition is derived in mathematical terms and is applied to experimental data of analyses of calcium in aqueous solutions containing different dissolved substances as matrix variants. The matrix compensation effectiveness of various wavelengths of scattered radiation can be clearly indicated. Interpretation of the results in terms of basic spectroscopic parameters is offered.


1968 ◽  
Vol 22 (4) ◽  
pp. 321-324 ◽  
Author(s):  
Frank Cuttitta ◽  
Harry J. Rose

A new approach to solving matrix problems in x-ray fluorescence analysis of trace elements has been applied to the determination of bromine in saline waters and zinc in silicates. The method requires no prior knowledge of the chemical composition of the sample. Marked matrix effects are minimized by dilution, and the problem of variable backgrounds due to residual matrix effects is solved by using a slope-ratio technique. In this proposed technique, the slope of a standard curve prepared from pure solutions is compared with that of spiked samples. The ratio of the slopes of these two curves permits the calculation of an adjusted background which does not significantly differ from that of an absorbent impregnated with the sample matrix free of the element sought. Experimental parameters concerning the technique are presented. The excellent agreement of the zinc and bromine data with analytical results obtained by more conventional methods suggests that the technique can be used for the determination of other trace constituents in geologic materials. Application of the slope-ratio technique to other modes of instrumental analysis appears feasible.


2020 ◽  
Vol 38 (12) ◽  
pp. 1331-1344
Author(s):  
Shohel Siddique ◽  
Kyari Yates ◽  
Kerr Matthews ◽  
Laszlo J Csetenyi ◽  
James Njuguna

Oil-based mud (OBM) waste from the oil and gas exploration industry can be valorised to tailor-made reclaimed clay-reinforced low-density polyethylene (LDPE) nanocomposites. This study aims to fill the information gap in the literature and to provide opportunities to explore the effective recovery and recycling techniques of the resources present in the OBM waste stream. Elemental analysis using inductively coupled plasma–optical emission spectrometry (ICP-OES) and X-ray fluorescence analysis, chemical structural analysis by Fourier transform infrared (FTIR) spectroscopy, and morphological analysis of LDPE/organo-modified montmorillonite (LDPE/MMT) and LDPE/OBM slurry nanocomposites by scanning electron microscopy (SEM) have been conducted. Further analysis including calorimetry, thermogravimetry, spectroscopy, microscopy, energy dispersive X-ray analysis and X-ray diffraction (XRD) was carried out to evaluate the thermo-chemical characteristics of OBM waste and OBM clay-reinforced LDPE nanocomposites, confirming the presence of different clay minerals including inorganic salts in OBM slurry powder. The microscopic analysis revealed that the distance between polymer matrix and OBM slurry filler is less than that of MMT, which suggests better interfacial adhesion of OBM slurry compared with the adhesion between MMT and LDPE matrix. This was also confirmed by XRD analysis, which showed the superior delamination structure OBM slurry compared with the structure of MMT. There is a trend noticeable for both of these fillers that the nanocomposites with higher percentage filler contents (7.5 and 10.0 wt% in this case) were indicated to act as a thermal conductive material. The heat capacity values of nanocomposites decreased about 33% in LDPE with 7.5 wt% MMT and about 17% in LDPE with 10.0 wt% OBM slurry. It was also noted, for both nanocomposites, that the residue remaining after 1000°C increases with the incremental wt% of fillers in the nanocomposites. There is a big difference in residue amount (in %) left after thermogravimetric analysis in the two nanocomposites, indicating that OBM slurry may have significant influence in decomposing LDPE matrix; this might be an interesting area to explore in the future. The results provide insight and opportunity to manufacture waste-derived renewable nanocomposites with enhanced structural and thermal properties.


Clay Minerals ◽  
2006 ◽  
Vol 41 (3) ◽  
pp. 717-725 ◽  
Author(s):  
S. Battaglia ◽  
L. Leoni ◽  
F. Sartori

AbstractA new method for determining the cation exchange capacity (CEC) of clays is proposed. The method is based on X-ray fluorescence analysis of natural and Ba-exchanged clays following the analytical procedure suggested by Franzini et al. (1975). This procedure, which utilizes powder pellets and is based on a full matrix correction method, is frequently applied in Earth Sciences laboratories for the routine analysis of minerals and rocks. For the analysis of Ba-exchanged clays, Franzini's procedure has been modified slightly to account for the contribution of Ba to matrix effects.The new method, which furnishes both the CEC and the chemical compositions of the whole natural clay samples, has been tested on the eight ‘Source Clays’ of The Clay Minerals Society. The results compare well with data reported in the literature and confirm the accuracy and precision of the method and make it a valid alternative to techniques based on wet chemistry, execution of which is usually more time-consuming and which often requires greater analytical skill.


1967 ◽  
Vol 11 ◽  
pp. 1-22
Author(s):  
Eugene P. Bertin

AbstractUsually X-ray spectrometric analyse? of samples in their original forms—solid, powder, small fabricated parts, liquid, etc.—are more rapid and convenient than analyses by any other method. Thus, the analyst is well advised to strive to analyze samples in their original form whenever practical. However, it is often necessary to reduce nonliquid samples to some other form, for example, when standards are unavailable in the original form, when the same substance is received for analysis in a variety of forms, when homogeneity or matrix effects are severe, or when an internal standard must be added. In such cases, samples and standards are often reduced to a powder, a fusion product, or a solution. If the decision is made to put the sample into solution, the many well-known advantages of solution techniques are realised, including: (1) homogeneity; (2) easy preparation of standards and blanks; (3) easy concentration, dilution, separation, and other treatment; (4) reduced matrix effects and wide choice of ways to deal with matrix effects; (5) wide choice of ways to present the specimen to the spectrometer; and (6) applicability of internal-standard, standard-addition or -dilution, indirect, absorption, and scatter methods. This paper reviews work reported since 1960 in which the specimen is presented to the spectrometer in liquid form. The review is not particularly critical and stresses experimental techniques and treatment of data rather than specific materials and results. The work is discussed in the following categories: (1) sensitivity ; (2) liquid-specimen cells; (3) interaction of primary beam and liquid specimens; (4) matrix effects; (5) indirect (association) analysis; (6) X-ray scatter methods; and (7) X-ray absorption-edge spectrometry.


1957 ◽  
Vol 1 ◽  
pp. 297-313
Author(s):  
Theodore Hall

AbstractAn X-ray fluorescence analysis unit has been designed and built especially for the measurement of certain mineral elements in individual biological tissue sections. Such a section may contain in the neighborhood of 10-10 grams of an element of interest, in a concentration in the range of 1-100 p.p.m.The unit consists of a special high-power X-ray tube with a builtin interchangeable secondary radiator, which irradiates the speciman with the characteristic lines of the radiator element) and a proportional counter and pulse-height analyzer system, which provides analysis of the X-ray spectrum emitted by the specimen. Because the emitted spectrum is greatly simplified by the use of an appropriate radiator element, a diffracting crystal can be omitted, permitting a great increase in absolute sensitivity.The system is feasible only because of two peculiarities of our biological specimens: they are so thin that matrix effects are negligible, and they consist essentially of a few mineral elements in a light matrix.Design considerations, calibration procedures, procedures for the analysis of the observed proportional counter pulse-height spectra and results to date will be discussed.


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