Effect of the matrix in mass spectrometry using an inductively coupled plasma

1998 ◽  
Vol 65 (5) ◽  
pp. 804-811 ◽  
Author(s):  
A. A. Pupyshev ◽  
N. L. Vasil’eva ◽  
S. V. Golik
2021 ◽  
Vol 25 (2) ◽  
pp. 98-109
Author(s):  
P. A. Otopkova ◽  
◽  
A. M. Potapov ◽  
A. I. Suchkov ◽  
A. D. Bulanov ◽  
...  

In order to study the isotopic effects in semiconductor materials, single crystals of high chemical and isotopic purity are required. The reliability of the obtained data on the magnitude and the direction of isotopic shifts depends on the accuracy of determining the concentration of all stable isotopes. In the isotopic analysis of enriched “silicon-28” with a high degree of enrichment (> 99.99%), it is necessary to determine the impurities of 29Si and 30Si isotopes at the level of 10-3 ¸ 10-5 at. %. At this concentration level, these isotopes can be considered as impurities. It is difficult to achieve high measurement accuracy with simultaneous registration of the main and “impurity” isotopes in such a wide range of concentrations. The registration of analytical signals of silicon isotopes must be carried out in the solutions with different matrix concentrations. The use of the solutions with the high concentration of the matrix element requires the introduction of corrections for matrix noise and the drift of the instrument sensitivity during the measurement. It is possible to reduce the influence of the irreversible non-spectral interference and sensitivity drift by using the method of internal standardization. The inconsistency of the literature data on the selection criteria for the internal standard required studying the behavior of the signals of the “candidates for the internal standard” for the ELEMENT 2 single-collector high-resolution inductively coupled plasma mass spectrometer on the matrix element concentration and the nature of the solvent, as well as on the solution nebulizing time. Accounting for the irreversible non-spectral matrix noise and instrumental drift in isotopic analysis of enriched “silicon-28” and initial 28SiF4 by inductively coupled plasma mass spectrometry had allowed us to reduce by 3-5 times the random component and by more than an order of magnitude the systematic component of the measurement error in comparison with the external standard method. This made it possible to carry out, with sufficient accuracy, the operational control of the isotopic composition of enriched “silicon-28”, both in the form of silicon tetrafluoride and polycrystalline silicon obtained from it, using a single serial device in the range of isotopic concentrations 0.0001–99.999%.


Minerals ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 583 ◽  
Author(s):  
Wu ◽  
Li ◽  
Ling ◽  
Yang ◽  
Li ◽  
...  

The oxygen (O) and neodymium (Nd) isotopic composition of monazite provides an ideal tracer of metamorphism and hydrothermal activity. Calibration of the matrix effect and monitoring of the external precision of monazite O–Nd isotopes with microbeam techniques, such as secondary ion mass spectrometry (SIMS) and laser ablation-multicollector-inductively coupled plasma-mass spectrometry (LA-MC-ICPMS), require well-characterized natural monazite standards for precise microbeam measurements. However, the limited number of standards available is impeding the application of monazite O–Nd isotopes. Here, we report on the RW-1 monazite as a potential new working reference material for microbeam analysis of O–Nd isotopes. Microbeam measurements by electron probe microanalysis (EPMA), SIMS, and LA-MC-ICPMS at 10–24 µm scales have confirmed that it is homogeneous in both elemental and O–Nd isotopic compositions. SIMS measurements yield δ18O values consistent, within errors, with those obtained by laser fluorination techniques. Precise analyses of Nd isotope by thermal ionization mass spectrometry (TIMS) are consistent with mean results of LA-MC-ICPMS analyses. We recommend δ18O = 6.30‰ ± 0.16‰ (2SD) and 143Nd/144Nd = 0.512282 ± 0.000011 (2SD) as being the reference values for the RW-1 monazite.


2021 ◽  
Vol 87 (7) ◽  
pp. 17-22
Author(s):  
Е. M. Dvoryanchikova ◽  
К A. Dzhevello ◽  
D. D. Galuzin

The impurities contained in lead and lead-based alloys, which are widely used in various branches of industry, i.e., nuclear, medical, electrical engineering, etc., affect their physicochemical properties which necessitates developing of the reliable method for the impurity determination. Photometric, spectral, and chemical — spectral methods used to address this problem are labor-intensive and do not always have the required sensitivity. A method of inductively coupled plasma mass spectrometry (ICP-MS) coupled with High Matrix Introduction (HMI) technology has been proposed as alternative easy to use procedure designed to be more sensitive. The Agilent HMI Sample Injection System provides inline dilution of the sample aerosol (supplied from the spray chamber to the burner) with pure argon. This method of sample introduction provides for analysis of the solutions with a solute content of up to 1% and higher. The aerosol dilution reduces concentration of the matrix and solvent at the inductively coupled plasma interface without conventional dilution. In this case, the matrix suppression of impurities is almost eliminated and CeO+/Ce+ is reduced to 0.2%, while the typical CeO+/Ce+ ratio for the Agilent 7500 mass spectrometers is 1 – 2%, but no more than 3%. We present application of this method to the analysis of Mg, Ca, Fe, Cu, As, Ag, Sn, Sb, Bi in lead by an Agilent 7500cx ICP-MS with preliminary acid digestion of lead samples in a microwave autoclave. The use of the HMI system made it possible to exclude the stage of sample dilution, reducing the possibility of sample contamination with a diluent, and to determine the content of impurities in a highly concentrated matrix at a level of 10–4 – 10–5 %. The efficiency of the method, as well as the possibility of using multi-element standard solutions prepared with 1% nitric acid for analysis of the samples with high lead content is shown.


1989 ◽  
Vol 43 (7) ◽  
pp. 1252-1257 ◽  
Author(s):  
David Ekimoff ◽  
Ann Marie Van Norstrand ◽  
David A. Mowers

The capabilities of Inductively Coupled Plasma Mass Spectrometry for elemental survey analysis have been characterized. The analysis is a three-step process which involves collecting a spectrum from mass 5 to 240, deconvolving the spectrum into elemental constituents, and converting the elemental count rates to concentrations. The entire process takes less than 10 min per sample. Detection limits are generally less than 1 ng/mL, and the precision of 16 replicate analyses of a sample is between 5 and 20% for the majority of the elements detected. It was determined that the figures of merit for this analysis did not vary significantly as the matrix changed.


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