Metrological Study of Atomic Emission Spectrometers Based on CCD Lines

We proposed two simple, rapid, and convenient spectrophotometric methods are described for the determination of Amoxicillin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in first method) and colorimetric determination of the green colored solution for manganite ion at 610 nm formed after reaction of Amoxicillin with potassium permanganate as oxidant agent (in the second method) in basic medium. The working conditions of the methods were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 5-45 μg/ml. The detection limits and relative standared deviations were (2.573, 2.814 μg/ml) (2.137, 2.498) for the flame emission photometric method and (1.844, 2.016 μg/ml) (1.645,1.932) for colorimetric methods for capsules and suspensions respectively. The methods were successfully applied to the determination of Amoxicillin in capsules and suspensions, and the obtained results were in good agreement with the label claim. No interference was observed from the commonly encountered additives and expectancies.

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Rapid Catalyst Capture Enables Metal-Free Parahydrogen-Based Hyperpolarized Contrast Agents

10.26434/chemrxiv.6076175.v1 ◽

2018 ◽

Author(s):

Danila Barskiy ◽

Lucia Ke ◽

Xingyang Li ◽

Vincent Stevenson ◽

Nevin Widarman ◽

...

Keyword(s):

Magnetic Resonance ◽

Contrast Agents ◽

Inductively Coupled Plasma ◽

Organometallic Compounds ◽

Atomic Emission ◽

Platinum Group Metals ◽

Resonance Spectroscopy ◽

Plasma Atomic Emission ◽

Inductively Coupled

Hyperpolarization techniques based on the use of parahydrogen provide orders of magnitude signal enhancement for magnetic resonance spectroscopy and imaging. The main drawback limiting widespread applicability of parahydrogen-based techniques in biomedicine is the presence of organometallic compounds (the polarization transfer catalysts) in solution with hyperpolarized contrast agents. These catalysts are typically complexes of platinum-group metals and their administration in vivo should be avoided. Herein, we show how extraction of a hyperpolarized compound from an organic phase to an aqueous phase combined with a rapid (less than 10 seconds) Ir-based catalyst capture by metal scavenging agents can produce pure parahydrogen-based hyperpolarized contrast agents as demonstrated by high-resolution nuclear magnetic resonance (NMR) spectroscopy and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The presented methodology enables fast and efficient means of producing pure hyperpolarized aqueous solutions for biomedical and other uses.

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Rapid Catalyst Capture Enables Metal-Free Parahydrogen-Based Hyperpolarized Contrast Agents

10.26434/chemrxiv.6076175 ◽

2018 ◽

Author(s):

Danila Barskiy ◽

Lucia Ke ◽

Xingyang Li ◽

Vincent Stevenson ◽

Nevin Widarman ◽

...

Keyword(s):

Magnetic Resonance ◽

Contrast Agents ◽

Inductively Coupled Plasma ◽

Organometallic Compounds ◽

Atomic Emission ◽

Platinum Group Metals ◽

Resonance Spectroscopy ◽

Plasma Atomic Emission ◽

Inductively Coupled

Hyperpolarization techniques based on the use of parahydrogen provide orders of magnitude signal enhancement for magnetic resonance spectroscopy and imaging. The main drawback limiting widespread applicability of parahydrogen-based techniques in biomedicine is the presence of organometallic compounds (the polarization transfer catalysts) in solution with hyperpolarized contrast agents. These catalysts are typically complexes of platinum-group metals and their administration in vivo should be avoided. Herein, we show how extraction of a hyperpolarized compound from an organic phase to an aqueous phase combined with a rapid (less than 10 seconds) Ir-based catalyst capture by metal scavenging agents can produce pure parahydrogen-based hyperpolarized contrast agents as demonstrated by high-resolution nuclear magnetic resonance (NMR) spectroscopy and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The presented methodology enables fast and efficient means of producing pure hyperpolarized aqueous solutions for biomedical and other uses.

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Silicate analysis of carbonated rocks using ICP-AES with calibration by the concentration ratio

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2020-86-5-16-21 ◽

2020 ◽

Vol 86 (5) ◽

pp. 16-21

Author(s):

T. A. Karimova ◽

G. L. Buchbinder ◽

S. V. Kachin

Keyword(s):

Inductively Coupled Plasma ◽

Concentration Ratio ◽

Total Error ◽

Atomic Emission ◽

Emission Spectrometry ◽

Calibration Error ◽

Plasma Atomic Emission Spectrometry ◽

Standard Samples ◽

Inductively Coupled ◽

Carbonate Materials

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).

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Dc arc emission analysis of rare earth metals and their oxides with sorption preconcentration of impurities

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2018-84-11-9-14 ◽

2018 ◽

Vol 84 (11) ◽

pp. 9-14

Author(s):

E. S. Koshel ◽

V. B. Baranovskaya ◽

M. S. Doronina

Keyword(s):

Rare Earth ◽

Rare Earth Metals ◽

Analytical Signal ◽

Graphite Powder ◽

Atomic Emission ◽

Standard Samples ◽

Emission Analysis ◽

Sorption Preconcentration ◽

Sample Shape

The analytical capabilities of arc atomic emission determination of As, Bi, Sb, Cu, Te in rare earth metals (REM) and their oxides after preparatory group concentration using S,N-containing heterochain polymer sorbent are studied on a high-resolution spectrometer “Grand- Extra” (“WMC-Optoelectron-ics” company, Russia). Sorption kinetics and dependence of the degree of the impurity extraction on the solution acidity are analyzed to specify conditions of sorption concentration. To optimize the procedure of arc atomic emission determination of As, Bi, Sb, Cu, and Te various schemes of their sorption preconcentration and subsequent processing of the resulted concentrate with the addition of a collector at different stages of the sorption process have been considered. Graphite powder is used as a collector in analysis of rare earth oxides due to universality and relative simplicity of the emission spectrum. Conditions of analysis and parameters of the spectrometer that affect the analytical signal (mass and composition of the sample, shape and size of the electrodes, current intensity and generator operation mode, interelectrode spacing, wavelengths of the analytical lines) are chosen. The evaporation curves of the determinable impurities were studied and the exposure time of As, Bi, Sb, Cu, and Te in the resulted sorption concentrate was determined. Correctness of the obtained results was evaluated using standard samples of the composition and in comparisons between methods. The results of the study are used to develop a method of arc chemical-atomic emission analysis of yttrium, gadolinium, neodymium, europium, scandium and their oxides in a concentration range of n x (10-2 - 10-5) wt.%.

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Plasma parameters in atomic-emission spectral analysis of phosphate concentrates of the fission products

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2019-85-2-17-22 ◽

2019 ◽

Vol 85 (2) ◽

pp. 17-22

Author(s):

M. I. Khamdeev ◽

E. A. Erin

Keyword(s):

Spectral Analysis ◽

Chemical Composition ◽

Reference Materials ◽

Fission Products ◽

Atomic Emission ◽

Electric Arc ◽

Physical Parameters ◽

Arc Plasma ◽

Atomic Emission Spectral Analysis ◽

Excitation Processes

Physical parameters of electric arc plasma as well as their time dependences are calculated when analyzing phosphate precipitates of the fission products of irradiated nuclear fuel. Phosphate concentrates of the fission products are known for their complex chemical composition and high thermal and chemical stability. Hence, direct atomic emission spectral analysis of phosphate powders without transferring them into solutions is advisable. Different conditions of sample preparation and synthesis of the reference materials determine the different chemical forms of the elements to be determined. This, in turn, affects the kinetics of their evaporation in the electrode crate and excitation processes in the plasma. The known mechanisms of those processes cannot always be transferred to specific conditions of the given method of analysis thus entailing the necessity of studying the effect of the samples chemical composition on the results of determination, proper choice of spectroscopic carriers, detailed study of spectra excitation processes in spectral analysis, and analysis of the physical parameters of the electric arc plasma. We used the lines Zn I 307.206 nm and Zn I 307.589 nm to measure the effective temperature of the central hot sections of the arc in a range of4500 - 6500 K. NaCl, BaCl2 and NaCl + T1C1 were studied to reduce the effect of the sample elemental composition on excitation conditions of the spectra and their stabilization as a spectroscopic carrier. In control experiments we used carrier-free samples. The coincidence of the values of the plasma physical parameters within the measurement error not exceeding 20%, as well as the identity of the nature of the kinetic curves for samples of phosphate precipitates and synthetic reference materials prove their correctness. The result of the study substantiate correctness of the direct atomic-emission spectral procedure in analysis of phosphate concentrates of fission when using synthetic reference materials.

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ICP-MS AND ICP-AES ANALYSIS OF PLANT REFERENCE MATERIALS

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2019-85-6-11-24 ◽

2019 ◽

Vol 85 (6) ◽

pp. 11-24

Author(s):

I. V. Nikolaeva ◽

A. A. Kravchenko ◽

S. V. Palessky ◽

S. V. Nechepurenko ◽

D. V. Semenova

Keyword(s):

Reference Material ◽

Mass Spectrometer ◽

Reference Materials ◽

Atomic Emission ◽

Icp Ms ◽

Lithium Metaborate ◽

Relative Standard ◽

Microwave System ◽

Total Analysis ◽

Siberian Pine

Two methods — ICP-MS and ICP-AES are used for certification of the new reference material — needles of Siberian pine (NSP-1). Techniques of the analysis include decomposition of plant samples in two different ways: acid digestion in a microwave system MARS-5 and lithium metaborate fusion followed by ICP-MS and ICP-AES analysis of the solutions. Simultaneous determinations of all the elements were carried out in low, medium and high resolution using SF-mass-spectrometer ELEMENT and atomic-emission spectrometer IRIS Advantage with external calibrations and internal standards (In — ICP-MS, Sc —ICP-AES). Middle and high resolutions of ICP mass spectrometer were used for interference corrections. Data obtained by ICP-MS and ICP-AES with different decomposition techniques are in good agreement. The ICP-MS and ICP-AES techniques have been validated by the analysis of three plant reference materials: LB-1 (leaf of a birch), Tr-1 (grass mixture) and EK-1 (Canadian pondweed). These techniques were used for the determination of 38 elements in the new reference material NSP-1. Relative standard deviations for most of the determined elements were below 10%. Combination of ICP-MS and ICP-AES techniques for certification of the new reference material makes it possible to expand the set of elements to be determined and to reduce the total analysis time.

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