scholarly journals A Comparison of ETV and LA for the Determination of Trace Elements in Solid Samples by MIP OES

2019 ◽  
Vol 26 (3) ◽  
pp. 429-441
Author(s):  
Henryk Matusiewicz ◽  
Mariusz Ślachciński
Keyword(s):  
Trace Elements ◽  
Certified Reference Materials ◽  
Detection Limits ◽  
Optimization Procedure ◽  
Sample Introduction ◽  
Matrix Composition ◽  
Emission Spectrometry ◽  
Solid Samples ◽  
Mip Oes

Abstract The performance of electrothermal vaporization (ETV) and laser ablation (LA) of dry aerosols as sample introduction systems for microwave induced plasma optical emission spectrometry (MIP OES) are compared and evaluated in terms of detection limits, precision and accuracy for the determination of trace elements (Ca, Cd, Cu, Fe, Mg, Mn, Sr, Zn) in the same solid micro samples. In MIP OES both radiation sources can be independently adjusted to optimize the sampling process and then its subsequent excitation. A univariate approach and simplex optimization procedure were used to obtain the best signal/noise (S/N) ratio and derive analytical figures of merit. A comparison using a Student’s t-test between the results obtained by both ETV/LA-MIP OES methods for trace elements, and concentrations in standard reference material (SRM) and certified reference materials (CRMs) showed that there was no significant differences on a 95 % confidence level. The detection limits of the tested elements in solid samples by ETV/LA-MIP OES were in the range of 0.1 to 11 µg g−1 for all elements determined, while the corresponding absolute values in the range of ng. The precision of the results for ETV-MIP OES and LA-MIP OES varied between 2 and 4 % and 3 and 7 %, respectively. The linear dynamic ranges in the ETV/LA-MIP OES are extend over three decades of concentration. The methods were validated by the analysis of NIST SRM 2711Montana Soil, NRCC CRM PACS-2 Marine Sediment and NRCC CRM TORT-2 Lobster Hepatopancreas of different matrix composition and by the standard addition technique.

Determination of non-metallic inclusions in metal alloys by spark atomic emission spectrometry (review)

2018 ◽  
Vol 84 (12) ◽  
pp. 5-19
Author(s):  
D. N. Bock ◽  
V. A. Labusov
Keyword(s):  
Spectral Line ◽  
Internal Standard ◽  
Detection Limits ◽  
Radiation Detectors ◽  
Metal Alloys ◽  
Emission Spectrometry ◽  
Direct Production ◽  
Metallic Inclusions ◽  
Dissolved Form

A review of publications regarding detection of non-metallic inclusions in metal alloys using optical emission spectrometry with single-spark spectrum registration is presented. The main advantage of the method - an extremely short time of measurement (~1 min) – makes it useful for the purposes of direct production control. A spark-induced impact on a non-metallic inclusion results in a sharp increase (flashes) in the intensities of spectral lines of the elements that comprise the inclusion because their content in the metal matrix is usually rather small. The intensity distribution of the spectral line of the element obtained from several thousand of single-spark spectra consists of two parts: i) the Gaussian function corresponding to the content of the element in a dissolved form, and ii) an asymmetric additive in the region of high intensity values ??attributed to inclusions. Their quantitative determination is based on the assumption that the intensity of the spectral line in the single-spark spectrum is proportional to the content of the element in the matter ablated by the spark. Thus, according to the calibration dependence constructed using samples with a certified total element content, it is possible not only to determine the proportions of the dissolved and undissolved element, but also the dimensions of the individual inclusions. However, determination of the sizes is limited to a range of 1 – 20 µm. Moreover, only Al-containing inclusions can be determined quantitatively nowadays. Difficulties occur both with elements hardly dissolved in steels (O, Ca, Mg, S), and with the elements which exhibit rather high content in the dissolved form (Si, Mn). It is also still impossible to determine carbides and nitrides in steels using C and N lines. The use of time-resolved spectrometry can reduce the detection limits for inclusions containing Si and, possibly, Mn. The use of the internal standard in determination of the inclusions can also lower the detection limits, but may distort the results. Substitution of photomultipliers by solid-state linear radiation detectors provided development of more reliable internal standard, based on the background value in the vicinity of the spectral line. Verification of the results is difficult in the lack of standard samples of composition of the inclusions. Future studies can expand the range of inclusions to be determined by this method.

Cross Double Point Discharge as Enhanced Excitation Source for Highly Sensitive Determination of Arsenic, Mercury and Lead by Optical Emission Spectrometry

2021 ◽  
Author(s):  
Lin He ◽  
Peixia Li ◽  
Kai Li ◽  
Tao Lin ◽  
Jin Luo ◽  
...  
Keyword(s):  
Double Point ◽  
Hydride Generation ◽  
Optical Emission ◽  
Sample Introduction ◽  
Excitation Source ◽  
Emission Spectrometry ◽  
Highly Sensitive ◽  
Point Discharge ◽  
Sensitive Determination

A new cross double point discharge (CrossPD) microplasma was designed as an excitation source to construct a miniaturized optical emission spectrometer with hydride generation (HG) for sample introduction. The CrossPD...

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