Development of ICP-AES-based Methodology for the Determination of Trace Metallic Constituents in Zr-Nb Alloy

Pathak, Sunita; Sengupta, Arijit

doi:10.46770/as.2017.06.002

Cited by 9 publications

(8 citation statements)

References 24 publications

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“…This identification of lines must be based on the analytical performances as well as interference free. Since, Zr is multi‐electronic system, it is expected to interfere during determination of analytes at trace level specially in atomic emission spectrometry [42,46,47] . The detection limit was calculated based on the concentration relates to the intensity which is equivalent to the average value of 11 replicate measurements plus three times of the standard deviation for the measurements.…”

Section: Resultsmentioning

confidence: 99%

“…In a similar fashion, same exercise was carried out for D.C.Arc carrier distillation OES methods. Based on our earlier investigation on the spectral interference of Zr on different analytes based on CCD based inductively coupled plasma atomic emission spectrometry, the least interfered analytical lines for the elements were chosen [38,42,43] . Table 2 summarizes the results.…”

Section: Resultsmentioning

confidence: 99%

“…Since, Zr is multi-electronic system, it is expected to interfere during determination of analytes at trace level specially in atomic emission spectrometry. [42,46,47] The detection limit was calculated based on the concentration relates to the intensity which is equivalent to the average value of 11 replicate measurements plus three times of the standard deviation for the measurements. The sensitivity was calculated based on the slopes of the calibration curves, which corresponds to the intensity of the unit concentration of the analytes.…”

Section: Optimization Of Methodologiesmentioning

confidence: 99%

“…Based on our earlier investigation on the spectral interference of Zr on different analytes based on CCD based inductively coupled plasma atomic emission spectrometry, the least interfered analytical lines for the elements were chosen. [38,42,43] . However, in this high energy zone, the atmosphere also starts getting excited resulting subsequent emission lines, which highly interfere the determination of the non-metals like S, I etc.…”

Section: Optimization Of Methodologiesmentioning

confidence: 99%

“…D.C.Arc carrier distillation technique was used for atomic emission spectrometry, where based on the volatilization, the minor and trace analytes would sweep away to the excitation source D.C.Arc by leaving refractory elements like Zr, Si into the electrode in major amount physically. This physical way of separation helps in avoiding spectral interference of the major elements on analytes for their trace level determination.ICP-OES requires chemical separation of major matrices, which not only is time consuming but requires selective ligand system to serve the purpose, [42][43][44][45] while suitable carrier can cater the need by means of physical separation. [46][47][48][49] AgCl being extensively used as carrier for Zr matrix and hence was adopted in present investigation.…”

Section: Introductionmentioning

confidence: 99%

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Development of Methodologies for the Chemical Quality Control of Zircon, A Precursor for Zirconium Production

Jayabun

Sengupta

2021

ChemistrySelect

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Methodologies have been developed for the chemical quality control of zircon mineral by EDXRF and D.C.Arc carrier distillation technique. EDXRF technique was found to be preferred for major and minor constituents including non‐metal analytes, while D.C.Arc carrier distillation OES was found to be good for minor and trace metallic constituents including low Z elements. A comparative evaluation of the analytical performance (detection limit, sensitivity, precision, linear dynamic range) was performed. A multipoint standardization was carried out using the base material of 1 : 1 SiO2 : ZrO2 powder mixture to establish calibration curves for the analytes after identification of interference free and the best performed emission and X‐ray analytical lines. In zircon sample, Si, Zr and Y were found to be present as major constituent, with Ga, Ca, Ru, Rh, Fe, Mn, Mg, I, S as minor and Zn, Cr, Sn, Li as trace constituents. The total uncertainty of the EDXRF measurements was evaluated. The statistical t‐test analysis was carried out for 10 degrees of freedom with 95 % confidence interval. The experimentally obtained t‐values were found to be lower compared to the corresponding tcri value revealing the reliability of the measurements. Elemental distributions of the analytes were also investigated using five different zircon samples.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Optimization Of Methodologiesmentioning

confidence: 99%

Section: Optimization Of Methodologiesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Development of Methodologies for the Chemical Quality Control of Zircon, A Precursor for Zirconium Production

Jayabun

Sengupta

2021

ChemistrySelect

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A Comprehensive Investigation alongwith the Statistical Evaluation for the Characterization of Ilmenite Mineral by X‐ray Fluorescence Spectrometry and Optical Emission Spectrometry

2021

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A comparative investigation on characterization of ilmenite manuscript was performed by energy dispersive X‐ray fluorescence spectrometry (EDXRF) and carrier distillation direct current arc atomic emission spectrometry (D.C. Arc AES) along with the statistical evaluation of the data obtained. 5 % AgCl was used as carrier in AES to avoid spectral interference arising out of the emission rich matrix elements. An exercise was performed to evaluate the total uncertainty associated with the methodology for characterization of base reference materials. The developed methodologies were validated using synthetic samples. ∼30 % Fe and ∼35 % Ti as major elements alongwith Ca, Mg, Cr, Si, Al, Ni, Mn, V, Zr, Eu, Mo, Na and Cd as minor and trace level were reported in real ilmenite samples. Student t test was performed at 95 % confidence limit with 10 degrees of freedom revealed that the null hypothesis persisted, i. e. the data obtained by both the methods are reliable and within the limit of statistical fluctuation. The F test on variance revealed that all the variance estimated for all the analytes were less than the critical value (Fc=2.98) and hence the variance is also within the statistical fluctuation

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Development of ICP‐OES Based Analytical Method with Prior Preferential Removal of Emission Rich Matrix by Elevated Temperature Ionic Liquid Based Extractive Mass Transfer for Determination of Metallic Constituents in U‐Mo Alloy: The Next Generation Nuclear Fuel

et al. 2022

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An (ICP‐OES) based analytical methodology was developed for the determination of metallic constituents (Al, Ca, Co, Cr, Cu, Fe, Ga, In, Mn, Mg, Na, Ni, Si, V, W and Zn) at minor and trace level in U−Mo alloy fuel after preferential separation of emission rich major matrix using TBP‐HDBO‐NTf2 without any compromise on the determination of analytes at trace levels. Application of ionic liquid, HDBO‐NTf2 drastically reduced the time of analysis (30 min reduction per sample) and generation of toxic organic waste (20 mL per sample) containing U and Mo. The method was optimized by identification of analytical lines of the elements free from spectral interference of U and Mo, establishing the calibration curves using those lines and evaluation of analytical performances (detection limit, linear dynamic range etc.) in U−Mo matrix. The preferential separation of U and Mo were found to follow anion exchange and cation exchange mechanism involving UO2((NO)3)3.2TBP− and MoO2(NO3) TBP+ species, respectively, which differ in their conventional separation by solvation mechanism involving ML2 and ML1 neutral species, respectively. Preferential separation by HDBO‐NTf2 based system can be effectively used for determination of analytes of 10 ppm concentration at 10 % error limit. The total uncertainty in estimation of each analyte have been estimated. The real sample analyses data were compared to that obtained by n‐dodecane based ICP‐OES method and direct analysis of Energy Dispersive X‐ray Fluorescence spectroscopic (EDXRF) method. The data were found to be in good agreement with each other. The experimentally obtained results were subjected to t‐test with 95 % confidence limit and 10 degrees of freedom. The texpt was found to be less than tcrit 2.228 revealing reliability of the methods. The experimentally obtained variance values (Fexpt) were found to be less than Fcrit∼2.980 revealing the variance values are within acceptable statistical error limit.

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Development of ICP-AES-based Methodology for the Determination of Trace Metallic Constituents in Zr-Nb Alloy

Cited by 9 publications

References 24 publications

Development of Methodologies for the Chemical Quality Control of Zircon, A Precursor for Zirconium Production

Development of Methodologies for the Chemical Quality Control of Zircon, A Precursor for Zirconium Production

A Comprehensive Investigation alongwith the Statistical Evaluation for the Characterization of Ilmenite Mineral by X‐ray Fluorescence Spectrometry and Optical Emission Spectrometry

Development of ICP‐OES Based Analytical Method with Prior Preferential Removal of Emission Rich Matrix by Elevated Temperature Ionic Liquid Based Extractive Mass Transfer for Determination of Metallic Constituents in U‐Mo Alloy: The Next Generation Nuclear Fuel

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