Determination of residual chloride content in ionic liquids using LA-ICP-MS

Bonta, Maximilian; Anderl, Thomas; Cognigni, Alice; Hejazifar, Mahtab; Bica, Katharina; Limbeck, Andreas

doi:10.1039/c6ra21203d

Cited by 3 publications

(4 citation statements)

References 30 publications

(32 reference statements)

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Section: Introductionmentioning

confidence: 99%

“…Additionally, the stoichiometric formation of an alkali salt, for example, LiCl, as a byproduct is yet another issue in the light of sustainability as exhaustive extractive work-up is required to suppress the residual halide content to a minimum. 16 These problems with ion metathesis and residual metal and/ or halide content can be circumvented in the synthetic route that relies on dimethyl carbonate as a cheap methylating agent. 17 The method is based on the formation of a methyl carbonate intermediate which is further reacted with equimolar amounts of acid to form the IL upon release of CO 2 and methanol.…”

Section: ■ Introductionmentioning

confidence: 99%

“…Similarly, the anion metathesis step is problematic due to the onerous removal of metal and halide residues that decidedly influence the physical and chemical behavior of the ILs. Additionally, the stoichiometric formation of an alkali salt, for example, LiCl, as a byproduct is yet another issue in the light of sustainability as exhaustive extractive work-up is required to suppress the residual halide content to a minimum …”

Section: Introductionmentioning

confidence: 99%

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Halide-Free Continuous Synthesis of Hydrophobic Ionic Liquids

Stagel

Szpecht

Zielinski

et al. 2022

ACS Sustainable Chem. Eng.

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Herein, we present a novel approach for the halide-free, continuous-flow preparation of hydrophobic ionic liquids (ILs) relying on the bis(trifluoromethanesulfonyl)imide (bistriflimide, NTf 2 – ) anion. The simple yet fast two-step synthetic route, which involves the formation of different alkyl bistriflimides (R 4 NTf 2 ), followed by the quaternization with an amine nucleophile, led to the desired ILs in high yields and excellent purities without any byproduct formation. The variable alkyl chain (R 4 ) length and the broad range of the applicable nucleophiles (R 1 R 2 R 3 N) offer considerable flexibility to the synthetic protocol. The quaternization can be performed under solvent-free conditions; moreover, the homogeneous nature of these reactions allows the application of modern continuous-flow technologies. Given these advantages, the methodology can afford not just a fast and efficient alternative for the conventional synthesis of such compounds with reduced waste water production but their negligible halide content might provide a significantly broader application range of the IL products, especially for the field of materials science.

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Section: Introductionmentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Halide-Free Continuous Synthesis of Hydrophobic Ionic Liquids

Stagel

Szpecht

Zielinski

et al. 2022

ACS Sustainable Chem. Eng.

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“…However, the technique is sensitive to various sample preparation parameters such as the sample amount and drying time and is therefore more prone to human errors . Other reported techniques include capillary electrophoresis (CE), (laser ablation) inductively coupled plasma mass spectrometry ((LA-)ICP-MS), , and electrochemical methods . Most of these are characterized by either long analysis times or time-consuming sample preparations, calibrations, and method developments.…”

Section: Introductionmentioning

confidence: 99%

Determination of Chlorides in Ionic Liquids by Wavelength Dispersive X-ray Fluorescence Spectrometry

et al. 2021

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The synthesis of ionic liquids (ILs) usually involves two steps: (i) quaternization of a precursor followed by (ii) a salt metathesis reaction to introduce the desired anion. A consequence of the second step is that most ILs still contain some amount of the initial anion, often chloride. In this work, wavelength dispersive X-ray fluorescence (WDXRF) spectrometry is presented for the direct measurement of chlorides in ILs. The WDXRF settings were optimized, and the system was calibrated for the detection of chloride in several analogues of the commercially available IL Aliquat 336, [A336][X] (with X = I–, Br–, NO3 –, or SCN–). The Cl Kα intensity showed excellent linearity for samples with a conversion >0.80 (approximately Cl < 8000 ppm). Synthetic quality control samples showed that the instrumental error and deviations induced by the calibration procedure were small with maximum values of 1 and 5%, respectively. Detection and quantification limits depended strongly on the matrix (i.e., anion system and dilution) but were relatively low: 42–191 and 127–578 ppm Cl, respectively. Compared with other analytical techniques used for this purpose, the strengths of WDXRF include its ease of use, rapid measurements, the near absence of sample preparation steps, and versatility in terms of anion systems and chloride concentration range.

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