Methodological Procedures for As Speciation Essay

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Objectives of the Research Study

This main objective was to look into the methodological procedures for As speciation conducted by an HG-based non-qualitative assessment. It also assessed the distinctness of some toxicologically pertinent As species: MMA, DMA, As (V), and As (III), which reacted differently under different exposures. The results helped in the critical preparation of the various hydrides and assessing the connection between the individual signals of As. From that assessment, it was easy to point out the erroneous interpretation of the final results. Systematic processes for selective determination and discrimination of different species of MMA, DMA, As (III), and As (v) were developed (Welna and Pohl, 2017). This relied on various responses of the main As species toward HG. In the end, a proposal was made for both fractionation and speciation schemes accompanied by the processes for the entire As determination.

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Main Experimental Methods

The study had three main experimental methods. The first one was reagents and solutions, which revealed that all chemicals had a methodological grade. Respective salts of solutions MMA, DMA, and As (III) were analyzed, and standard stock solutions were obtained. The solutions were disodium methyl arsenate (CH3AsNa2O3), sodium cacodylate (C2H6AsNaO2 × 3H2O), and sodium metaarsenite (NaAsO2), all obtained from Sigma-Aldrich. The mentioned mixtures were processed together at once and later kept at a 4 °C temperature (Welna and Pohl, 2017). There were no preservatives added to the species stock solutions. For instance, a Merck ICP standard solution was used for As (v).

The stock standards were serially diluted with water to obtain single and mixed working solutions in all the experiments; artificial sample products of the As species were all set and decompounded. For each of the examined As species, single standard solutions were acidified with various acid media, made in water only, or made with the aid of different pre-conducting agents, and all these were checked correctly.

The second method of the experiment was pre-treating the samples using pre-reducing agents. This was the re-reduction of all the As species. This experiment began with pre-reducing the potassium iodide alone and later with its mixture with amino acid, making potassium iodide and amino acid. The same was also done for TU and its combination with AA, making TU-AA (Welna and Pohl, 2017). For these, the right portions of the pre-reducing solutions’ non-diluted mixtures were put in Polypropylene-capped holders, where the right proportions of the working standards of MMA, DMA, and As (v) were mixed.

The last non-diluted solution of the individual pre-reducing agents was obtained, mixed, and completed with a solution of hydrochloric acid. This was done to attain the needed acidity. It was then allowed to mix well before making the right calculations of hydride generation, which were coupled plasma optical emission spectrometry inductively. It is important to note that the As (III) standard mixture had to be preserved with the selected agents needed for the pre-reduction process. This was done to effectively determine the results of all the agents on As and mercury and get the right As species (Welna and Pohl, 2017). There was also an appropriate blank mixture of the solutions, which were usually organized in the same manner as the main mixture and included in the final and last results.

The third experimental method was obtaining the generation and calculations of the arsenic hydride. From the four main As species, corresponding arsines or arsenic hydrides were obtained. They were then generated through a continuous flow system using an ICP OES spectrometer combined directly with a separation of gas-liquid phase (Welna and Pohl, 2017). The system was made up of an improved cyclonic sprayer, which played a phase separator, Y-shaped connectors, a parallel Burgener-type pneumatic nebulizer, and peristaltic pumps attached to delivery tubes, a reaction oil, and Y-shaped connectors.

The two peristaltic pumps helped simultaneously pump the reagents, an additional acid, sample S, and the NaBH4 (R) solutions in different streams. In the first experiment, solutions A and S were all placed in the initial connector. The obtained acid mixture was taken to the second connector and merged with the next R mixture. The mixture coil brought forward the found heterogeneous reaction solution to a dedicated cavity at the chamber’s bottom and set aside the liquid state’s volatile species. A bearer- Aromatic ring stream brought in through the inlet of the nebulizer’s gas swept arsines and the remaining gaseous co-products and moved them swiftly to the other end (Welna and Pohl, 2017). This clogged the nebulizer’s inlet of the solution. With the third peristaltic pump’s help, the post-reaction solution was later drained into the chamber.

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Major Finding

From the study, selective HG comes out clearly as one of the best ways of creating non-chromatographic methodologies in any arsenic application. It is generally attained by adjusting the HG conditions, including the concentrations and types of acids, the NaBH 4 buffers and concentration, and the pre-adjusting agents’ use (Welna and Pohl, 2017). As (III) and As (v) come out as the easiest and perhaps fastest speciation of the arsenic species, and this can be attained by reacting the mercury of As (III) with 10M of hydrochloric acid. The pre-reduction of As (v) to As (III) and ascorbic acid should also be included.

Procedures based on hydride generation are simpler to execute and cheap than those based on the coupled plasma mass spectrometry but depend on the analytical instrumentation required (Welna and Pohl, 2017). Excellent results can be achieved when the mercury, coupled to optical emission spectrometry, creates one of the best speciation (Welna and Pohl, 2017). The atomic absorption spectrophotometry application of hydride generation is not the best for identifying such non-hydride-forming species as the B species. Five speciation arsenic species-selective HG procedures were evaluated by Welna and Pohl (2017). The five speciations included SP3, SP2, SP1 (As III), SP5, and SP4 (DMA and MMA). This was achieved by comprehensively analyzing reductants and pre-reductants, the acids, buffers.

Conclusion

Determining As by hydride generation, which is inductively coupled plasma optical emission spectrometry in its reaction with sodium borohydride in the acidic medium, is not easy. However, the study proved that four main As species react with sodium borohydride in three different ways. The first one is based on the mixture of the reductant, while the other one is founded upon the type of the pre-reducing agent used in pre-reduction. The basis of the third is on the reaction method applied for the preparation of the As hydrides. The mixture of ICP MS with HPLC is today used as the best method for elements speciation since it offers a whole and advanced picture of the species cleansed from a single sample injection. Therefore, it is quantified at the level of the trace. Even though these research results refer to natural and standard drinking water (the simple sample solutions), they further show the likelihood of properly fractionating and speciating As through chromatographic separation.

References

Welna, M., and Pohl, P. Potential Of The Hydride Generation Technique Coupled To Inductively

Coupled Plasma Optical Emission Spectrometry For Non-Chromatographic As Speciation. J. Anal. At. Spectrom.,2017, 32, 1766.

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IvyPanda. "Methodological Procedures for As Speciation." February 21, 2022. https://ivypanda.com/essays/methodological-procedures-for-as-speciation/.

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