environmental chemistry research papers pdf

2019 Best Papers published in the Environmental Science journals of the Royal Society of Chemistry

In 2019, the Royal Society of Chemistry published 180, 196 and 293 papers in Environmental Science: Processes & Impacts , Environmental Science: Water Research & Technology , and Environmental Science: Nano , respectively. These papers covered a wide range of topics in environmental science, from biogeochemical cycling to water reuse to nanomaterial toxicity. And, yes, we also published papers on the topic of the environmental fate, behavior, and inactivation of viruses. 1–10 We are extremely grateful that so many authors have chosen our journals as outlets for publishing their research and are equally delighted at the high quality of the papers that we have had the privilege to publish.

Our Associate Editors, Editorial Boards, and Advisory Boards were enlisted to nominate and select the best papers from 2019. From this list, the three Editors-in-Chief selected an overall best paper from the entire Environmental Science portfolio. It is our pleasure to present the winners of the Best Papers in 2019 to you, our readers.

Overall Best Paper

In this paper, Johansson et al. examine sea spray aerosol as a potential transport vehicle for perfluoroalkyl carboxylic and sulfonic acids. The surfactant properties of these compounds are well known and, in fact, key to many of the technical applications for which they are used. The fact that these compounds are enriched at the air–water interface makes enrichment in sea spray aerosols seem reasonable. Johansson et al. systematically tested various perfluoroalkyl acids enrichment in aerosols under conditions relevant to sea spray formation, finding that longer chain lengths lead to higher aerosol enrichment factors. They augmented their experimental work with a global model, which further bolstered the conclusion that global transport of perfluoroalkyl acids by sea spray aerosol is and will continue to be an important process in determining the global distribution of these compounds.

Journal Best Papers

Environmental Science: Processes & Impacts

First Runner-up Best Paper: Yamakawa, Takami, Takeda, Kato, Kajii, Emerging investigator series: investigation of mercury emission sources using Hg isotopic compositions of atmospheric mercury at the Cape Hedo Atmosphere and Aerosol Monitoring Station (CHAAMS), Japan , Environ. Sci.: Processes Impacts , 2019, 21 , 809–818, DOI: 10.1039/C8EM00590G .

Second Runner-up Best Paper: Avery, Waring, DeCarlo, Seasonal variation in aerosol composition and concentration upon transport from the outdoor to indoor environment , Environ. Sci.: Processes Impacts , 2019, 21 , 528–547, DOI: 10.1039/C8EM00471D .

Best Review Article: Cousins, Ng, Wang, Scheringer, Why is high persistence alone a major cause of concern? Environ. Sci.: Processes Impacts , 2019, 21 , 781–792, DOI: 10.1039/C8EM00515J .

Environmental Science: Water Research & Technology

First Runner-up Best Paper: Yang, Lin, Tse, Dong, Yu, Hoffmann, Membrane-separated electrochemical latrine wastewater treatment , Environ. Sci.: Water Res. Technol. , 2019, 5 , 51–59, DOI: 10.1039/C8EW00698A .

Second Runner-up Best Paper: Genter, Marks, Clair-Caliot, Mugume, Johnston, Bain, Julian, Evaluation of the novel substrate RUG™ for the detection of Escherichia coli in water from temperate (Zurich, Switzerland) and tropical (Bushenyi, Uganda) field sites , Environ. Sci.: Water Res. Technol. , 2019, 5 , 1082–1091, DOI: 10.1039/C9EW00138G .

Best Review Article: Okoffo, O’Brien, O’Brien, Tscharke, Thomas, Wastewater treatment plants as a source of plastics in the environment: a review of occurrence, methods for identification, quantification and fate , Environ. Sci.: Water Res. Technol. , 2019, 5 , 1908–1931, DOI: 10.1039/C9EW00428A .

Environmental Science: Nano

First Runner-up Best Paper: Janković, Plata, Engineered nanomaterials in the context of global element cycles , Environ. Sci.: Nano , 2019, 6 , 2697–2711, DOI: 10.1039/C9EN00322C .

Second Runner-up Best Paper: González-Pleiter, Tamayo-Belda, Pulido-Reyes, Amariei, Leganés, Rosal, Fernández-Piñas, Secondary nanoplastics released from a biodegradable microplastic severely impact freshwater environments , Environ. Sci.: Nano , 2019, 6 , 1382–1392, DOI: 10.1039/C8EN01427B .

Best Review Article: Lv, Christie, Zhang, Uptake, translocation, and transformation of metal-based nanoparticles in plants: recent advances and methodological challenges , Environ. Sci.: Nano , 2019, 6 , 41–59, DOI: 10.1039/C8EN00645H .

Congratulations to the authors of these papers and a hearty thanks to all of our authors. As one can clearly see from the papers listed above, environmental science is a global effort and we are thrilled to have contributions from around the world. In these challenging times, we are proud to publish research that is not only great science, but also relevant to the health of the environment and the public. Finally, we also wish to extend our thanks to our community of editors, reviewers, and readers. We look forward to another outstanding year of Environmental Science , reading the work generated not just from our offices at home, but also from back in our laboratories and the field.

Kris McNeill, Editor-in-Chief

Paige Novak, Editor-in-Chief

Peter Vikesland, Editor-in-Chief

• A. B Boehm, Risk-based water quality thresholds for coliphages in surface waters: effect of temperature and contamination aging, Environ. Sci.: Processes Impacts , 2019, 21 , 2031–2041,   10.1039/C9EM00376B .
• L. Cai, C. Liu, G. Fan, C Liu and X. Sun, Preventing viral disease by ZnONPs through directly deactivating TMV and activating plant immunity in Nicotiana benthamiana , Environ. Sci.: Nano , 2019, 6 , 3653–3669,   10.1039/C9EN00850K .
• L. W. Gassie, J. D. Englehardt, N. E. Brinkman, J. Garland and M. K. Perera, Ozone-UV net-zero water wash station for remote emergency response healthcare units: design, operation, and results, Environ. Sci.: Water Res. Technol. , 2019, 5 , 1971–1984,   10.1039/C9EW00126C .
• L. M. Hornstra, T. Rodrigues da Silva, B. Blankert, L. Heijnen, E. Beerendonk, E. R. Cornelissen and G. Medema, Monitoring the integrity of reverse osmosis membranes using novel indigenous freshwater viruses and bacteriophages, Environ. Sci.: Water Res. Technol. , 2019, 5 , 1535–1544,   10.1039/C9EW00318E .
• A. H. Hassaballah, J. Nyitrai, C. H. Hart, N. Dai and L. M. Sassoubre, A pilot-scale study of peracetic acid and ultraviolet light for wastewater disinfection, Environ. Sci.: Water Res. Technol. , 2019, 5 , 1453–1463,   10.1039/C9EW00341J .
• W. Khan, J.-Y. Nam, H. Woo, H. Ryu, S. Kim, S. K. Maeng and H.-C. Kim, A proof of concept study for wastewater reuse using bioelectrochemical processes combined with complementary post-treatment technologies, Environ. Sci.: Water Res. Technol. , 2019, 5 , 1489–1498,   10.1039/C9EW00358D .
• J. Heffron, B. McDermid and B. K. Mayer, Bacteriophage inactivation as a function of ferrous iron oxidation, Environ. Sci.: Water Res. Technol. , 2019, 5 , 1309–1317,   10.1039/C9EW00190E .
• S. Torii, T. Hashimoto, A. T. Do, H. Furumai and H. Katayama, Impact of repeated pressurization on virus removal by reverse osmosis membranes for household water treatment, Environ. Sci.: Water Res. Technol. , 2019, 5 , 910–919,   10.1039/C8EW00944A .
• J. Miao, H.-J. Jiang, Z.-W. Yang, D.-y. Shi, D. Yang, Z.-Q. Shen, J. Yin, Z.-G. Qiu, H.-R. Wang, J.-W. Li and M. Jin, Assessment of an electropositive granule media filter for concentrating viruses from large volumes of coastal water, Environ. Sci.: Water Res. Technol. , 2019, 5 , 325–333,   10.1039/C8EW00699G .
• K. L. Nelson, A. B. Boehm, R. J. Davies-Colley, M. C. Dodd, T. Kohn, K. G. Linden, Y. Liu, P. A. Maraccini, K. McNeill, W. A. Mitch, T. H. Nguyen, K. M. Parker, R. A. Rodriguez, L. M. Sassoubre, A. I. Silverman, K. R. Wigginton and R. G. Zepp, Sunlight mediated inactivation of health relevant microorganisms in water: a review of mechanisms and modeling approaches, Environ. Sci.: Processes Impacts , 2018, 20 , 1089–1122,   10.1039/C8EM00047F .

Environmental Chemistry Letters

Environmental Chemistry Letters covers the interfaces of geology, chemistry, physics and biology. Articles published here are of high importance to the study of natural and engineered environments.

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Environmental Chemistry

Environmental Chemistry publishes papers reporting chemistry that enhances our understanding of the natural and engineered environment (including indoor and outdoor air, water, soil, sediments, and biota). Read more about the journal

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Just Accepted

Collections, these articles are the latest published in the journal. environmental chemistry has moved to a continuous publication model. more information is available on our continuous publication page ., en24011 quantification of palladium-labelled nanoplastics algal uptake by single cell and single particle inductively coupled plasma mass spectrometry.

Environmental context.  Plastic pollution is widespread and continues to be a major concern, both for the environment and human health. Identifying nanoplastics is challenging but it is important to understand how they behave once in the environment. It is shown that a combination of single particle (SP)– and single cell (SC)–inductively coupled plasma–mass spectrometry (ICP-MS) can be used to quantify nanoplastics on a per cell basis after exposure to algal cells. (Image credit: E. C. Bair.)

EN23111 Testing of the bioremediation on model substrates for complex refinery contaminants arising from accidental or deliberate facility damage

Environmental context.  Mitigating the environmental fallout of industrial accidents is crucial. In a recent study, researchers conducted tests on model substrates to explore the effectiveness of bioremediation in treating complex refinery contaminants resulting from both accidental and deliberate facility damage. The research reveals that bioremediation can be a promising, eco-friendly solution for cleaning up such pollutants, aligning with broader efforts to combat environmental harm resulting from industrial incidents.

EN24021 A critical assessment of physicochemical indices used to characterise natural dissolved organic carbon (DOC), their inter-relationships, and the effects of pH

Environmental context.  Dissolved organic carbon (DOC) is ubiquitous in freshwater and concentrations are rising universally while pH is decreasing with climate change. This study demonstrates the interrelationships among DOC characterisation techniques and the pH-sensitive aspects of these techniques that were previously not well understood. As DOC regulates important processes within ecosystems, understanding DOC behaviour at altered pH and identifying techniques to effectively evaluate DOC composition are critical requirements for monitoring aquatic ecosystem health. (Image credit: Carolyn Morris.)

EN24024 A comprehensive analysis of water-soluble arsenicals in Icelandic macroalgae

Environmental context.  Seaweeds are known to accumulate high levels of arsenic, and cellular concentrations may reach several orders of magnitude higher than that of the surrounding environment. Arsenic may be methylated by seaweed cells and further metabolised to water-soluble arsenic-containing sugars through unknown pathways. Whether these compounds are the result of a detoxification process or are produced with a biological purpose remains to be seen. (Image credit: Rebecca Sim.)

EN23105 Developing a modern approach to assess ecological risk from pesticides without unnecessary vertebrate animal testing

Environmental context.  Pesticides are critical to agriculture and food production but require ecological risk assessments. Although most risk assessments require data from vertebrate animal testing, we have developed an approach to assess risk to fish, birds and mammals using other means. This approach could help to ensure protection of the environment while minimising animal testing.

This article belongs to the collection NAMs in Environmental Chemistry and Toxicology.

EN23117 Potential for atmospheric acid processing of mineral dust to supply bioavailable trace metals to the oceans

Environmental context.  Mineral dust is an important external source of trace metals to the offshore ocean. Dust exposure to acids is a significant driver of the release of dissolved trace elements. This study provides an analysis of mineral dust interaction with acid, as a proxy for atmospheric processes. An insight is given into the processes that may occur in the atmosphere where desert dust may add nutrient or toxic metals to oceans.

This article belongs to the collection Dedication to Prof. Edward Tipping.

EN23117 Abstract  |  EN23117 Full Text  |  EN23117 PDF (1.3 MB)

EN23106 Characteristics, potential sources and interaction of carbonaceous components in PM 2.5 in two adjacent areas in Shanxi, China

Environmental context.  Carbonaceous components in PM 2.5 have a negative effect on the environment, human health and climate. We explored the pollution characteristic, potential sources and interaction of carbonous aerosols in two adjacent areas in Shanxi, China. The concentration levels of organic carbon and elemental carbon were of a moderate level of all those measured between 2009 and 2020. Vehicle exhaust and coal combustion were the two main sources, and Yuci may be affected by the regional transport of Taiyuan in winter.

EN23108 Size evolution of Eu III –fulvic acid complexes with pH, metal, and fulvic acid concentrations: implications for modelling of metal–humic substances interactions

Environmental context.  This study investigates how rare earth elements (REEs), such as europium (Eu), bind to organic matter. We are also gaining valuable insights into how these elements affect the structure of the organic matter that controls their mobility in natural systems, helping us to better understand the broader processes that govern the behaviour of trace metals in the environment.

EN23116 Distribution, speciation, mobility and ecological risk of potentially toxic elements in dust and PM 2.5 from abandoned mining areas

Environmental context.  Dust is a heterogeneous material deposited on the ground surface and is a source and sink for potentially toxic elements (PTEs) originating from the air and soil. Tracking the distribution and effects of PTEs in an abandoned mining area is critical as few studies have quantified the speciation and bioavailability of PTEs contained in dust and PM 2.5 . In this paper, we track the distribution of PTEs in an abandoned mining area, quantifying the mobility of PTEs using the speciation of PTEs in dust and PM 2.5 and quantitatively assess the environmental and ecological risks of PTE in a mining area.

EN23093 Natural cobalt–manganese oxide nanoparticles: speciation, detection and implications for cobalt cycling

Environmental context.   Cobalt is a technologically critical element due to its uses in the green energy transition, but its cycling is poorly constrained in surface environments. We determined the form of cobalt in naturally enriched soils and found that it is commonly associated with manganese as mixed oxide nanoparticles. These findings demonstrate that the behaviour of critical elements such as cobalt in the environment is in part governed at the nanoscale. (Photograph by O. P. Missen, 11 July 2022.)

EN23093 Abstract  |  EN23093 Full Text  |  EN23093 PDF (4.2 MB)  |  EN23093 Supplementary Material (233 KB)   Open Access Article

EN23114 Effects of arsenite and dimethylarsenic on the growth and health of hydroponically grown commercial Doongara rice

Environmental context.  Arsenic’s effect on rice plant health is a critical environmental issue. This study reveals that rice plants absorb inorganic arsenic and dimethylarsenic differently, with dimethylarsenic posing a greater threat to rice plant health. These findings contribute to our understanding of arsenic toxicity in plants, highlighting the need for further research into detoxification strategies for dimethylarsenic.

EN23114 Abstract  |  EN23114 Full Text  |  EN23114 PDF (1.6 MB)   Open Access Article

More content

These articles have been peer reviewed and accepted for publication. They are still in production and have not been edited, so may differ from the final published form.

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Photolysis characteristics and influencing factors of pesticide pyrimethanil in natural waters

Quantification of Palladium-labeled Nanoplastics Algal Uptake by Single Cell and Single Particle Inductively Coupled Plasma Mass Spectrometry

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Environmental chemistry and ecotoxicology: in greater demand than ever

• Martin Scheringer 1 , 2  

Environmental Sciences Europe volume  29 , Article number:  3 ( 2017 ) Cite this article

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Environmental chemistry and ecotoxicology have been losing support, resources, and recognition at universities for many years. What are the possible causes of this process? A first problem may be that the need for research and teaching in environmental chemistry and ecotoxicology is no longer seen because chemical pollution problems are considered as largely solved. Second, environmental chemistry and ecotoxicology may be seen as fields dominated by routine work and where there are not many interesting research questions left. A third part of the problem may be that other environmental impacts such as climate change are given higher priority than chemical pollution problems. Here, several cases are presented that illustrate the great demand for innovative research and teaching in environmental chemistry and ecotoxicology. It is crucial that environmental chemistry and ecotoxicology are rooted in academic science and are provided with sufficient equipment, resources, and prospects for development.

Environmental chemistry and ecotoxicology under pressure

The publication of Silent Spring in 1962 [ 1 ] made the problem of chemical pollution broadly visible and initiated a political and scientific development that has shaped environmental chemistry and ecotoxicology as we know them. Since 1962, a lot of progress has been made, many important insights have been gained, and new methods have been developed. The objective of this paper is not to provide a critical review of the development over the last decades, but to analyze the current situation, the standing of environmental chemistry and ecotoxicology in the academic system with a focus on Germany and Switzerland. The result from this analysis is that the relevance and reputation of environmental chemistry and ecotoxicology in the academic system have been decreasing for years and also today, in 2016, the prospects are not good.

It is not for the first time that this concern is raised. In 2008, A. Schäffer, M. Roß-Nickoll, H.T. Ratte, and H. Hollert, all at RWTH Aachen, initiated UFOH, an association of university institutes active in environmental research and teaching. The goal of UFOH was to analyze both the status quo of chemical-related environmental research at universities and the prospects for its future development. In 2009, the members of this group stated [ 2 ]:

“Although qualified young environmental scientists are in great demand by industry and authorities, the number of university chairs in this field is steadily and disproportionately declining. Also, the financial support for research projects has been significantly shortened, unlike in other research areas, such as biotechnology or nanotechnology. (…) We are more than concerned that, in the future, both research and education will severely suffer with the ongoing budget reductions in environmental sciences at universities.”

Since then, this trend has been exacerbated. Recent examples from Switzerland include the following: after many years of successful and important work in the field of environmental organic trace analysis, the analytical chemistry group at EMPA has been reshaped and given a different focus; at the Department of Chemistry and Applied Biosciences of ETH Zurich, the Safety & Environmental Technology Group, where I have worked for 20 years, will be closed down in 2018 without a continuation; and, in 2015, the Swiss Society for Food Chemistry and Environmental Chemistry dropped the “Environmental” from its name and is now called Swiss Society for Food Chemistry [ 3 ].

Discussions with journalists and science writers seem to echo the lack of interest in chemicals, environment, and health. “Chemicals” as a topic is seen as too abstract and unwieldy; in science writing for newspapers and magazines, chemicals are frequently presented as an—important—element of other topics such as climate change or bee decline, but it is not often that chemicals as such are the main topic of a report.

Among industry, government authorities, and universities, industry appears to retain the importance of environmental chemistry and ecotoxicology. Obviously, this is because there is an immediate need for well-trained scientific and technical experts who work on the characterization and assessment of chemicals as an essential contribution to the registration of chemical products. In government authorities, the situation is mixed. In chemical-related units, the importance of environmental chemistry and ecotoxicology is fully acknowledged, but in other units, chemical-related work is often seen as a routine process in a highly regulated and clearly structured field without any open questions. In the universities, the situation is most difficult because here environmental chemistry and ecotoxicology are often seen as rather traditional or even outdated fields and priority is given to other, apparently more innovative, and more timely topics.

What are the root causes of the reservations, skepticism, and lack of support that environmental chemistry and ecotoxicology meet within universities? Three possible explanations are as follows:

environmental chemistry and ecotoxicology are no longer needed because chemical-related problems have been solved to a large extent (“no need”);

environmental chemistry and ecotoxicology are no longer vital and productive as academic subjects because they do not offer any interesting and novel research questions (“boring”); and

environmental chemistry and ecotoxicology may be relevant and interesting, but other environmental problems such as climate change are more pressing and need to be given priority.

Why environmental chemistry and ecotoxicology are in great demand

The examples presented below are two cases related to my own field of research, but there are many more cases that could be used to demonstrate the high demand for research and higher education in environmental chemistry and ecotoxicology.

Example 1: polychlorinated biphenyls (PCBs)

The case of PCBs is particularly important and revealing because it concerns a subject that may be considered boring and outdated because so much research has been done on PCBs in the last decades. PCBs became a paradigmatic case of environmental contaminants when the paper by Jensen et al. [ 4 ], “DDT and PCB in marine animals from Swedish waters”, was published in Nature . But have the problems related to PCBs been solved? In 2016, almost 50 years later, Jepson and Law [ 5 ], in a paper in Science , call for more research into PCBs:

“In East Greenland polar bears, blubber PCBs increased unexpectedly between 2010 and 2013, resulting in PCB concentrations that were as high in 2013 as in 1983. (…) Future research should investigate pathways of PCB contamination of the marine environment.”

The problems caused by PCBs have not yet been solved. Surprisingly, even today, substantial PCB emissions take place [ 6 ], and, at the same time, it is not sufficiently clear what the sources of these emissions are. Government authorities assumed for more than 20 years that there were no relevant PCB emissions left after new production of PCBs had been banned in the 1980s in many countries, but this was not true. However, it took several years before our group at ETH Zurich was able to obtain funding for compiling an updated and more comprehensive PCB emission inventory for Switzerland (this project is currently ongoing).

Beyond the case of PCBs, the lesson learned from this example is that using highly persistent chemicals in numerous applications and products implies that research in environmental chemistry and ecotoxicology will be necessary for many decades. Importantly, also under REACH, many highly persistent chemicals have been registered and will be on the market for many years to come.

Example 2: Incremental substitution and chemical property data under REACH

Under REACH, the European Chemicals Agency, ECHA, hosts a database that contains the various types of data submitted with the chemicals’ registration dossiers. The list of chemicals registered up to now and the chemical property data of these chemicals as they are presented in the ECHA database [ 7 ] highlight two problems that define important research needs for environmental chemistry and ecotoxicology:

The chemicals registered under REACH include many former “existing chemicals” that are structurally (very) similar to acknowledged POPs (persistent organic pollutants) or PBT chemicals (chemicals that are persistent, bioaccumulative, toxic). Accordingly, these “emerging chemicals” share hazardous properties such as high persistence and bioaccumulation potential with the structurally related POPs and PBT chemicals. Examples are brominated aromatic substances placed on the market as replacements of polybrominated diphenyl ethers (PBDEs used as flame retardants; one replacement is decabromodiphenyl ethane, see below) and a large group of poly- and perfluorinated alkyl substances (PFASs) placed on the market as replacements of the so-called long-chain PFASs such as PFOA or PFOS that were used, among others, in impregnating agents. These are cases of incremental substitution or regrettable substitution . Environmental chemists and ecotoxicologists need to use their extensive knowledge on legacy POPs and PBT substances in order to demonstrate, as quickly as possible, the environmental and health hazards associated with these “new” chemical products. Otherwise, the problems associated with the hazardous chemicals that have been banned (here: PBDEs, long-chain PFASs) will occur again and will then be perpetuated for many years and decades [ 8 ].

An unknown, but probably high number of these former existing chemicals that are placed on the market now as replacements of hazardous substances are still very poorly characterized. This is obvious from the data contained in the ECHA database, and the database suffers from a serious problem of insufficient data quality. A striking example is the brominated flame retardant DBDPE (CAS no. 84852-53-9), which has been registered with a very high volume of 10,000–100,000 t/year. For the octanol–water partition coefficient (log K ow ) of this substance, the database shows a value of log K ow  = 3.55, which is too low by several log units, which is caused by a measurement error. The actual log K ow of DBDPE is on the order of log K ow  = 11 [ 9 ]. This is an extreme case, but there are many more substances in the database for which erroneous data have been submitted in the registration dossiers. A systematic chemical and toxicological assessment of these data is urgently needed, but the methods and procedures for that are not yet in place. This complex evaluation of a vast amount of data requires substantial experience in physical chemistry, environmental chemistry, toxicology, and ecotoxicology.

Conclusions on the demand for environmental chemistry and ecotoxicology

There is a serious misconception that needs to be rectified, namely that a problem has been solved as soon as it is covered by legislation. A regulation entering into force, such as REACH or the Water Framework Directive or the Stockholm Convention on POPs, does not indicate that the job has been done and that no more work will be needed. On the contrary, it marks the beginning of a period of increased demand for work: when a regulation is in place, this implies an obligation to establish the empirical basis that will make it possible to effectively implement and enforce the regulation. This means that empirical findings and data need to be generated, in-depth investigations to be carried out, and the state-of-affairs to be documented, often in considerable detail. Importantly, this goes beyond the routine work, but also includes long-term tasks such as the development of methods for sampling and data generation, methods for data interpretation, and transfer of all these methods to users in authorities and contract laboratories. All these elements will then form the empirical and conceptual foundations that need to be in place for a meaningful implementation of the legislation and, subsequently, its effectiveness evaluation. The problem of data availability and data quality under REACH is a case in point.

The two examples presented above demonstrate that the demand for research in environmental chemistry and ecotoxicology is caused by unresolved old problems such as the emissions and environmental and health impacts of PCBs, but also by many new issues such as the incremental substitution of hazardous chemicals under REACH or the monitoring of POPs that is a long-term obligation under the Stockholm Convention. For example, Wöhrnschimmel et al. [ 10 ] have shown that many more years of data generation will be needed before the effectiveness of the Stockholm Convention can be assessed. One would expect that the wide range of important and complex tasks for environmental chemistry and ecotoxicology would have helped to firmly establish these fields at universities. However, this is not the case and the ongoing cut-back on positions and resources for environmental chemistry and ecotoxicology is short-sighted and irresponsible. The underlying reasons for this situation may be manifold; to some extent, it could simply be lack of awareness and/or preferences for other, more “modern”, topics among the decision makers in universities. Another reason may be that environmental chemistry and ecotoxicology are perceived as fields of applied research without “true” academic relevance in comparison to well-established fields such as organic chemistry or booming areas such as material sciences.

Academic standing of environmental chemistry and ecotoxicology

To evaluate the academic productivity of a field of research, two questions can be asked: (i) are new methods that are genuine to the field developed on the basis of ongoing research, i.e., is improving the methods, techniques, and tools a component of active and ongoing research in the field? (ii) Are the problems and questions investigated in the field continuously refined and are new questions and research objectives derived from the insights gained?

A closer inspection of our fields shows that both requirements are fulfilled for environmental chemistry and ecotoxicology. Obviously, there have been extraordinary improvements of analytical methods, but also a multitude of environmental factors that govern the environmental fate of chemicals, the many impacts of anthropogenic chemicals on environmental and human health, and the emission sources of many types of chemicals released to the environment are increasingly better understood, mechanistically characterized, and assembled as the elements of a big picture. However, as scientists in these fields, we have to point out the productivity of our research more explicitly. These discussions need to reach the decision makers in academic institutions.

What is to be done?

First, a real danger to environmental chemistry and ecotoxicology is that they may be perceived (and presented) as fields where lists of routine tasks are worked down. If this happens, it will eliminate environmental chemistry and ecotoxicology as academic subjects. To confront this danger, the great demand for research and teaching in environmental chemistry and ecotoxicology and their academic productivity need to be pointed out explicitly in discussions in university committees tasked with priority setting—when positions, curricula, equipment, laboratory space, and financial resources are to be assigned and overall research priorities are to be determined.

Second, in addition to applied research and practical work, environmental chemistry and ecotoxicology have always had a strong component of basic research. Basic research is an essential part of these fields, and practical applications of methods and tools by authorities and industry are only possible because there is basic research that develops these methods and contributes to the scoping of problems and identifying relevant questions and tasks. Therefore, environmental chemistry and ecotoxicology need to be rooted in academic science, along with sufficient equipment, resources, and prospects for development. Environmental chemistry and ecotoxicology investigate a complex set of societally relevant issues, and there are many open and pressing problems related to the use of chemicals that have not been solved. As long as so many chemicals are present in so many technical applications and consumer products—which is considered a desirable aspect of modern societies—environmental chemistry and ecotoxicology are absolutely essential as the fields that help identify and understand the risks associated with the ever increasing use of chemicals.

Third, the environmental and health impacts of chemical pollution are not less important than other environmental impacts. Chemical pollution is one of the several globally relevant impacts as pointed out by Rockström et al. [ 11 ], who have identified nine impacts of global importance, ranging from climate change to chemical pollution, and they emphasize that these impacts do not act independently, but often reinforce one another. Recently, Rockström [ 12 ] stated:

“Among these nine there are three that have kind of come out as being the fundamental endgame of how all the planetary boundaries operate, and the number one is biodiversity. (…) The second fundamental boundary is climate change. (…) And the third of the big three is what we call “novel entities”. The totally man-made boundary. It has nothing to do with anything that the planet has ever experienced before, and it is our invention of chemicals, compounds, that are alien to nature like persistent organic pollutants (…).”

The call for a strong environmental chemistry and ecotoxicology could not be clearer.

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Helpful comments by Miriam Diamond are gratefully acknowledged.

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Scheringer, M. Environmental chemistry and ecotoxicology: in greater demand than ever. Environ Sci Eur 29 , 3 (2017). https://doi.org/10.1186/s12302-016-0101-x

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Synthesis of Polynorbornene Based Molecular Self-Assembly for the Detection of Copper Ions Present in the Environmental Water Samples

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Metal-assisted molecular self-assembly finds applications in optoelectronics, chemical sensing and catalysis. In this article, fluorescein based polynorbornene is synthesized and its molecular self-assembly is used to detect the presence of copper (II) ions in environmental water samples (pond waters). First of all, the sequential procedures of the synthesis of norbornene and polynorbornene are accomplished using simple organic compounds available in the Indian market. Various intermediate compounds and norbornene are characterized by 1H NMR and 13C NMR techniques. Structure of polynorbornene is proved by 1H NMR spectroscope. Molecular weight of polynorbornene is obtained using Acquity advanced polymer chromatography. Particle size of polymer nano-aggregates is derived by using FESEM microscope. This polynorbornene (PNor-Flu) is used for the selective and sensitive detection of the copper(II) ions with an excellent LOD of 0.27 µM, far below the limit decided by the Environmental Protection Agency (EPA) of USA. This is achieved with the help of UV-Vis studies and spectroscopic titrations using OD416/OD350. As far the self-assembly is concerned using microscopic analysis, polynorbornene with a higher number of hydroxyl groups shows rod-like self-assembly. Polynorbornene structure is again transformed to a spherical shape in the presence of the copper(II) ions even in micromolar concentration. From this change, it is believed that the poynorbornene has a high potentiality for sensing the copper(II) ions, which helps it to impart unique morphological properties. From the tests performed on real water samples, polynorbornene has proved its high efficiency of selective and sensitive detective power for detecting copper (II) ions in pond waters.

Fluorescein; Molecular Self-assembly; Polymer; Polynorbornene; Sensing

Introduction

Nature organized itself with a wide variety of molecular architecture with different types of nanostructural self-assembly which includes DNA double helix, tubulin assembly lipid build blocks, etc. Molecular self-assembly is a highly efficient process that involves non-covalent interactions such as hydrogen bonding, hydrophobic forces, π-stacking interactions, van der Waals forces, metal coordination, and electrostatic interactions. These forces help in transforming a disordered system into an ordered one, with well-organized shapes, sizes, and dimensions 1 . Molecular self-assembly   assists   in   the spontaneous   association   of   the macromolecules to adopt dynamic supramolecular assemblies such as nanofibers, nanoparticles, and nanotubes. By connecting the unique properties of host-guest with molecular self-assembly, it is possible to unlock new frontiers in optoelectronics, sensing, and catalysis. This simple and efficient approach offers tremendous potential for advancing cutting-edge technologies and solving complex scientific challenges. In this article, it is proposed to make a polymer-based metal-assisted molecular self-assembly. Its sensing properties have enough potential for real-life application in the sensing area 2-5 . Heavy metals, particularly copper (II) ions, are crucial for the metabolism of living organisms 6 . Copper (II) ions serve as a cofactor for cuproenzymes and help regulate various metabolic processes in our bodies, including neuro-signal transduction and gene expression 7 . This highlights the importance of copper (II) ions in maintaining optimal physiological functions. Excessive intake of copper can be extremely harmful to our health as it is highly toxic and can result in various health complications such as liver function abnormalities, liver cirrhosis, or Wilson’s disease. Industries that use copper without proper regulation can lead to contamination of environmental water, and it can ultimately enter our bodies through the food chain 8 . Therefore, it is important to detect and monitor Cu 2+ ions in water or other aqueous solutions to ensure environmental safety and promote good health. Numerous methods have been reported in the scientific literature for detecting and monitoring the presence of copper (II) ions in water. Most of these methods involve electromagnetic or mass spectroscopy techniques such as ICP-MS, ICP-OES, atomic absorption spectrometry, laser-induced breakdown spectroscopy, voltammetric techniques, and atomic emission spectrometry 9 . However, the major drawback of these techniques is that they require expensive equipment and difficult sample preparation procedures, which makes them less widely available and restricts their application for detection of copper. On the other hand, colorimetric sensors derived from polymers are in high demand due to their unique self-assembly based on host-guest interaction 10-11 . They are also very economical and easily accessible for detecting copper ions. Our present work represents a new sensor for the detection of copper ions from environmental samples. A fluorescein-derived norbornene-based monomer, Nor-Flu, and its polymer, PNor-Flu, are introduced in this article. These compounds demonstrate exceptional selectivity and sensitivity for copper ions detection. With this new work, it is possible to detect copper ions with greater accuracy and efficiency, making it a highly valuable tool for environmental monitoring and analysis. It was previously reported that copper has a higher affinity to make coordination bonds with the electronegative nitrogen atom of the imine bond and oxygen atom of the hydroxyl group which presents very adjacently to make a stable complex along with color change of the solution in the presence of the copper due to the formation of the highly stable ligand to metal charge transfer complex. It was confirmed that both the monomer (Nor-Flu) and the polymer (PNor-Flu) exhibited excellent LOD which is quite below the limit stated by US-EPA. Also in the case of the polymer due to the presence of amphiphilicity within the polymeric macromolecules, it is showing interesting host-guest molecular self-assembly in the presence and the absence of the copper ions with unique molecular architecture.

Materials and Methods

Organic chemicals such as cis-5-norbornene-exo-2,3-dicarboxylic anhydride, 4-aminophenol, Acetic acid, Hexamethelene diamine (HMTA), Trifluoroacetic acid, Fluorescein, Hydrazine hydride, Ethanol, Grubb’s 2nd generation Grubbs catalyst, Ethyl vinyl ether, Dimethyl sulfoxide (DMSO), Dichloromethane (DCM), Diethyl ether (Et 2 O), CDCl 3 , DMSO-d 6 , Sodium Hypochlorite, Hydrogen peroxide, and Tertiary butyl hydroperoxide are bought from from Sigma Aldrich, Spectrochem, and Combiblocks.  The stock analyte solutions of CuSO 4 , MgCl 2 , FeSO 4 , K 2 CO 3 , PbNO 3 , AgNO 3 , NiCl 2 , CdSO 4 , CaSO 4 , and AlCl 3 were prepared by using analar chermicals.

NMR characterizations were performed on a Bruker 500 MHz instrument for both 13 C and 1 H NMR and   13 C NMR spectroscopic techniques, employing DMSO-D 6 and CDCl 3 as the NMR solvents. Throughout the experiments, Tetramethylsilane (TMS) served as the internal standard for calibration. Acquity Advanced Polymer Chromatography (APC) was used to get thhe molecular weight of the polymer with Omnisec Reveal detector, employing refractive index (RI), light scattering (RALS 90°, LALS 7° angle), and a viscometer for detection.

UV-visible absorption studies were performed using a Perkin-Elmer Lambda35 UV-Vis spectrometer, with a scan rate of 480 nm/min. Each absorption spectrum was measured individually in a 1 cm quartz cell for every solution. Sample preparation for UV-Vis studies were done with utmost care. All stock solutions of Nor-Flu and PNor-Flu were initially prepared in DMSO and later diluted with water for various experiments. Metal solutions were exclusively prepared in water. UV-Vis spectroscopy involved maintaining fixed concentrations of Nor-Flu (μM) and PNor-Flu (μM). Spectroscopic titrations were conducted by introducing fixed concentrations of Nor-Flu solution to successive increasing concentrations of Cu 2+ ions. Real samples were consistently prepared using water as the solvent. Scanning electron microscope (SEM) was employed the high-performance variable pressure FE-SEM (Zeiss SUPRA 55VP-Field Emission Scanning Electron Microscope) to determine the size of the nano-aggregates. This FESEM utilizes patented GEMINI column technology and a Schottky type field emitter system, with a single condenser featuring a crossover-free beam path. In high vacuum mode, the resolution is 1.0 nm at 15 kV and 1.6 nm at 1 kV, while in variable pressure mode, it is 2.0 nm at 30 kV.

Though synthesis of polynorbornene (PNor-Flu) is not main objective of the research article, the synthetic methodology is shown in Scheme-1. The equential procedures of synthesis of polynorbornene is done using simple organic compounds available in the Indian market. Synthesis of the compounds 1-3, Nor-Flu and PNor-Flu involves synthetic procedures as detailed below. Synthesis of Compound-1 was synthesized first from analar chemicals. Cis-5-Norbornene-exo-2,3-dicarboxylic anhydride (1 g, 0.006 mol) was taken in a 100 mL roundbottom flask followed by the addition of glacial acetic acid. The mixture was stirred for 15 minutes. To the mixture 4-aminophenol (0.665 g, 0.006 mol) was added and refluxed at 110 ºC for 24 hours. After completion of the reaction, the mixture was cooled to room temperature. The formed precipitate was filtered and recrystallized from ethanol to obtain Compound 1 as brown solid (1.2 g, 77%). Synthesis of Compound-2 was synthesized from Compound-1. First Compound-1 (1 g, 0.004 mol) was taken in a 250 mL round-bottom flask and 50 mL of TFA added to it. After complete solubility of Compound-1, HMTA (660 mg, 0.0048 mol) was added to the reaction mixture and kept in refluxing condition for 24 hours. After completion of the reaction, the mixture was cooled to room temperature. The cooled reaction mixture was transferred to a 250 mL separating funnel with DCM and extracted with 2(N) HCl solution, water, and brine. Then combined DCM layer was dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to obtain the crude product. Flash column chromatography was carried out t:o obtain Compound 2 as a white powder (700 mg. 64%). Synthesis of Compund-3 was synthesized from Compound-2. First Compound-2 (500 mg, 0.0018 mol) was dissolved in DMF and K 2 CO 3 (300 mg, 0.0022 mol) was added to it. The reaction mixture was stirred for 5 minutes followed by the addition of ethyl iodide (280mg, 0.0018 mol). The overall mixture was stirred for 24 hours at room temperature and the progress of the reaction was monitored using TLC. After completion of the reaction, the mixture was poured into ice-cold water. A white-colored precipitate was observed, which was filtered and washed with cold water to remove unreacted compounds. After drying, Compound-3 was obtained as a white-colored powder (490 mg, 90%). Compounds 1-3  were characterized using 1 H-NMR and 13 C-NMR spectral techniques 12-17 .

Synthesis of monomer Nor-Flu was obtained from Compounds-2&3. In a 100 mL round-bottom flask, 732 mg (2.116 mmol) of Compound-3 was dissolved in 5 mL of ethanol with the assistance of a stirring magnetic bar. Following this, 600 mg (2.116 mmol) of Compound-2 was introduced into the flask, accompanied by the addition of 5 drops of acetic acid, and the mixture was refluxed for 18 hours. After the reaction concluded, the reaction mixture was concentrated and poured into a beaker containing cold water, resulting in the formation of a white precipitate. This precipitate was subsequently filtered and subjected to multiple washes with water. Finally, the precipitate was dried to obtain the absolutely pure product as a white solid, yielding 486 mg (81%). Synthesis of polymer PNor-Flu was accomplished from Nor-Flu. It involves a ring-opening polymerization. Nor-Flu (0.0816 mmol, 1 eq.) was placed in a dried 10 mL polymerization vial under a complete nitrogen atmosphere and dissolved in 1 mL of dry DCM. Subsequently, a catalytic amount of Grubbs second-generation catalyst (0.01 eq.) was added by dissolving 200 μL of dry DCM solution, and the reaction mixture was stirred at a specified temperature for 7 hours under a nitrogen atmosphere. The polymerization reaction was then quenched using ethyl vinyl ether. The resulting reaction mixture was precipitated in diethyl ether to obtain a white solid random copolymer. Confirmation of polymerization was achieved through 1 H NMR spectroscopy.  Additionally, confirmation was obtained from Advanced Permeation Chromatography to get number average molecular weight and polydispersity index 12-17 .

Results and Discussion

Photophysical studies of Nor-Flu

After successfully synthesizing Nor-Flu and PNor-Flu, it is the examination of its photophysical properties of the sensor application. It is anticipated that the sensor molecule would form a stable complex in the solution in the presence of copper ions, resulting in colourimetric responses. To achieve this, UV-Vis spectroscopic studies of Nor-Flu in the presence and absence of copper (II) ions was performed. Initially, optimization of the solvent system by varying nonpolar to polar and protic to aprotic solvents was done.

The present observations revealed that Nor-Flu exhibited an excellent response only in the case of DMSO. The photophysical studies of Nor-Flu were conducted in DMSO. It was observed that in the absence of copper ions, Nor-Flu showed an absorption peak at a wavelength of 343 nm. However, in the presence of copper ions, Nor-Flu exhibited a new, red-shifted absorption peak at a wavelength of 417 nm, accompanied by a change in the color of the solution from colorless to yellow. To determine the full response time of the monomer, a time-dependent study was carried out. This study revealed that the absorption maxima at 417 nm reached saturation within one minute, indicating that the sensing of copper in the presence of Nor-Flu is instantaneous (Fig.1-A). To assess the selectivity properties of Nor-Flu, UV-Vis spectroscopic studies were performed in the presence of different types of metal ions. The results, shown in Fig.1-B and Fig.1-C, clearly indicated that Nor-Flu only responds in the presence of copper (II) ions, as evidenced by both UV-Vis spectroscopy and pictorial visualization. Having obtained positive results in the selectivity and time-dependent studies of Nor-Flu, it is quite essential to investigate its sensitive properties. UV-Vis spectroscopic titration of Nor-Flu with successive increases in the concentration of copper(II) ions from 0 µM to 80 µM was performed (Fig.2).

A ratiometric titration curve was obtained, where the absorption maxima at 417 nm increased and the absorption maxima at 343 nm decreased with the addition of the copper(II) ions. It is observed that after adding 50 µM of copper(II) ions, the absorption intensity at 417 nm and 343 nm became saturated. To determine the lower limit of detection of copper, the calibration curve has been drawn in the lower concentration region (0 µM to 30 µM) and achieved an excellent linearity with R 2 value of 0.98087. From the calibration curve, the LOD value of 78 nM was obtained, which is well below the limit provided by the WHO for environmental water. Based on the obtained results, it was found that Nor-Flu can detect copper(II) ions instantly with excellent selectivity and sensitivity, with an LOD of 78 nM.

Determination of the binding constant and stoichiometry

The positive results in the case of selectivity, time-dependent study, and titration have motivated us to further investigate the photophysical properties of Nor-Flu, as shown in Fig.3. It is hypothesized that Nor-Flu forms a complex in the presence of copper(II) ions by creating a coordination bond with the nitrogen atom of the imine bond and the oxygen atom of the hydroxyl bond 12-17 . Additionally, ligand-to-metal charge transfer likely occurs during the formation of the complex, leading to the observed color change in the presence of copper(II) ions. The binding constant was determined from the UV-Vis titration to be approximately 2.47×10 5 , using the Benesi-Hildebrand equation. Furthermore, employing Job’s method, UV-Vis spectroscopy analysis was performed with increasing mole fraction of Nor-Flu and calculated a binding ratio of 1:2 for Nor-Flu and copper(II) ions.

Photophysical studies of PNor-Flu

After achieving excellent results in the photophysical studies of the monomer (Nor-Flu), It proceeded to investigate the photophysical properties of the polymer (PNor-Flu). Although Nor-Flu demonstrates exceptional photophysical properties for the selective and sensitive detection of copper(II) ions, its practical application is limited. Due to the lack of amphiphilicity, the challenge lies in producing films, paper strips, and unique self-assembly properties. To overcome this issue, synthesis was accomplished by ring-opening metathesis-based polynorbornenes for the selective and sensitive detection of copper(II) ions, as well as to study its host-guest self-assembly with copper(II) ions. Following the synthesis of the final polymer, the average molecular weight of PNor-Flu was determined using advanced polymer chromatography, which was found to be approximately 8000 Da with a PDI value of 1.10. To assess the photophysical properties of PNor-Flu,  UV-Vis spectroscopic study was conducted in the presence and absence of copper(II) ions (Fig.4). In the absence of copper(II) ions, PNorFlu exhibited an absorption peak at 350 nm in DMSO. Upon addition of copper(II) ions to the PNor-Flu solution in DMSO, the peak at 350 nm decreased, and a new red-shifted peak at 416 nm emerged, accompanied by a change in the color of the solution from colorless to yellow.

Furthermore, a time-dependent study was performed to determine the time required for the complete sensing of copper(II) ions by PNor-Flu. The sensing of copper(II) ions by PNor-Flu is instantaneous, as the peak OD 416 /OD 350 reaches its maximum within one minute after the addition of the copper (II) ions. Afterwards, the LOD was determined. For that purpose, the concentration-dependent UV-Vis titration of the PNor-Flu was obtained with the increase of the concentration of Copper(II) ions from 0 µM to 100 µM. It was observed that with an increase of the copper(II) ions concentration, the absorption maxima at 416 nm increased and absorption maxima at 350 nm decreased which suggests that it was ratiometric titration pattern with the isobestic point of 370 nm. Also from the OD 416 /OD 350 vs concentration of the PNor-Flu at a lower concentration range, the calibration curve was plotted with an excellent R 2 value of 0.99319 and from the 3σ/K equation, the LOD of 0.27 µM was obtained. So far the obtained result related to the PNor-Flu, it looks that like the Nor-Flu, PNor-Flu has a higher selectivity and the sensitivity of LOD value 0.27 µM for the detection of the copper(II) ions instantaneously within one minute. The lower LOD value suggests that PNor-Flu can be utilized as a sensor for the detection of copper ions in environmental contaminants.

Morphological analysis of the PNor-Flu in the presence of copper(II) ions

Metal-based molecular self-assembly is another important aspect of this work. The results obtained in the sensing study of the Nor-Flu and PNor-Flu clearly show that a definite self-assembly pattern will observed in the absence and the presence of the copper(II) ions. Along with that, a definite level of amphiphilicity is there in the polar solvent of PNor-Flu because of the presence of a large number of hydroxyl groups in the PNor-Flu. To check the morphological properties of the PNor-Flu, initially, the dynamic light scattering study of the PNor-Flu was done by increasing the concentration from 0.025 mg/ml to 0.05 mg/ml. It was observed that in between the concentration range from 0.03 mg/ml to 0.05 mg/ml the size of the PNor-Flu becomes fixed which is about to be 91 nm. Also, form the same DLS study was repeated with the addition of the copper ions. In this case, the hydrodynamic diameter of 100 nm with the concentration range of the polymer 0.035 mg/ml was obtained. Next work performed was checking the SEM images of the PNor-Flu in the presence and absence of the copper(II) ions. It was observed that in the absence of copper(II) ions, the PNor-Flu is showing rod-like self-assembly (Fig.5, B, C). Whereas in the presence of copper(II), it shows spherical-like self-assembly (Fig.5, E, F). All the self-assembly properties were investigated in the THF and water 1:1 mixture. Each of the monomers contains three hydroxyl groups, they take part in higher-order hydrogen bonding in the polymeric form and form rod-shaped self-assembly. Whereas in the presence of the copper(II) ions, it is forming a coordination bond with the oxygen atom of the hydroxyl group next to the imine group which lifted the possibility of the hydrogen bonding. That’s why in the presence of the copper(II) ions it forms spherical self-assembly.

Real sample analysis

It has been observed that copper(II) contamination often occurs due to the uncontrolled release of copper-based metal derivatives into the environment, which pollutes water bodies. To assess the ability of PNor-Flu to detect unknown amounts of copper(II) ions in environmental water, a real sample analysis was conducted. First, a calibration curve has been drawn using known concentrations of copper(II) ions in the presence of PNor-Flu. Then, different unknown concentrations of copper(II) ions were introduced into pond water (India) and added a fixed concentration of PNor-Flu to each solution. Subsequently, UV-Vis spectroscopy was recorded and were compared the OD 416 /OD 350 with the calibration curve to determine the corresponding copper(II) ion concentrations. The present polymeric sensor PNor-Flu is capable of determining the unknown concentration of copper(II) in environmental contaminants with more than 98% accuracy (Table 1).

Table 1: Real sample analysis using PNor-Flu solution

Conclusions

Synthesis of the fluorescein-based polynorbornenes has been completed, PNor-Flu, for the selective and sensitive detection of copper(II) ions from environmental contaminants. Through concentration-dependent titration, it has been demonstrated that PNor-Flu exhibits very high sensitivity and selectivity for copper(II) ions, with a limit of detection (LOD) value of 0.27 µM, which is lower than the limit permitted by the EPA. Additionally, It has been investigated the host-guest molecular self-assembly of PNor-Flu in the absence and presence of copper(II) ions. The present observations revealed that in the absence of copper(II) ions, PNor-Flu exhibits rod-like self-assembly, whereas in the presence of copper(II) ions, it forms spherical aggregates. Furthermore, present investigation based on real sample analysis indicates that PNor-Flu has an efficiency of over 98% in determining the copper(II) ion content in contaminated water.

Acknowledgement

Author’s special thanks goes to his wife and son for their continuous moral support.

Conflict of Interests

There is no conflicts of interests in this work

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