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  • 1. Khaled, Amina
    et al.
    Richard, Claire
    Redin, Lisa
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Niinipuu, Mirva
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Janson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jaber, Farouk
    Sleiman, Mohamad
    Characterization and Photodegradation of Polybrominated Diphenyl Ethers in Car Seat Fabrics from End-of-Life Vehicles2018In: Environmental Science and Technology, ISSN 0013-936X, E-ISSN 1520-5851, Vol. 52, no 3, p. 1216-1224Article in journal (Refereed)
    Abstract [en]

    In this study, we examined the photodegradation of decabromodiphenyl ether (BDE-209) on the surface of car seat covers from end-of-life vehicles (ELVs). Samples were collected at two car dismantling facilities in Sweden and cover car models from 1989 to 1998. The content of polybrominated diphenyl ethers (PBDEs) in nine real samples (fabric and polyurethane foam) was first characterized. Fabric samples that did not contain BDE-209 were then spiked with BDE-209 and irradiated in the laboratory and under sunlight. Photoproducts were identified using high performance liquid chromatography coupled to electrospray ionization mass spectrometer (HPLC-ESI-Orbitrap-MS), whereas volatile products were analyzed by gas chromatography mass spectrometry (GC-MS). Similar photodegradation rates and oxidation products were observed in fabric samples irradiated in the laboratory and those collected from ELVs. Estimated half-life of BDE-209 on fabric inside vehicles ranged from 3 to 6 years. Thirteen major photoproducts were identified as lower brominated products, hydroxylated BDEs, brominated and hydroxylated dibenzofurans (PBDFs) and dioxins (PBDDs). Furthermore, several photoproducts were found to be transferable into water, particularly bromophenols and hydroxylated BDEs, and others into gas phase, such as bromomethanol and 1,2-dibromoethane. This should be taken into consideration for better estimating exposure to PBDEs and to develop strategies for ELV recycling.

  • 2.
    Niinipuu, Mirva
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Tailoring residue-derived carbon materials for the removal of wastewater contaminants: adsorption and surface properties2019Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    The availability of effective, low-cost wastewater treatment is necessary for increased water recycling and the prevention of environmental pollution on a global scale. Adsorption on activated carbons is commonly applied in wastewater treatment, but the high cost of conventional activated carbons limits the use of this technique. Several waste streams, such as the residues and by-products of food processing, agriculture and industrial processes, are currently inefficiently utilized and could be transformed into value-added carbon materials. Re-thinking how waste is utilized could reduce waste handling costs and increase resource efficiency, which would provide both economic and environmental benefits. Therefore, low-cost carbon materials prepared from renewable low-cost resources are an attractive alternative to decreasing the costs of wastewater treatment.

    The research underlying this thesis investigated the potential of carbonized residue materials to remove environmentally relevant concentrations of organic and inorganic contaminants from wastewater. The research covered in this thesis included the carbonization of tomato- and olive press wastes, rise husks, horse manure, municipal wastewater sludge and bio- and fiber sludges from pulp and paper mills. The effect of carbonization temperature and starting material was studied in terms of surface properties and contaminant removal to gain knowledge on which surface features are beneficial for the removal of different contaminants. The extent to which different chemical activations of carbonized materials improve the contaminant removal was also studied.

    The results demonstrate that carbonized materials are generally quite ineffective at removing organic compounds from water, which may be due to the low surface areas of these materials. Carbonization temperature was shown to alter the surface functionalities of the carbons, more specifically, high carbonization temperatures decreased oxygen-containing surface functionalities that benefitted the removal of most contaminants (which was most pronounced for Zn and trimethoprim). Further experiments investigated the role of the water matrix, and the results unexpectedly showed higher removal from a complex water matrix. Chemical activation improved removal efficiencies for all of the studied compounds, with the most pronounced effects observed for organic compounds. The activated carbons were able to completely remove fluconazole and trimethoprim from the landfill leachate water, and also showed high removal efficiensies (50-96%) of Cu and Zn. Furthermore, the results showed that adsorbate compounds may interact with the adsorbent surface in diverse ways, for example, via properties such as porosity and the presence of oxygen-containing functionalities or minerals. Also, adsorbate hydrophobicity (log Kow) affected the removal of organic compounds in some of the studied hydrochars. The research discussed in this thesis has highlighted that future studies should study the broad range of environmentally-relevant adsorbates through multi-component adsorption systems that include several complex water matrices.

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  • 3.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bergknut, Magnus
    MTC-Miljötekniskt Center AB, Umeå, Sweden.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rosenbaum, Erik
    MTC-Miljötekniskt Center AB, Umeå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Influence of water matrix and hydrochar properties on removal of organic and inorganic contaminants2020In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 27, p. 30333-30341Article in journal (Refereed)
    Abstract [en]

    The removal of contaminants from water using low-cost adsorbents has been widely studied, yet studies employing a realistic water matrix are still lacking. This study investigated the removal of organic compounds (trimethoprim, fluconazole, and perfluorooctanoic acid (PFOA)) and metals (As, Zn, and Cu) from landfill leachate. Additionally, tests in pure water, humic acid, and ion matrices were carried out to better understand how the water matrix affects adsorption. The hydrochars were produced from four feedstocks at three carbonization temperatures. The results show that the removal efficiencies for organic pollutants were low and metal removal by hydrochars was comparable with commercial activated carbon. The removal of all compounds from pure water was substantially lower. Tests with humic acid and ion-containing matrices could not fully explain the increased removal in the landfill leachate, which may be due to the combination of the water matrix and presence of soluble species from the hydrochars.

  • 4.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bergknut, Magnus
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Tailoring the functionality of waste materials using hydrothermal carbonization for water treatment applicationsManuscript (preprint) (Other academic)
    Abstract [en]

    Purpose:

    The material properties of carbons from hydrothermal carbonization (HTC), typically referred to as hydrochars, are crucial for hydrochar use in adsorption-related applications. More knowledge is needed on how HTC temperature is altering material properties of different wet low-cost materials and how it is affecting adsorption of contaminants. Studies systematically comparing different feedstocks and carbonization temperatures are needed, because comparisons between available studies are obstructed by the differences in reaction conditions and analysis techniques. 

    Methods: In this study, hydrochars were prepared at 180℃, 220℃, and 260℃ from fiber sludge and biosludge from a paper mill, digested sewage sludge, and horse manure. Surface properties of the raw materials and chars were characterized and the adsorption capacity of methylene blue was studied. 

    Results: The most substantial change, i.e., a decrease in the oxygen-functionalities of cellulose-rich materials (horse manure and fiber sludge), was caused by degradation of cellulose, while digested sludge types (biosludge and sewage sludge) seemed not to change substantially with the HTC temperature. Adsorption capacities varied between 9.0 and 68 mg g-1 char, being highest for biosludge treated at 220℃. Adsorption dropped drastically at the highest HTC temperature (260℃), which may be due to the decrease in oxygen-containing functionalities. Also substantial differences were seen between different feedstock materials. 

    Conclusions: These results suggest that adsorption properties can be tailored both by selection of HTC temperature and feedstock.

  • 5.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bergknut, Magnus
    MTC-Miljötekniskt Center AB, Umeå, Sweden.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    The impact of hydrothermal carbonization on the surface functionalities of wet waste materials for water treatment applications2020In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 27, no 19, p. 24369-24379Article in journal (Refereed)
    Abstract [en]

    Hydrothermal carbonization (HTC) is an energy-efficient thermochemical process for converting wet waste products into value added materials for water treatment. Understanding how HTC influences the physicochemical properties of the resultant materials is critical in optimizing the process for water treatment, where surface functionality and surface area play a major role. In this study, we have examined the HTC of four wet waste streams, sewage sludge, biosludge, fiber sludge, and horse manure at three different temperatures (180 degrees C, 220 degrees C, and 260 degrees C). The physicochemical properties of these materials were examined via FTIR, SEM and BET with their adsorption capacity were assessed using methylene blue. The yield of solid material after hydrothermal carbonization (hydrochar) decreased with increasing temperature for all samples, with the largest impact on horse manure and fiber sludge. These materials also lost the highest degree of oxygen, while HTC had minimal impact on biosludge and sewage sludge. The differences here were due to the varying compositions of each waste material, FTIR identified resonances related to cellulose in horse manure and fiber sludge, which were not detected in biosludge and sewage sludge. Adsorption capacities varied between 9.0 and 68 mg g(-1) with biosludge HTC at 220 degrees C adsorbing the highest amount. Adsorption also dropped drastically at the highest temperature (260 degrees C), indicating a correlation between adsorption capacity and HTC conditions. This was attributed to the loss of oxygen functional groups, which can contribute to adsorption. These results suggest that adsorption properties can be tailored both by selection of HTC temperature and feedstock.

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  • 6.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    From waste to water treatment: Physicochemical and wastewater adsorption properties of activated hydrothermally carbonized waste materialsManuscript (preprint) (Other academic)
    Abstract [en]

    Activated carbon forms an important step in the treatment of waste water in water treatment facilities. These facilities produce a range of underutilized sludge materials, which can be synthesized into activated carbon, reducing the amount of disposed sludge. Other waste materials high in organic matter, such as horse manure, are also ideal contenders for activated carbon upgrading. This study compares the hydrothermal carbonization followed by activation of sewage sludge and horse manure. Chemical activation was conducted using KOH and H3PO4, with physicochemical properties and adsorption of multiple contaminants being tested. Yield and inorganic content varied considerably, with KOH activated materials producing lower yields with higher inorganic content. A maximum surface area of 1363 m2g-1 and 343 m2g-1 was achieved for the horse manure and sewage sludge, respectively. Horse manure activated carbons displayed a high affinity for all adsorbates, other than arsenic, which was associated with high carbon content, carbon-oxygen functional groups and low mineral content.

  • 7.
    Niinipuu, Mirva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Industrial Doctoral School, Umeå University.
    Latham, Kenneth G.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    The influence of inorganic components and carbon-oxygen surface functionalities in activated hydrothermally carbonized waste materials for water treatment2020In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 27, no 30, p. 38072-38083Article in journal (Refereed)
    Abstract [en]

    In this study, we have examined how the activation of hydrothermally carbonized sewage sludge and horse manure influences the inorganic component of these materials and surface chemistry. This was examined through statistical correlations between kinetic tests using trimethoprim, fluconazole, perfluorooctanoic acid, and copper, zinc, and arsenic and physicochemical properties. Yield and inorganic content varied considerably, with potassium hydroxide-activated materials producing lower yields with higher inorganic content. Phosphoric acid activation incorporated inorganically bound phosphorus into the material, although this showed no statistically relevant benefit. A maximum surface area of 1363 m(2)g(-1)and 343 m(2)g(-1)was achieved for the horse manure and sewage sludge. Statistical analysis found positive correlations between carbon-oxygen functionalities and trimethoprim, fluconazole, perfluorooctanoic acid, and copper removal, while inorganic content was negatively correlated. Conversely, arsenic removal was positively correlated with inorganic content. This research provides insight into the interactions with the organic/inorganic fraction of activated waste materials for water treatment.

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  • 8.
    Redin, Lisa
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Niinipuu, Mirva
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Occurrence of brominated diphenyl ethers, dibenzo-p-dioxins and dibenzofurans in foam materials in scrapped car seats from 1985 to 20122017In: Waste Management, ISSN 0956-053X, E-ISSN 1879-2456, Vol. 61, p. 300-306Article in journal (Refereed)
    Abstract [en]

    Abstract The purpose of this study was to evaluate the occurrence of polybrominated diphenyl ethers (PBDEs), dibenzo-p-dioxins (PBDDs) and dibenzofurans (PBDFs) in polyurethane foam (PUF) from car seats of end-of-life vehicles (ELVs) and compare the concentrations of PBDEs with the stipulated regulations in the POP Directive. The method comprised screening by X-ray fluorescence (XRF) and GG-MS analysis. Of 59 tested samples from ELVs, 17 samples showed lines above limit of detection (LOD) levels when screening by XRF. Those samples were selected as replicates and for further analysis by GC-MS. The majority of the studied samples showed low or non-detectable concentrations of PBDEs and PBDD/Fs, but two samples showed concentrations of Σ Te-HpBDEs close to the regulated level for Te-HpBDEs in waste (1000 mg kg−1); one was slightly higher (1390 mg kg−1) and the other slightly lower (570 mg kg−1). It was concluded that brominated pollutants such as Te-HpBDEs occur in low levels in automotive applications in scrapped cars produced in years when brominated flame retardants were used. However, two of the 59 samples tested showed levels close to those stipulated by regulations concerning POPs in waste.

  • 9.
    Späth, Jana
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Brodin, Tomas
    Department of Wildlife, Fish, And Environmental Studies, Swedish University of Agricultural Sciences, Umeå, Sweden.
    Falås, Per
    Department of Chemical Engineering, Lund University, Lund, Sweden.
    Niinipuu, Mirva
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Lindberg, Richard
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Fick, Jerker
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Nording, Malin
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Effects of conventionally treated and ozonated wastewater effluent on the damselfly larva oxylipidome in response to on-site exposure2022In: Chemosphere, ISSN 0045-6535, E-ISSN 1879-1298, Vol. 309, article id 136604Article in journal (Refereed)
    Abstract [en]

    Pharmaceutical residues discharged through insufficiently treated or untreated wastewater enter aquatic environments, where they may adversely impact organisms such as aquatic invertebrates. Ozonation, an advanced wastewater treatment technique, has been successfully implemented to enhance the removal of a broad range of pharmaceuticals, however diverse byproducts and transformation products that are formed during the ozonation process make it difficult to predict how ozonated wastewater may affect aquatic biota. The aim of this study was to investigate effects on fatty acid metabolites, oxylipins, in a common invertebrate species, damselfly larvae, after on-site exposure to conventional wastewater treatment plant (WWTP) effluent and additionally ozonated effluent at a full-scale WWTP. Subsequent ozonation of the conventionally treated wastewater was assessed in terms of i) removal of pharmaceuticals and ii) potential sub-lethal effects on the oxylipidome. Northern damselfly (Coenagrion hastulatum) larvae were exposed for six days in the treatment plant facility to either conventional WWTP effluent or ozonated effluent and the effects on pharmaceutical levels and oxylipin levels were compared with those from tap water control exposure. Ozonation removed pharmaceuticals at an average removal efficiency of 67% (ozone dose of 0.49 g O3/g DOC). Of 38 pharmaceuticals detected in the effluent, 16 were removed to levels below the limit of quantification by ozonation. Levels of two oxylipins, 12(13)-EpODE and 15(16)-EpODE, were reduced in larvae exposed to the conventionally treated wastewater in comparison to the tap water control. 15(16)-EpODE was reduced in the larvae exposed to ozonated effluent in comparison to the tap water control. One oxylipin, 8-HETE, was significantly lower in larvae exposed to conventional WWTP effluent compared to ozonated effluent. In conclusion, the study provides proof-of-principle that damselfly larvae can be used on-site to test the impact of differentially treated wastewater.

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  • 10.
    Weidemann, Eva
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Umeå Energi AB, Umeå, Sweden.
    Niinipuu, Mirva
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Industrial Doctoral School, Umeå University, Umeå, Sweden.
    Fick, Jerker
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Jansson, Stina
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Using carbonized low-cost materials for removal of chemicals of environmental concern from water2018In: Environmental Science and Pollution Research, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 25, no 16, p. 15793-15801Article in journal (Refereed)
    Abstract [en]

    Adsorption on low-cost biochars would increase the affordability and availability of water treatment in, for example, developing countries. The aim of this study was to identify the precursor materials and hydrochar surface properties that yield efficient removal of compounds of environmental concern (CEC). We determined the adsorption kinetics of a mixture containing ten CECs (octhilinone, triclosan, trimethoprim, sulfamethoxasole, ciprofloxacin, diclofenac, paracetamol, diphenhydramine, fluconazole, and bisphenol A) to hydrochars prepared from agricultural waste (including tomato- and olive-press wastes, rice husks, and horse manure). The surface characteristics of the hydrochars were evaluated via diffuse reflectance infrared spectroscopy (DRIFTS), X-ray photoelectron spectroscopy (XPS), and N2-adsorption. Kinetic adsorption tests revealed that removal efficiencies varied substantially among different materials. Similarly, surface analysis revealed differences among the studied hydrochars and the degree of changes that the materials undergo during carbonization. According to the DRIFTS data, compared with the least efficient adsorbent materials, the most efficient hydrochars underwent more substantial changes during carbonization.

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