Browsing by Author "Angelova L."

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    Characterization of Bulgarian Copper Mine Tailing as a Precursor for Obtaining Geopolymers
    (2024-02-01) Ilieva D.; Angelova L.; Radoykova T.; Surleva A.; Chernev G.; Vizureanu P.; Burduhos-Nergis D.D.; Sandu A.V.
    Valorization of high-volume mine tailings could be achieved by the development of new geopolymers with a low CO2 footprint. Materials rich in aluminum and silicon with appropriate solubility in an alkaline medium can be used to obtain a geopolymer. This paper presents a study of copper mine tailings from Bulgaria as precursors for geopolymers. Particle size distribution, chemical and mineralogical composition, as well as alkaline reactivity, acidity and electroconductivity of aqueous slurry are studied. The heavy metal content and their mobility are studied by leaching tests. Sequential extraction was applied to determine the geochemical phase distribution of heavy metals. The studied samples were characterized by high alkalinity, which could favor the geopolymerization process. The water-soluble sulphates were less than 4%. The Si/Al ratio in mine tailing was found to be 3. The alkaline reactivity depended more so on the time of extraction than on the concentration of NaOH solution. The main part of the heavy metals was found in the residual fraction; hence, in high alkaline medium during the geopolymerization process, they will stay fixed. Thus, the obtained geopolymers could be expected to exert low environmental impact. The presented results revealed that studied copper mine tailing is a suitable precursor for geopolymerization.
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    Comparative study of soil test methods for determination of plant available potassium in Bulgarian arable soils
    (2021-01-01) Angelova L.; Genova N.; Stoyanova S.; Surleva O.; Nekov I.H.; Ilieva D.; Surleva A.
    This comparative study was aimed at estimating analytical behavior of methods for determination of plant available potassium applied to Bulgarian arable soils and to reveal the relationship between the amount of extractable K. Twenty-four samples from two traditional agricultural regions in Bulgaria were studied. Soil potassium was extracted by NH4OAc/HOAc pH 4.5 (AA), diluted double acid (Mehlich 1), CaCl2, BaCl2 and a modified acetate/lactate method (ALM) and determined by Flame AES. The factors influencing the methods accuracy were identified and uncertainty was estimated. The expanded uncertainty was (in mg K2O (100 g dry soil)-1): 0.10 (ALM), 0.64 (Mehlich 1), 0.17 (CaCl2) and 1.1 (AA). The study revealed that the factor which mainly influence the uncertainty of the applied analytical methods for plant available potassium in soil was the calibration of Flame AES determination. The obtained results showed that extractable potassium lowered in the following order KALM ≥ KAA > KMechlich1 > KBaCl2 > KCaCl2. Soil potassium extracted by ALM procedure correlated with AA, BaCl2-K, CaCl2 –K and Mehlich 1 - K at 0.05 level of significance. ALM extracted between 1.2 to 5.8 times more soil K than other methods did. The obtained results provided a base for further study on correlation between extractable K and soil fertility indices for particular soil types and climatic regions in Bulgaria.
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    Contribution to the Molybdenum Blue Reaction and its Application in Soil Analysis
    (2022-01-01) Angelova L.; Genova N.; Pencheva G.; Statkova Y.; Yotova V.; Surleva A.
    This paper presents a study on the molybdenum blue reaction (MB) as a finishing detection step in soil analysis for quantification of plant available phosphorus. An ammonium acetate/calcium lactate reagent (pH= 4.2) was used for soil phosphorus extraction. The molybdenum blue color reaction using premixed Murphy-Riley reagent and ascorbic acid as a reductant was reinvestigated. UV-Vis characteristics of MB, optimal wavelength, reaction time and concentration of reductant were studied. The effect of ascorbic acid concentration and the reaction time on linearity, bias and uncertainty was discussed. The molybdenum blue reaction was found to obey Beer’s law in the targeted concentration range of 0.04 – 1.0 mg L-1 PO4 3--P. The linearity was proved by “lack-of-fit” test. The uncertainty budget was made and the uncertainty was estimated by modelling approach, as well as single laboratory and quality control approach. The recovery and the expanded uncertainty were found to be, respectively, (95.7 ± 8.7) % (P= 95%, n = 3) and 9.2 mg PO4 3--P /kg dry soil (k = 2). The results showed that the soil sample inhomogeneity and the repeatability of extraction process were the main factors which contribute to the uncertainty of measurement in soil analysis.
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    Ensuring the Quality of the Analytical Process in a Research Laboratory
    (2024-04-01) Surleva A.; Angelova L.; Ilieva D.; Ivanova V.; Surleva O.; Chavdarova K.
    Featured Application: The approaches for estimation of the analytical behavior of measuring methods could be applied in a research laboratory aiming at the characterization of new materials or a new method for analysis. The limitations of well-known approaches are described, and the alternatives are discussed. This paper discusses approaches for verification of methods of measurements of chemical and physical characteristics of specific samples. The limitations of well-known approaches are discussed. Some examples of alternatives are given to demonstrate specific issues encountered in the research laboratory analyzing new materials or characterizing new properties of materials. Application of sequential procedure using lower quantities of samples and reagents is presented. A standard addition to solid samples is discussed. The approach of control charts for estimation of method uncertainty for determination of plant available phosphorus is presented. The method comparison is applied as an approach to verification of alkaline reactivity by inductively coupled plasma–optical emission spectroscopy (ICP-OES) measurement, as well as density of newly synthesized chalcogenide glass materials. The presented examples demonstrated that alternative approaches are needed in order to verify the methods applied due to the great variety of activities and corresponding tasks in a research laboratory.
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    Estimation of soil and tailing dump toxicity: Development and validation of a protocol based on bioindicators and ICP-OES
    (2019-08-02) Ilieva D.; Angelova L.; Drochioiu G.; Murariu M.; Surleva A.
    A protocol for estimation of soil toxicity based on germination test, open acid sample digestion and ICP-OES determination of heavy metals and metalloids was proposed. Triticum aestivum was used as a bioindicator and germinated on contaminated soils. After estimation of the state of the plantlets, the accumulated heavy metals and metalloids content were determined. The sample digestion procedure and ICP-OES measurement were validated by analysing plant certified reference material. Additionally, standard addition before sample pretreatment was applied for estimation of method recovery at the levels of heavy metals found in plants from contaminated region. The recovery obtained was between 97 and 105 %. The precisions of the complete protocol (RSD), which included germination tests, sample digestion and ICP-OES measurements, ranged between 4.7% for Mn and 11 % for As. The expanded uncertainty was estimated. The proposed protocol was applied for estimation of soil toxicity and heavy metals bioavailability of tailing dump material and surrounding soils from an abandoned barite mine in Tarnita, Suceava, Romania. The coltsfoot used for remediation of the soil in the studied region was analysed. Cu, Ni, Zn, Mn, Pb, Fe and Al were found in the sample harvested nearby the tailing dump.