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Cortés-Sánchez, Julián David; Marino, Natalie; Vaquero, M. Carmen; Ansorena, J.; Legorburu, I.

doi:10.1023/a:1004925922786

Cited by 43 publications

(9 citation statements)

References 26 publications

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“…The examination of slags can provide significant information about chemical transformation rates and the metal stability associated therein [15][16][17][18][19][20]. Multiple geochemical investigations show that, historically, lead production has had an impact on environmental pollution since the Roman times, e.g., in England [21], Sweden [22], and Spain [23]. Metal transfer from the waste to the environment can occur even for several hundred years after the end of metallurgy or mining [24,25].Medieval lead and silver metallurgy is studied using mineralogical investigations of slags in France [26], Czech Republic [11,27], Germany [10], Italy [28].…”

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confidence: 99%

Pb-Rich Slags, Minerals, and Pollution Resulted from a Medieval Ag-Pb Smelting and Mining Operation in the Silesian-Cracovian Region (Southern Poland)

Cabała

Warchulski

Rozmus³

et al. 2019

Minerals

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Since the 12th century in the Silesian-Cracovian area, lead, litharge, and silver have been produced by the pyrometallurgical processing of Pb-Ag-Zn ore. Slags and soils contaminated with heavy metals (Zn, Pb, Cd, Fe, Mn, As) were the subject of this research. Samples were collected during archaeological works in the area of early medieval metallurgical settlement. The main goals of the analyses (Scanning Electron Miscroscopy-Energy Dispersive Spectroscopy (SEM-EDS), Electron Probe Microanalyzer (EPMA), X-ray diffraction (XRD), Atomic Absorption Spectroscopy (AAS)) were the determination of the mineralogical composition of furnace batches and smelting temperatures and conditions. In soils, the anthropogenic phases enriched in Pb, Zn, Fe, Mn, P, and primary minerals like goethite, ferrihydrite, sphalerite, galena, smithsonite, minrecordite, cerussite, gypsum, anglesite, jarosite, and hemimorphite were identified. The soil from former metallurgical settlements contained up to 1106 mg·kg −1 Pb, 782 mg·kg −1 Zn, 4.7 mg·kg −1 Cd in the fine fraction. Much higher heavy metal concentrations were observed in the waste products of ore rinsing, up to 49,282 mg·kg −1 Pb, 64,408 mg·kg −1 Zn, and 287 mg·kg −1 Cd. The medieval smelting industry and Pb-Ag-Zn ore processing are marked by highly anomalous geochemical pollution (Pb, Zn, Cd, Fe, Mn, Ba) in the topsoil. The methods of mineralogical investigation, such as SEM-EDS or EMPA, can be used to identify mineralogical phases formed during metallurgical processes or ore processing. Based on these methods, the characteristic primary assemblage and synthetic phases were identified in the area polluted by medieval metallurgy and mining of Pb-Ag-Zn ores, including MVT (Mississippi Valley Type) deposits. The minerals distinguished in slags and the structural features of metal-bearing aggregates allow us to conclude that batches have included mostly oxidised minerals (PbCO 3 , ZnCO 3 , CaZn(CO 3 ) 2 , FeOOH), sulfides (PbS and ZnS) and quartz (SiO 2 ). The laboratory experiment of high-temperature heating of the examined slags showed that smelting temperatures used in the second half of 13th century were very high and could have reached up to 1550 • C. The results indicate, that geochemical and mineralogical methods can be used to obtain important information from archaeological sites, even after archaeological work has long ceased.Minerals 2020, 10, 28 2 of 16 mining and metallurgy centres since Roman times. In the period between the 10th and 12th centuries, iron, lead, tin, silver, and gold had become more important for the development of civilization in Central and Eastern European countries. Since the beginning of the 10th century in medieval Europe, in areas where ores of Ag-Pb, Au, As-Au, Cu, Sn and Fe occurr, mining centres have appeared, such as at the Ore Mountains (Erzgebirge), Harz Mountains, and Sudetes.One of Europe's largest Zn-Pb, MVT (Mississippi Valley) type ore deposits can be found in the Silesian-Cracow area (southern Poland) [1]. Shallow deposits are represented...

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confidence: 99%

Pb-Rich Slags, Minerals, and Pollution Resulted from a Medieval Ag-Pb Smelting and Mining Operation in the Silesian-Cracovian Region (Southern Poland)

Cabała

Warchulski

Rozmus³

et al. 2019

Minerals

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“…25 The rate of dissolution of oxide films formed on the surface of TiO 2 -NPs in the presence of the strong acid solution is slower, and low recovery of thermodynamically stable rutile TiO 2 -NPs by HF/HNO 3 mixed acids in the current study is consistent with the literature. 12 However, the deviation of anatase and brookite TiO 2 -NPs from the same trend, indicated that HF/HNO 3 mixed acid digestion may not be a poor dissolution technique across all polymorphs of TiO 2 -NPs as previously noted, 16,18 but dissolution appears to be polymorph crystal structure-dependent (Table 4).…”

Section: Effect Of Digestion Type On Different Polymorphs Of Tio 2 -N...mentioning

confidence: 57%

“…Previous research revealed that nano-scale anatase and brookite polymorphs may alter phase stability and transform to rutile when heated. 16,22 For example, Smith et al 31 revealed that the transformation of anatase to rutile is thermodynamically favorable at all temperatures between 0 and 1300 K on the basis of Gibbs free energy calculations. However, others reported that conversion of anatase and brookite to rutile only occurred at temperature ranges between 800-1023 K, much greater than the 573 K in the current experiment.…”

Section: Effect Of Heat and Pressure On Different Polymorphs Of Tio 2...mentioning

confidence: 99%

“…In addition, the application of HF is required for the complete digestion and quantification of refractory metals in geological and environmental sample matrices such as soil, sediments and dusts. 16,17 This is because HF dissolves the aluminosilicate structure of environmental materials and facilitates the liberation of metals. 8,18 However, a recent study, 13 reported that Ti recovery by alkaline fusion using lithium metaborate (LiBO 2 ) was greater than open-vessel HF mixed acid digestion for rutile-rich environmental samples.…”

Section: Introductionmentioning

confidence: 99%

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Polymorph-dependent titanium dioxide nanoparticle dissolution in acidic and alkali digestions

Silva

Nadagouda

Patterson

et al. 2014

Environ. Sci.: Nano

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“…The prevalence of aluminosilicate structures in most environmental and geological samples (soils, sediments and dusts) necessitates their digestion in hydro-uoric acid (HF) if complete dissolution of the elements for analysis is desired. 11,12 While each method has its own advantages and disadvantages depending on the sample matrix, the underlying use of HF acid has long been identied as hazardous because of the extreme health and safety risks associated with its properties. 13 Due to the extreme risks associated with use of HF acid, it is desirable to develop a dissolution method which could serve as a safer alternative.…”

Section: Introductionmentioning

confidence: 99%

Examining the efficiency of muffle furnace-induced alkaline hydrolysis in determining the titanium content of environmental samples containing engineered titanium dioxide particles

Silva

Nadagouda

Webster

et al. 2013

Environ. Sci.: Processes Impacts

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A novel muffle furnace (MF)-based potassium hydroxide (KOH) fusion digestion technique was developed and evaluated for different titanium dioxide materials in various solid matrices. Digestion of different environmental samples containing sediments, clay minerals and humic acid with and without TiO(2) particles was first performed utilizing the MF-based KOH fusion technique and its dissolution efficacy was compared to a Bunsen burner (BB)-based KOH fusion method. The three types of TiO(2) particles (anatase, brookite and rutile) were then digested with the KOH fusion techniques and microwave (MW)-based nitric (HNO3)–hydrofluoric (HF) mixed acid digestion methods. Statistical analysis of the results revealed that Ti recoveries were comparable for the KOH fusion methods (BB and MF). For pure TiO(2) particles, the measured Ti recoveries compared to calculated values were 96%, 85% and 87% for anatase, brookite and rutile TiO(2) materials, respectively, by the MF-based fusion technique. These recoveries were consistent and less variable than the BB-based fusion technique recoveries of 104%, 97% and 72% and MW-based HNO3–HF mixed acids digestion recoveries of 80%, 81% and 14%, respectively, for anatase, brookite and rutile. Ti percent recoveries and measurement precision decreased for both the BB and MF methods when TiO(2) was spiked into sediment, clay minerals, and humic acid. This drop in efficacy was counteracted by more thorough homogenization of the spiked mixtures and by increasing the mass of KOH in the MF fusion process from 1.6 g to 10.0 g. The MF-based fusion technique is consistently superior in digestion efficiency for all three TiO(2) polymorphs. The MF-based fusion technique required 20 minutes for digestion of 25 samples (based on in-house Lindberg MF capacity) compared to 8 hours for the same number of samples using the BB-based fusion technique. Thus, the MF-based fusion technique can be used to dissolve a large number of samples in a shorter time (e.g., 500 samples per 8 hours) while conserving energy and eliminating health and safety risks from methods involving HF.

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Cited by 43 publications

References 26 publications

Pb-Rich Slags, Minerals, and Pollution Resulted from a Medieval Ag-Pb Smelting and Mining Operation in the Silesian-Cracovian Region (Southern Poland)

Pb-Rich Slags, Minerals, and Pollution Resulted from a Medieval Ag-Pb Smelting and Mining Operation in the Silesian-Cracovian Region (Southern Poland)

Polymorph-dependent titanium dioxide nanoparticle dissolution in acidic and alkali digestions

Examining the efficiency of muffle furnace-induced alkaline hydrolysis in determining the titanium content of environmental samples containing engineered titanium dioxide particles

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