Amicarbazone, atrazine, and metribuzin behavior was examined in a field setting in Tennessee and in a laboratory setting using soils collected from Illinois and Tennessee. Fields planted to corn were sampled from 0 to 8 cm depth, and the samples were analyzed using methanolic extraction followed by tandem mass spectrometry analysis to determine residual herbicide concentrations. Conditions were favorable for herbicide degradation, including warm temperatures and adequate rainfall. All herbicide half-lives were <10 d. Laboratory research using soils with known atrazine-use histories showed that amicarbazone did not exhibit enhanced microbial degradation due to previous atrazine use. Apparent amicarbazone and metribuzin persistence levels implied that early-season weed control would be expected, but carryover to injure sensitive rotational crops would not be anticipated under these environmental conditions. Dissipation under field conditions of amicarbazone and metribuzin was not affected by being applied to separate plots or by coapplication to the same plots.

Soybean [Glycine max (L.) Merr.] that lack resistance to auxin herbicides [i.e., not genetically modified for resistance] have well-documented responses to those particular herbicides, with yield loss being probable. When a soybean field is injured by auxin herbicides, regulatory authorities often collect a plant sample from that field. This research attempted to simulate soybean exposures due to accidental mixing of incorrect herbicides, tank contamination, or particle drift. This research examined whether analytical testing of herbicide residues on soybean to aminocyclopyrachlor (ACP), aminopyralid, 2,4-D, or dicamba would be related to the visual observations and yield responses from these herbicides. ACP and aminopyralid were applied to R1 soybean at 0.1, 1, and 10 g ae ha−1; 2,4-D and dicamba were applied at 1, 10, and 100 g ae ha−1. Visual evaluations and plant sample collections were undertaken at 1, 3, 7, 14, and 21 d after treatment (DAT), and yield was measured. The conservative limits of detection for the four herbicides in this project were 5, 10, 5, and 5 ng g−1 fresh weight of soybean for ACP, aminopyralid, 2,4-D, and dicamba, respectively. Many of the plant samples were non-detects, especially at lower application dosages. All herbicide concentrations rapidly declined soon after application, and many reached nondetectable limits by 14 DAT. All herbicide treatments caused soybean injury, although the response to 2,4-D was markedly lower than the responses to the other three herbicides. There was no apparent correlation between herbicide concentrations (which were declining over time) and the observed soybean injury (which was increasing over time or staying the same). This research indicated that plant samples should be collected as soon as possible after soybean exposure to auxin herbicides.

Mollusk shells are often found in archeological sites, given their great preservation potential and high value as a multipurpose resource, and they can often be the only available materials useful for radiocarbon (14C) dating. However, dates obtained from shells are often regarded as less reliable compared to those from bones, wood, or charcoals due to different factors (e.g., Isotope fractionation, reservoir effects etc.). The standard acid etching pretreatment for mollusk shells is the most used in many 14C laboratories, although another protocol known as CarDS (Carbonate Density Separation) was introduced just over a decade ago. We compare these two methods with two newly proposed methods for intracellular organic matrix extraction. We applied all four methods to samples selected from different archeological layers of the well-known Upper Paleolithic site of Vale Boi, rich in mollusk specimens throughout the stratigraphic sequence. Here we compare our results to previous dates to determine which of these pretreatment methods results in the most reliable 14C dates. Based on the results of this study, all four methods gave inconsistent ages compared to previous dates and the stratigraphic attribution.

Obtaining accurate radiocarbon (14C) results from wood samples requires the extraction of cellulose. In the past, this has been done using different combinations of methods including acidified bleaching, acid-base-acid, and strong bases. This often becomes a time-consuming task in most analyses, especially when single ring isotope chronologies are needed from wood samples. Using 14C and Fourier-transform infrared spectroscopy (FTIR), we tested four different pretreatment methods to determine their ability to produce high quality cellulose. We then adjusted the best methods to determine a method for pretreating wood laths of multiple rings. A sequence of base-acid-base-acid-bleach + strong base (BABAB+) and BABAB produced the most accurate results when compared to the Bomb20 Northern Hemisphere Zone 1 curve with an average difference in Δ14C of 1.3‰ and 5.8‰ respectively. These methods were adjusted to pretreat an entire wood lath and a comparison of the FTIR results suggest that our adjusted BABAB+ and BABAB produced high quality cellulose comparable to that of an individually pretreated ring. The possibility to pretreat wood lath samples has the potential to more than double the number of tree rings which can be pretreated in a week. This is a significant reduction in time when creating long tree ring chronologies.

Microprobe analyses of optically homogeneous detrital biotites from sandstones of the Visingsö Group and the Dala Sandstone, Sweden, revealed a consistently low K content (generally <0.75 atom/formula unit) and variable amounts of Fe, Mg, Al, and Si. Electron probe profiles of some biotite grains indicated two major types of interstratification, one consisting of mainly illite layers and the other apparently consisting of chlorite layers. The layer thicknesses commonly ranged between 0.5 and 3 μm. Microprobe analyses of some thick (∼5 μm) illitic layers indicated a phengitic composition, wherein the mica was relatively rich in octahederal Fe and Mg. The chloritic layers appeared to be Fe-Mg-rich and generally had octahederal totals of <6 atom/formula unit. Variations in the chemical composition of the biotite and some of the illite and chlorite were probably due to an uneven distribution of small amounts of the interstratified phases. The illite and chlorite layers were apparently formed by pseudomorphic replacement of detrital biotites, i.e., gradual replacement of one biotite layer by one layer(s) of illite and/ or chlorite during diagenesis.

A program of simultaneous linear equations has been developed to calculate component proportions and/or component property values for mineral mixtures in soil clays and sediments. The analysis is based on quantitatively measured chemical and physical properties of samples and involves (1) qualitative identification of the mineral components in the mixture by any appropriate means; (2) quantitative measure of the sample property values selected for use in the program; (3) estimation of the proportion of each component in the mixture by a technique such as X-ray powder diffraction; (4) assignment of limits to component property ranges; (5) selection of one of four available calculation options and application of the simultaneous linear-equations program; (6) examination of the residuals of the analysis and, if appropriate, adjustment of the initial estimates for component proportions or property ranges and then repeating step 5; and (7) verification of the final component proportions by comparison with information from step 1. Completeness and/or accuracy of the final results for component proportions may be checked by the closeness of approach to 1.0 for the sum of the component proportions. The method requires that, at minimum, the number of properties measured must equal the number of components in the samples being analyzed and that the minimum number of samples must equal the number of properties measured.

Using the clay fractions of 15 Pennsylvania soils containing kaolinite, illite, smectite, vermiculite, chlorite, interstratified vermiculite/chlorite, quartz, and noncrystalline material, and measuring methylene blue cation-exchange capacity, the amount of Ca displaced by Mg from a Ca-saturated clay, the amount of K displaced by NH4 from a K-saturated clay heated to 110°C, % K2O, % SiO2, % MgO, and weight loss at 110°–300°C and 300°–950°C, the adjustment of property values was found to have the lowest residual value and the most consistent results. The source of analytical errors was also located by examination of residual tables. Samples that were similar in composition gave more reliable component proportions.

Mineralogical and chemical analyses of fine clay fractions from in and around Lake Abert, Lake County, Oregon, show that the pyroclastic rocks supplying detritus to the lake weather to a suite of layer silicate clay minerals varying from high-charge dioctahedral montmorillonite to montmorillonite/intergrade smectite-chlorite interstratifications. In the lake these clays extract K, Mg, and Si to form authigenic interstratified illite and a trioctahedral, Mg-rich mineral resembling stevensite in composition. Both the neoformed interstratifications contribute little unambiguously to X-ray powder diffraction patterns, which are dominated by the reflections of detrital clays. From limited data it appears that the illite occurs below 0.8 m depth in sediments of a possibly somewhat fresher (brackish) lake and the trioctahedral interstratification between 0.4 and 0.2 m depth in sediments of a lake of about the same size and salinity (about 30–90 g/kg) as that of the present lake.

Two rapid methods for the decomposition and chemical analysis of clays were adapted for use with 20–40-mg size samples, typical amounts of ultrafine products (<0.5-μm diameter) obtained by modern separation methods for clay minerals. The results of these methods were compared with those of “classical” rock analyses. The two methods consisted of mixed lithium metaborate fusion and heated decomposition with HF in a closed vessel. The latter technique was modified to include subsequent evaporation with concentrated H2SO4 and re-solution in HCl, which reduced the interference of the fluoride ion in the determination of Al, Fe, Ca, Mg, Na, and K. Results from the two methods agree sufficiently well with those of the “classical” techniques to minimize error in the calculation of clay mineral structural formulae. Representative maximum variations, in atoms per unit formula of the smectite type based on 22 negative charges, are 0.09 for Si, 0.03 for Al, 0.015 for Fe, 0.07 for Mg, 0.03 for Na, and 0.01 for K.

A standardless method of energy dispersive X-ray fluorescence in conjunction with scanning electron microscopy was used to analyze selected areas of clay-size particles of talc, pyrophyllite, and kaolinite supported by a carbon planchet. Peak intensity ratios of fluorescing elements relative to silicon were converted directly to weight or mole ratios using conversion factors determined theoretically. The conversion factors depend upon particle thickness and mass adsorption coefficients of the sample for the elements analyzed. The effects of particle thickness become significant above ~0.1 μm. Without using particle thickness corrections, the mean molar ratios of metal to Si agreed to within 6.1,0.5, and 9.7% of the theoretical ratios for kaolinite, pyrophyllite, and talc, respectively.

Selective-dissolution techniques by ammonium oxalate (OX), dithionite-citrate-bicarbonate (DCB), and dithionite-ethylenediaminetetraacetic acid (D-EDTA), and X-ray diffraction and Mössbauer spectroscopy were used to identify and characterize iron oxides and oxyhydroxides in the <2-mm, <50-μm, and <2-μm size fractions of a Mollisol from Bahia Bianca, Argentina. Iron compounds are present at low concentrations in mixtures with quartz, Na-rich feldspar, illite, interstratified illite-montmorillonite, and traces of kaolinite. Total Fe and Al content increases as soil particle size decreases, from 4.3 and 13.3 wt. % in the <2-mm size fraction to 8.5 and 22.8 wt. % in the clay fraction (<2 μm), respectively. No more than 25–30% of the total Fe is associated with the crystalline and the amorphous Fe oxides. Weakly ferromagnetic hematite and goethite were identified in the different fractions. These phases have small particle sizes and/or low crystallinity. They may also have Al for Fe substitutions. Crystalline magnetite or maghemite is rare. These Fe-rich phases are probably coating coarser particles.

The efficiency of Fe removal is highest for the D-EDTA treatment and least efficient for the OX method, for all fractions. The opposite is true for Al removal. Poorly crystalline hematite and goethite, which are soluble in oxalate, are only present in the coarser fractions. Poorly crystalline and crystalline hematite and goethite, which are soluble in DCB and EDTA, are present in coarser fractions, but do not occur in the clay fraction. DCB treatment probably dissolves Al in the 2:1 type phyllosilicates occurring in this soil, whereas D-EDTA dissolves Fe in the hydroxy interlayers of the smectite minerals or in the silicate phases.

A dispersion-centrifugation-decantation procedure was used to isolate various particle size fractions from a sample of clay (<2 µm fraction) separated by sedimentation from the Ap horizon of a Webster soil (fine-loamy, mixed, mesic Typic Haplaquoll). The 0.02–0.06 µm size fraction was found to be enriched in an illitic phase associated with randomly interstratified smectite/illite. X-ray powder diffraction, chemical analysis, and high-resolution transmission electron microscopy confirmed that most of the illitic material in the 0.02–0.06 µm size fraction was composed of two-layer elementary illite particles with a layer charge of −0.47 per formula unit. The results demonstrate that this low-charge illitic phase can be physically separated from soil materials and that the low-charge illitic phase has chemical, morphological, and mineralogical properties that are uniquely different from those of smectite and illite.

The chemical and the mineralogical composition of a group of pumiceous tuffs associated with recent salic volcanic episodes from Tenerife (Canary Islands) have been studied. The investigation focused on the two main types of pyroclastic deposits of the zone: ash-flows and ash-falls. The samples can be classified chemically as trachytic and phonolitic rocks with an intermediate silica content and a high percentage of alkali cations (Na+ and K+). The mineralogical composition, determined by X-ray diffraction, scanning electron microscopy, and optical microscopy, shows the occurrence of zeolites (mainly phillipsite, with lesser chabazite and analcime), associated with the parent glass. K-feldspar (sanidine) and calcite are accessory minerals. Zeolites are significantly more abundant in the ash-flow deposits. Zeolite formation by hydrothermal weathering in closed-system conditions varies according to the nature and the origin of the pyroclastic deposits. Tenerife phillipsites differ from typical diagenetic, lacustrine, and deep-sea phillipsites, both in chemical and mineralogical features. Alkali cations exceed divalent cations in the unit-cell that, assuming a monoclinic symmetry, has the following parameters: a = 8.46–10.55 Å, b = 14.21–14.40 Å, c = 7.80–8.70 Å, and β = 105°–110°.

A hydrothermally altered rhyolitic hyaloclastite from Ponza island, Italy, has four alteration zones with unique clay assemblages: (1) a non-pervasive argillic zone characterized by smectite; (2) a propylitic zone with interstratified illite-smectite (I-S) containing 10–85% illite (I); (3) a silicic zone composed of I-S with ≥90% I and pure illite; and (4) a sericitic zone with I-S ranging from 66% I to pure illite. Atomic force microscopy reveals abrupt changes in particle morphology with illitization, including initial changes from anhedral plates to laths and then to euhedral plates and hexagonal plates. I-S particles progressively thicken with illitization and mean particle area (basal plane) remains constant from pure smectite to I-S with 80% I. However, particle area increases from 90 to 100% illite. Computer modeling of I-S structural forms indicates octahedral cation ordering progressively changes from cis- vacant smectite to interstratified cis- and tnuis-vacant I-S, and then to trans-vacant illite. In addition, polytypes progressively change from 1 Md to 1M, and then to 2M, illite. Electron-microprobe and X-ray fluoresence analyses show that I-S chemistry progressively changes during illitization, evolving toward a phengitic composition with ∼0.89 fixed interlayer K+ per O10(OH)2. Octahedral Mg2+ shows little change with illitization, varying from 0.3 to 0.5 cations per O,10(OH)2. The layer charge of smectite is ~0.38 equivalents per O10(OH)2.

On the basis of abrupt changes in morphology and progressive changes in polytype and chemistry, smectite illitization on Ponza involved a dissolution and recrystallization mechanism with multiple stages of nucléation and crystal growth. In this multi-step model, temperature of alteration provided the major control for the layer composition, polytype, and morphology of I-S crystallites. Other factors that may play a secondary role include: K+ availability, water-rock ratio, and permeability. Alternatively, the mechanism of I-S and illite formation at Ponza and other hydrothermal environments may occur by direct precipitation of I-S crystallites from rhyolite glass and may not involve progressive reactions of smectite precursors.

Calling males of Anastrepha obliqua release volatile compounds to attract conspecific males to form leks and females to mate. Male volatiles from Mexican and Brazilian populations of A. obliqua have been previously identified. However, there are differences in the number and identity of volatile compounds between the populations. These differences in volatile profiles may be due to male origin (e.g. wild or mass-reared flies) or methodological issues (e.g. sampling techniques). In this study, we evaluated the attractiveness of wild, laboratory non-irradiated, and laboratory-irradiated flies under semi-field conditions. Male volatiles were collected using dynamic headspace sampling (DHS) and solid-phase microextraction (SPME) techniques, and identified using gas chromatography-coupled mass spectrometry. The results showed no difference in the attractiveness of wild, laboratory non-irradiated, and irradiated males to females. However, the number of captured females differed according to the origin; wild and non-irradiated females were captured more frequently than the irradiated flies. A total of 21 compounds were found using SPME, whereas only 12 were collected using DHS, although the relative amounts of these compounds were higher than those obtained using the former sampling technique. In addition, only laboratory non-irradiated males released α-pinene and menthol, which have not been previously reported in this fruit fly species. Additionally, we identified novel compounds in A. obliqua; however, certain compounds previously reported were not detected. This study suggests that despite the qualitative and quantitative variations in the volatile profiles of A. obliqua males, their attractiveness was unaffected.

The National Environmental Isotope Facility (NEIF) Radiocarbon Laboratory at the Scottish Universities Environmental Research Centre (SUERC) performs radiocarbon measurement of a wide range of sample matrices for applications in environmental research. Radiocarbon is applied to palaeoenvironmental, palaeoceanographic, and palaeoclimatic investigations, as well as work to understand the source, fate, turnover, and age of carbon in the modern carbon cycle. The NEIF Radiocarbon Laboratory supports users in the development and deployment of novel sampling techniques and laboratory approaches. Here, we give an overview of methods and procedures used by the laboratory to support the field collection, laboratory processing, and measurement of samples. This includes in-house development of novel and/or specialized methods and approaches, such as field collection of CO2 and CH4, hydropyrolysis, and ramped oxidation. The sample types covered include organic remains (e.g., plant material, peat, wood, charcoal, proteins), carbonates (e.g., speleothems, foraminifera, mollusc shell, travertine), waters (dissolved organic and inorganic carbon), gases (CO2 and CH4), soils and sediments (including sub-fractions).

For several decades, many efforts have been dedicated to enhancing the accuracy of mortar radiocarbon dating and evaluating the reliability of the results concerning the typology of the examined specimens. Several assumptions that are fundamental for the application of the method may be in many cases not fulfilled, such as (a) complete primary limestone dissociation during calcination, (b) efficient separation of geogenic carbon contained in calcareous aggregates, (c) short carbonation time, and (d) absence of secondary calcite. Many laboratories all over the world have proposed different methods to select suitable fractions of mortar.

The first intercomparison attempt, involving eight international laboratories, was organized in 2016 aiming at comparing and statistically treating the results obtained on the same materials by different laboratories with their own characterization and pre-treatment methods (Hajdas et al. 2017; Hayen et al. 2017). Following this first step, a new intercomparison experiment was proposed and set up in 2018 during the Mortar Dating International Meeting (Bordeaux, FR). A new set of three mortar samples was chosen, taking care of the selection of standardized materials (homogeneity, known mineralogical composition, absence of exogenous inclusions, known expected age).

This work describes the results of two research teams involved in the intercomparison. The samples were characterized, selected, and dated depending on each laboratory strategy. The results stress the importance of the characterization of the raw material is to better understand the mineralogical and petrographical composition of the samples. Such information can support the choice of the most appropriate strategy for the extraction of CO2 and then for data interpretation.

Bentonite from the ‘Bogovina’ coal mine in Serbia, was characterized. The influence of acid treatment on its composition, as well as mathematical descriptions of this influence are reported. The purpose of this work was to correlate the concentration of the acid used for the treatment with the resulting bentonite composition. X-ray diffraction (XRD), infrared spectroscopy and quantitative chemical analysis were employed to define the changes caused by acid treatment.

The contents of all the cations, except Si, decreased exponentially with increasing concentration of the HCl used for the treatment of the bentonite. This approach was tested on previously published data and was shown to be valid.

The basal reflections of smectite decreased gradually and eventually disappeared after intense treatment, while the other reflections remained in the XRD patterns of all the samples, but decreased slightly with increasing acid strength. In addition, the amount of X-ray amorphous matter formed increased rapidly with increasing acid concentration up to 4.5 M. With further increase in the acid strength, the amount of X-ray amorphous matter remained virtually constant.