A new vacuum line to extract CO2 from carbonate and dissolved inorganic carbon (DIC) in water was established at Guangxi Normal University. The vacuum line consisted of two main components: a CO2 bubble circulation region and a CO2 purification collection region, both of which were made of quartz glass and metal pipelines. To validate its reliability, a series of carbonate samples were prepared using this system. The total recovery rate of CO2 extraction and graphitization exceeded 80%. Furthermore, the carbon content in calcium carbonate exhibited a linear relationship with the CO2 pressure within the system, demonstrating its stability and reliability. The system was also employed to prepare and analyze various samples, including calcium carbonate blanks, foraminiferal, shell, groundwater, and subsurface oil-water samples. The accelerator mass spectrometry (AMS) results indicated that the average beam current for 12C- in the samples exceeded 40 μA. Additionally, the contamination introduced during the liquid sample preparation process was approximately (1.77 ± 0.57) × 10−14. Overall, the graphitized preparation system for carbonate and DIC in water exhibited high efficiency and recovery, meeting the requirements for samples dating back to approximately 30,000 years.

The heavy atom content and distribution in chlorite were estimated using the relative intensities of basal X-ray powder diffraction (XRD) peaks. For these peaks to be meaningful, however, corrections had to be made for the effects of sample thickness, sample length, and preferred orientation of the mineral grains, all of which are 2θ dependent. The effects of sample thickness were corrected for by a simple formula. The effects of sample length were accounted for by using rectangular samples and by ensuring that the sample intersected the X-ray beam through the range of diffraction angles of interest. Preferred orientation of mineral grains were either measured directly or estimated. Estimated values were quicker and easier to obtain and were within 5% of measured values. A comparison of the compositional parameters of chlorite estimated before correcting for these sample effects with those estimated after the corrections had been applied indicate that the uncorrected values differed from the corrected values by as much as 55% of the latter values. Mounts of a single sample prepared by different filter-membrane peel and porous-plate techniques yielded widely different compositions until the measurements were corrected for sample effects. Analyses in triplicate indicated that the XRD intensity ratio 003/001 is preferred for calculating heavy atom distributions and abundances in chlorite because of the relative strength of the 001 peak.

X-ray diffraction patterns were obtained from rock fragments, < 1 μm randomly oriented freeze-dried powders, and < 1 μm oriented aggregates for 11 mixed-layered illite/smectite samples (K-bentonites) that cover the range from 14 to 100 percent expandable. In all cases, 00l and hkl comparisons show no evidence of laboratory induced artifacts. Either the laboratory procedures caused no disaggregation of fundamental illite particles, or, if they did, fundamental particle reaggregation during sample preparation duplicated the one and three-dimensional structures of the illite/smectite in the original, untreated rock.

Demodulation of the 20l, 13l reflections into a two-dimensional band shape occurred with increasing percent expandable layers in illite/smectite. This result strongly supports the contention that turbostratic displacements occur at the expandable interfaces between fundamental particles, and are limited to those sites.

A comparison of the quantities measured by powder X-ray diffraction and high resolution transmission electron microscope (TEM) lattice fringe image techniques for disordered crystals suggests that meaningful comparisons between the two methods can be made only if a sufficient number of images are recorded to define the statistical parameters of the disorder.

The degree of preferred orientation of mineral grains in powder X-ray diffraction (XRD) samples prepared by standard techniques has been evaluated by means of a correction model implemented in the Rietveld program, BGMN. It is demonstrated that neither front- nor side-loading of mineral powders obtained by wet grinding in a McCrone micronizing mill yield powder mounts with randomly oriented particles. Despite fine grinding, the primary sizes and shapes of mineral grains contained in multi-phase samples influence the degree of preferred orientation in XRD powder mounts. Two minerals, both of platy habit, were found to show different degrees of preferred orientation in front- and side-loaded samples. In contrast to these methods of sample preparation, the spray-drying technique yielded perfect randomness of the particles. The experiments on artificial mineral mixtures demonstrate that the model applied can effectively correct for preferred orientation allowing reliable Rietveld quantitative phase analysis of moderately textured samples prepared by standard techniques.

This paper describes an improved simple, sample-mounting method for random powder X-ray diffraction (XRD), namely the razor tamped surface (RTS) method, which prepares a powder mount by tamping the loose powder with the sharp edge of a razor blade. Four kaolinites and a quartz powder were used to evaluate the RTS method by quantifying the degree of orientation in the sample mounts using orientation indices. Comparisons between the RTS and other published simple methods, consisting of front loading, back loading and side loading, indicate that the RTS method produces minimum packing density and minimum preferred orientation in the powder mounts of all five samples. The quartz powder used in this study does exhibit a tendency to preferred orientation. The mechanism by which the RTS method reduces preferred orientation is examined by comparing the width of the sharp blade edge with the size of clay particles. The advantages and disadvantages of the RTS method are also discussed.

Electron tomography (ET) has gained increasing attention for the 3D characterization of nanoparticles. However, the missing wedge problem due to a limited tilt angle range is still the main challenge for accurate reconstruction in most experimental TEM setups. Advanced algorithms could in-paint or compensate to some extent the missing wedge artifacts, but cannot recover the missing structural information completely. 360° ET provides an option to solve this problem by tilting a needle-shaped specimen over the full tilt range and thus filling the missing information. However, sample preparation especially for fine powders to perform full-range ET is still challenging, thus limiting its application. In this work, we propose a new universal sample preparation method that enables the transfer of selected individual nanoparticle or a few separated nanoparticles by cutting a piece of carbon film supporting the specimen particles and mounting them onto the full-range tomography holder tip with the help of an easily prepared sharp tungsten tip. This method is demonstrated by 360° ET of Pt@TiO2 hollow cage catalyst showing high quality reconstruction without missing wedge.

A new system for preparing 14C samples was established for a compact accelerator mass spectrometer (GXNU-AMS) at Guangxi Normal University. This sample preparation system consists of three units: a vacuum maintenance unit, a CO2 purification unit, and a CO2 reduction unit, all of which were made of quartz glass. A series of radiocarbon (14C) preparation experiments were conducted to verify the reliability of the system. The recovery rate of graphite obtained was more than 80%. The carbon content in the commercial toner and wood sample was linearly fitted to the CO2 pressure in the measurement unit of the system. The results showed a good linear relationship, indicating that the reliability of the sample preparation system. AMS measurements were conducted on a batch of standard, wood, and dead graphite samples prepared using this system. The results showed that the beam current of 12C- for each sample was more than 40 μA, the carbon contamination introduced during the sample preparation process was ∼ 2 × 10–15, and that the new sample preparation system is compact, low-contamination, and efficient and meets the GXNU-AMS requirements for 14C samples.

The effect of sample preparation on a pre-aged Al–Mg–Si–Cu alloy has been evaluated using atom probe tomography. Three methods of preparation were investigated: electropolishing (control), Ga+ focused ion beam (FIB) milling, and Xe+ plasma FIB (PFIB) milling. Ga+-based FIB preparation was shown to introduce significant amount of Ga contamination throughout the reconstructed sample (≈1.3 at%), while no Xe contamination was detected in the PFIB-prepared sample. Nevertheless, a significantly higher cluster density was observed in the Xe+ PFIB-prepared sample (≈25.0 × 1023 m−3) as compared to the traditionally produced electropolished sample (≈3.2 × 1023 m−3) and the Ga+ FIB sample (≈5.6 × 1023 m−3). Hence, the absence of the ion milling species does not necessarily mean an absence of specimen preparation defects. Specifically, the FIB and PFIB-prepared samples had more Si-rich clusters as compared to electropolished samples, which is indicative of vacancy stabilization via solute clustering.

Manual selection of targets in experimental or diagnostic samples by transmission electron microscopy (TEM), based on single overview and detail micrographs, has been time-consuming and susceptible to bias. Substantial information and throughput gain may now be achieved by the automated acquisition of virtually all structures in a given EM section. Resulting datasets allow the convenient pan-and-zoom examination of tissue ultrastructure with preserved microanatomical orientation. The technique is, however, critically sensitive to artifacts in sample preparation. We, therefore, established a methodology to prepare large-scale digitization samples (LDS) designed to acquire entire sections free of obscuring flaws. For evaluation, we highlight the supreme performance of scanning EM in transmission mode compared with other EM technology. The use of LDS will substantially facilitate access to EM data for a broad range of applications.

A focused ion beam (FIB) technique describing the preparation of specimens for in situ thermal and electrical transmission electron microscopy is presented in detail. The method can be applied to a wide range of materials and allows the sample to be thinned down to electron transparency while it is attached to the in situ chip. This offers the advantage that the specimen can have a quality in terms of contamination and damage due to the ion beam that is comparable to samples prepared by means of conventional FIB preparation. Additionally, our technique can be performed by most commercially available FIB devices and only requires three simple, custom stubs for the procedure. This should enable a large userbase for this type of sample fabrication. One further benefit of our technique is that the in situ chip can be reused to create another sample on the same chip. The quality of the samples is demonstrated by high-resolution transmission electron microscopy as well as electron energy loss spectroscopy.

Detrital zircon geochronology can help address stratigraphic- to lithospheric-scale geological questions. The approach is reliant on statistically robust, representative age distributions that fingerprint source areas. However, there is a range of biases that may influence any detrital age signature. Despite being a fundamental and controllable source of bias, handpicking of zircon grains has received surprisingly little attention. Here, we show statistically significant differences in age distributions between bulk-mounted and handpicked fractions from an unconsolidated heavy mineral sand deposit. Although there is no significant size difference between bulk-mounted and handpicked grains, there are significant differences in their aspect ratio, circularity and colour, which indicate inadvertent preferential visual selection of euhedral and coloured zircon grains. Grain colour comparisons between dated and bulk zircon fractions help quantify bias. Bulk-mounting is the preferred method to avoid human-induced selection bias in detrital zircon geochronology.

CryoEM has become the method of choice for determining the structure of large macromolecular complexes in multiple conformations, at resolutions where unambiguous atomic models can be built. Two effects that have limited progress in single-particle cryoEM are (i) beam-induced movement during image acquisition and (ii) protein adsorption and denaturation at the air-water interface during specimen preparation. While beam-induced movement now appears to have been resolved by all-gold specimen support grids with very small holes, surface effects at the air-water interface are a persistent problem. Strategies to overcome these effects include the use of alternative support films and new techniques for specimen deposition. We examine the future potential of recording perfect images of biological samples for routine structure determination at atomic resolution.

The Radiocarbon Laboratory of the Fluminense Federal University was installed in 2009, and its NEC Single Stage Accelerator Mass Spectrometry system has been operational since 2012. As the first 14C-AMS facility in Latin America, the LAC-UFF became a reference center for radiocarbon (14C) dating in Brazil. Over the years we have implemented pretreatment protocols for several kinds of materials, such as cellulose, soil, bone, and biofuels. In the present paper we describe our current protocols for the preparation of these types of samples. Moreover, after 10 years of operation, with the aim of expanding the range of materials we are able to analyze, we report the results of several tests to improve accuracy, precision and background levels. For example, here we discuss how isotopic fractionation during the graphitization and measurement steps has been controlled. Concerning results interpretation, our research group has been using OxCal chronological models to analyze different contexts such as stromatolite growth, tree rings, soil deposition and marine reservoir effect (MRE) determination.

Cryo-electron microscopy (cryo-EM) has become the technique of choice for structural biology of macromolecular assemblies, after the ‘resolution revolution’ that has occurred in this field since 2012. With a suitable instrument, an appropriate electron detector and, last but not least, a cooperative sample it is now possible to collect images from which macromolecular structures can be determined to better than 2 Å resolution, where reliable atomic models can be built. By electron tomography and sub-tomogram averaging of cryo-samples, it is also possible to reconstruct subcellular structures to sub-nanometre resolution. This review describes the infrastructure that is needed to achieve this goal. Ideally, a cryo-EM lab will have a dedicated 300 kV electron microscope for data recording and a 200 kV instrument for screening cryo-samples, both with direct electron detectors, and at least one 120 kV EM for negative-stain screening at room temperature. Added to this should be ancillary equipment for specimen preparation, including a light microscope, carbon coater, plasma cleaner, glow discharge unit, a device for fast, robotic sample freezing, liquid nitrogen storage Dewars and a ready supply of clean liquid nitrogen. In practice, of course, the available budget will determine the number and types of microscopes and how elaborate the lab can be. The cryo-EM lab should be designed with adequate space for the electron microscopes and ancillary equipment, and should allow for sufficient storage space. Each electron microscope room should be connected to the image-processing computers by fibre-optic cables for the rapid transfer of large datasets. The cryo-EM lab should be overseen by a facility manager whose responsibilities include the day-to-day tasks to ensure that all microscopes are operating perfectly, organising service and repairs to minimise downtime, and controlling the budget. Large facilities will require additional support staff who help to oversee the operation of the facility and instruct new users.

With the wide application of ultra-microtome sectioning in the preparation of transmission electron microscopy (TEM) specimens with bio- and organic materials, here, we report an ultra-microtome-based method for the preparation of TEM specimens from cathodes of Li-ion batteries. The ultra-microtome sectioning reduces the sample thickness to tens of nanometers and yields atomic resolution from the core region of particles of hundreds of nanometers. Analysis indicates that the mechanical cross-sectioning introduces no observable microstructural artifacts or structural damage, such as microcracking and nanoporosity. These results demonstrate the high efficiency of the ultra-microtome approach in preparing well-thinned specimens of particulate materials that allow for atomic-scale TEM imaging of a large number of sectioned particles in one single TEM specimen, thereby providing statistically significant results of the TEM analysis.

Atom probe tomography (APT) is used to quantify atomic-scale elemental and isotopic compositional variations within a very small volume of material (typically <0.01 µm3). The small analytical volume ideally contains specific compositional or microstructural targets that can be placed within the context of the previously characterized surface in order to facilitate a correct interpretation of APT data. In this regard, careful targeting and preparation are paramount to ensure that the desired target, which is often smaller than 100 nm, is optimally located within the APT specimen. Needle-shaped specimens required for atom probe analysis are commonly prepared using a focused ion beam scanning electron microscope (FIB-SEM). Here, we utilize FIB-SEM-based time-of-flight secondary ion mass spectrometry (ToF-SIMS) to illustrate a novel approach to targeting <100 nm compositional and isotopic variations that can be used for targeting regions of interest for subsequent lift-out and APT analysis. We present a new method for high-spatial resolution targeting of small features that involves using FIB-SEM-based electron deposition of platinum “buttons” prior to standard lift-out and sharpening procedures for atom probe specimen manufacture. In combination, FIB-ToF-SIMS analysis and application of the “button” method ensure that even the smallest APT targets can be successfully captured in extracted needles.

Identifying and tackling recrystallization is a critical factor in the reliable radiocarbon (14C) dating of carbonates, since exogenous carbon can be incorporated and thus mask the real age of the samples. Vermetids are among the most important bioindicators used for paleo sea-level reconstruction, and the accuracy of their chronology can significantly impact sea-level curves. Age differences larger than 1 14C kyr before and after acid etching, combined with X-ray diffraction (XRD) analysis that indicates a significant amount of calcite still remains in the shell, led us to apply the previously developed carbonate density separation protocol (CarDS). Using a solution of sodium polytungstate, with density of 2.80 g/cm3, we successfully separated different carbonate fractions for a set of 10 vermetid samples from the coast of Rio de Janeiro, southeast of Brazil. Each separation was verified by XRD analysis and the 14C concentrations of different fractions were compared. The results show that the calcite fraction in the studied vermetid samples varied from 12 to 63% and aragonite fraction ages are up to 2 14C kyr older than the raw samples, thus confirming the efficacy of CarDS in removing young carbonates and the importance of density separation to vermetids prior to accelerator mass spectrometry (AMS) dating.

A new vacuum system for the preparation of graphite samples for radiocarbon (14C) measurement using an accelerator mass spectrometer (AMS) was constructed at the Dendrochronological Laboratory in AGH-UST Kraków. The central part of the system is a manual vacuum line for the production of graphite from carbon dioxide for subsequent AMS measurements. The graphitization system can handle up to five samples simultaneously, and the process lasts for approximately 1 hour. The graphitization line was built to support the preparation of wood samples for a project dedicated to dating a subfossil tree from the Younger Dryas period. For this purpose, the chemical preparation procedure for wood samples was optimized to obtain more reliable results. This includes the extraction of α-cellulose to increase the precision of the age determination. The performance of the system was tested with NIST OxII, IAEA standards (IAEA C3, C5, C6, and C8), and background samples. The results of the 13 samples of subfossil wood were tested and are presented. The methodology gives good reproducibility of results obtained for the samples prepared using this system.