Air-sensitive Samples Research Articles

Compact vacuum transfer devices for highly air-sensitive materials in scanning electron microscopy

Surface analysis experiments on air-sensitive substances are challenging to avoid their contact with air, leading to inaccurate results due to oxidation or hygroscopicity. To address this issue, we designed a compact vacuum transfer device (VTD) and applied it to scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) experiments. Our VTD features a split structure that can be opened and separated in the SEM specimen exchange chamber via magnetic control. This design allows the SEM manufacturer's stub to be fed directly into the SEM specimen chamber, preventing damage to the instrument's internal components and avoiding restrictions on specimen height. Additionally, the compact design maximizes the utilization of sample accommodation space. Besides, it can be flexibly customized in different sizes and types of stubs to adapt electron microscopes from various manufacturers. To confirm the reliability of our device, we applied it to several highly air-sensitive samples for morphology and chemical composition analysis by SEM and EDS. The EDS results showed that the atomic percentage of Na reaches 94.55 % after 14 minutes and 93.44 % after 30 minutes of storage when transferring metallic sodium. Furthermore, our VTD enables airtight recycling and re-transfer of samples after the SEM (-EDS) experiments. These results demonstrate that our device has excellent practicality and airtightness, making it suitable for medium- and long-distance sample transfer between laboratories on the campus.

Noble Dome: A Novel Air-Free Transfer System For Battery Research with Electron Microscopy

"Noble Dome: A Novel Air-Free Transfer System" introduces an innovative solution for loading air-sensitive samples into SEM/FIB instruments. Traditional loading methods expose samples to atmosphere during transfer, hindering investigations of reactive materials. The presented prototype, Noble Dome, directly attaches to the SEM/FIB, enabling sample transfer in an oxygen-free environment. The device's design and operational process are outlined, including airtight chambers, gas introduction, and modified venting systems. Experimental results demonstrate Noble Dome's effectiveness in preserving sample integrity. Compared to existing solutions, which often pose limitations, Noble Dome offers a practical approach for various research needs.Imaging and micromanipulation techniques such as Scanning Electron Microscopy (SEM) and Focused Ion Beam (FIB) can reveal critical information about the microstructure and composition of materials. To utilize these techniques, a sample must be loaded into the chamber of the instrument which is then pumped down to low vacuum conditions. In the process of removing a sample from its packaging and mounting it on the SEM/FIB stage, the sample is briefly exposed to atmosphere. This is problematic for researchers who are interested in investigating air sensitive samples or samples for which atmospheric contamination would detract from the investigation. This set of samples includes metals commonly used as battery materials such as lithium and sodium, which are highly reactive with elements in the air such as moisture or oxygen.We present a prototype for a glove box load lock that addresses this problem directly. This device attaches directly onto the side of a SEM/FIB and allows researchers to remove a sample from packaging and transfer it directly on the stage via an accessory port of the SEM/FIB in an oxygen-free environment and then pump the tool down to vacuum without any atmospheric exposure in the process, eliminating the use of an intermediary shuttle from a separate glove box. We call this device Noble Dome.In order to test Noble Dome’s ability to protect samples from atmosphere, we imaged and collected EDS spectra on the same location of a lithium metal sample in a pristine state, after sitting in Noble Dome for 30 minutes, and after sitting in atmosphere for 30 minutes.We note that there was very little change in the surface topography and oxygen counts between the sample in its pristine state and the sample after sitting in Noble Dome for 30 minutes. However, there is a marked increase in surface oxidation and topography after the sample sat in atmosphere for 30 minutes.Lithium-ion batteries are increasingly prolific in the landscape of modern technology. In order to improve the energy density, life cycle and safety of lithium-ion batteries, researchers require significant amounts of materials characterization pre-assembly, post-assembly and after several charge/discharge cycles. Electron microscopy is crucial for effective materials characterization, which necessitates a solution for loading samples into the vacuum chamber of the microscope without exposing these reactive samples to air.Other solutions currently on the market for loading air sensitive samples into a SEM/FIB involve manipulating the sample in a glove box which is separate from the instrument, loading the sample into an inert gas transfer shuttle which is closed by remote control, removing the shuttle from the glovebox, loading the shuttle into the SEM/FIB, and then opening the sample again via remote control. These solutions are not ideal because they're very expensive, have a variety of limitations on sample size, stage travel, and signal strength, and are high tech solutions prone to costly malfunction. These drawbacks highlight the demand for a more practical and efficient approach.The presented prototype, Noble Dome, addresses the challenge of loading air-sensitive samples into SEM/FIB instruments with a practical and innovative approach. The device eliminates the need for an intermediary glove box and inert gas transfer shuttle, allowing direct sample transfer onto the stage in an oxygen-free environment. The results demonstrate Noble Dome's efficacy in preserving sample integrity by minimizing atmospheric exposure, as evidenced by the minimal changes observed in surface topography and composition compared to samples exposed to atmosphere. Noble Dome enables research on reactive samples, used to pursue a carbon-free future. Figure 1

A method for rheological measurements of air sensitive samples.

The rheology of air or moisture sensitive liquids, gels, and glasses requires complicated rheometer-in-glovebox laboratory setups. Here, we demonstrate the use of a heavier-than-air cover gas, sulfur hexafluoride, and the design of a cover gas container that can attach to the lower geometry plate of any rheometer to carry out rheology experiments on air-sensitive liquids and soft solids. Rheological measurements of air-reactive ionic liquid trimethylsulfonium bromide-AlCl3, moisture sensitive titanium(IV) propoxide, and glycerin demonstrate the effectiveness of the cover-gas method for loading samples on acquiring correct temperature dependent viscosity data of the sample in the absence of reaction products.

Glovebox-assisted magnetic force microscope for studying air-sensitive samples in a cryogen-free magnet.

Most known two-dimensional magnets exhibit a high sensitivity to air, making direct characterization of their domain textures technically challenging. Herein, we report on the construction and performance of a glovebox-assisted magnetic force microscope (MFM) operating in a cryogen-free magnet, realizing imaging of the intrinsic magnetic structure of water and oxygen-sensitive materials. It features a compact tubular probe for a 50 mm-diameter variable temperature insert installed in a 12T cryogen-free magnet. A detachable sealing chamber can be electrically connected to the tail of the probe, and its pump port can be opened and closed by a vacuum manipulator located on the top of the probe. This sealing chamber enables sample loading and positioning in the glove box and MFM transfer to the magnet maintained in an inert gas atmosphere (in this case, argon and helium gas). The performance of the MFM is demonstrated by directly imaging the surface (using no buffer layer, such as h-BN) of very air-sensitive van der Waals magnetic material chromium triiodide (CrI3) samples at low temperatures as low as 5K and high magnetic fields up to 11.9T. The system's adaptability permits replacing the MFM unit with a scanning tunneling microscope unit, enabling high-resolution atomic imaging of air-sensitive surface samples.

Glovebox coupled TEM – a new method for versatile investigations of air-sensitive samples

Glovebox coupled TEM – a new method for versatile investigations of air-sensitive samples

Battery Materials: In-Situ Analysis with the Scanning Electron Microscope

The concept of decarbonisation has been gradually gaining ground. As a result, emphasis has been given to green energy technology in an attempt to offset the need for fossil fuels. The alternative to fossil fuels could be batteries. Not only can batteries be used for stationary energy storage but also for powering electric vehicles. However, more is increasingly required from batteries: they have to store more energy, perform reliably and function for longer, often under extreme conditions depending on the latitude. Among the different battery technologies that have been developed over the years, lithium ion batteries stand out. The main reason is their superior energy and power density, which can support demanding applications such as electromobility. The drive to make batteries more efficient and able to hold more energy, and eventually deliver more power requires in-depth analysis of materials; in order to understand what promotes or undermines materials performance, what leads to failure, and ultimately, the knowledge to design materials for the next generation of batteries.The scanning electron microscope is a powerful tool supporting in situ analysis of materials. In the short-term, as far as cathode precursor powders are concerned, costs are reduced by early detection of impurities and contamination. In the long-term, the battery quality and performance are safeguarded as failure caused by the presence of contaminants is minimised (contamination particles cause short-circuits by penetrating through the battery components). Scanning electron microscope(SEM)-based quality assurance/quality control of battery powders is routinely done with energy dispersive spectroscopy (EDS) and comes with the advantage of high throughput and minimum instrument down time.Battery materials analysis often focuses on formulation testing. That can be either at the industrial level (enquiring if the result is the intended) or R&D level, that is, experimenting with different recipes to single out the optimal one(s). One of the aspects that can be checked using SEM-based analytical techniques is the composition and distribution of coatings and dopants on the powder particle surface. The addition of coatings (Figure 1A) and dopants (Figure 1B) is crucial to ensuring battery performance. They act as performance enhancers (coatings) and dendrite formation suppressants (dopants). These can be detected and mapped in high resolution with SEM-EDS and they can be analysed more accurately with SEM-WDS. At a later stage, the same techniques can be applied to analyse black mass, the material coming from shredded, spent batteries.Given that the atomic numbers (Z) of the elements comprising the battery powders are often close, there is a limit to the information that an electron image can provide due to the closeness of the grey levels. However, there is need to characterise the internal structure of precursor cathode powders as well as other properties such as shape, size, grain boundaries and texture. SEM-EBSD can bypass this issue and can provide information about the particle internal structure by utilising backscattered electrons. The internal structure information of the particles can be used to study cracking development and propagation. A useful tool for battery components post-mortem analysis. The incorporation the Raman-in-SEM, RISE system provides an additional dimension to battery analysis, meaning we can access a wealth of molecular information. Raman spectroscopy can be employed to aid with the analysis of lithium-containing cathode materials in addition to investigating graphitic carbon anode materials.The primary benefit of the SEM-based techniques briefly discussed here is that they can all be applied in the same SEM chamber, in situ, allowing for data to be obtained under the same conditions as part of the same experiment/workflow, promoting, thus, efficiency and throughput – even more so for beam and/or air sensitive samples, saving time required for sample (re)preparation. Another practical benefit is straightforward data correlation which is facilitated when the exact same sample locations have been analysed. Figure 1

A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples

We report a compact laboratory-based, high resolution X-ray emission spectrometer installed in a glovebox for simultaneous measurement of phosphorus Kα and Kβ spectra of air-sensitive materials.

A sample holder for simultaneous neutron and dielectric spectroscopy – dielectric tests with glycerol, glycerol-water, water and phosphoric acid

We report on dielectric test measurements of a rectangular flat sample holder which serves as capacitor and which is aimed for simultaneous neutron and dielectric (n-DE) spectroscopy of acidic liquid samples. We describe technical details of the sample holder assembly and the dielectric and neutron equipment as well as the sample preparation procedure of the air sensitive acidic samples. The sample holder was characterised off-line from the neutron spectrometer by dielectric spectroscopy, but using the standard IN16B cryofurnace with a dielectric sample stick with 4-wire connection and a Novocontrol equipment, previously setup by a collaborative effort between ILL and Roskilde University. Temperature-dependent dielectric scans on standard samples (glycerol, glycerol-water, and Milli-Q water) were measured in the frequency range between 0.27 Hz and 1 MHz. Step-like temperature changes allowed to probe the temperature equilibrium conditions and continuous temperature changes were made to mimic typical IN16B backscattering neutron fixed window scans. Both type of scans were carried out in cooling and in heating. The standard samples show that our dielectric setup with flat sample holder is well suited for simultaneous n-DE-experiments. On the other hand, the dielectric scan on phosphoric acid reveals the limitations of our setup in case of high sample conductivities, but also shows that the DC-conductivity can still be accessed in a sufficiently wide low temperature range where the onset of conductivity can be simultaneously probed with the change in proton dynamics as seen by neutron spectroscopy.

Enabling LIFDI-MS measurements of highly air sensitive organometallic compounds: a combined MS/glovebox technique.

A new setup combining a ThermoFisher Exactive Plus Orbitrap Mass Spectrometer with a liquid injection field desorption ionization (LIFDI) source directly connected to an inert atmosphere glovebox is presented. The described setup allows for the analysis of very air- and moisture sensitive samples. Furthermore, the soft nature of LIFDI ionization gives access to the molecular ions of fragile molecules. This new setup is therefore especially useful for sensitive organometallic complexes. The functionality of the new setup is tested against [(Cp)2TiCl]˙, which is known for its notorious sensitivity to air and moisture. Its drastic colour change from green to orange upon exposure to air further supports the easy detection of traces of oxygen during the experiment. In addition, we applied this setup to the mass spectrometric analysis of the qualitative composition of a Cu/Al cluster mixture, which is not accessible by other analytical methods.

Design of a Sample Transfer Holder to Enable Air-Free X-ray Photoelectron Spectroscopy

Surface analysis of air-sensitive samples is difficult without controlled-environment sample transfer tubes or expensive vacuum transfer suitcases. Through the use of vacuum sealing and commercial ...

Charge Transport Study of in-Situ Cesium Doped Monolayer Graphene

Modifying graphene with surface adsorbates is a widely studied way of modifying graphene’s electronic properties. Different graphene/adatom systems have shown that it is possible to open a band gap in graphene1, engineer topological insulators2 and create magnetic moments3. The atomic thickness of graphene maximizes the effect of adsorbates, enabling chemical sensors that achieve single molecule sensitivity4. Alkali metal adatoms are a particularly efficient dopant for graphene due to their high electronegativity. Lithium/graphene systems have been studied for in the context of low-dimensional superconductivity5 and achieving ultrafast diffusion of lithium6 for battery applications.However, doping graphene with alkali metal adatoms bears challenges. Experiments with alkali metals must be conducted in an ultra-high vacuum or inert gas environment due to the high reactivity of the alkali. Alkali metal adsorbed graphene is not air stable, which imposes limits on the available characterization methods. An impurity free graphene surface must be achieved prior to adsorption to achieve efficient adsorption and avoid unwanted parasitic reactions. This problem is particularly acute for graphene samples prepared by the use of polymer handles. Alkali metal atoms can also intercalate under the graphene layer depending on substrate and sample preparation conditions. Moreover, it is possible for adatoms to form clusters on graphene surface7which negatively impacts both doping uniformity and efficiency.In this work, we report a new method of alkali doping of graphene to reach ultra-high doping (~1014cm-2) for charge transport studies beyond the limit of ionic liquid gating. We work with chemical vapor deposition grown graphene transferred onto quartz substrates. Quartz is the substrate of choice due to its chemical inertness and optical transparency, with the latter enabling non-invasive Raman spectroscopy through the substrate. Micron scale graphene devices were prepared using lithography-based methods and the samples were thermally annealed in a nitrogen glove box environment to desorb water prior to alkali doping. The graphene was subsequently exposed to cesium vapor at different temperatures using a flip-chip method that allows hermetic sealing of the air sensitive samples in an inert gas environment with a liquid cesium source of cesium vapour. We measured the in-situ variation of graphene resistivity as cesium atoms are adsorbed onto the graphene surface, and resistivity is modulated by charge transfer doping. Evidence of ultra-high doping is shown via Raman spectroscopy performed through the quartz substrate window, with G-peak shifts from 1589 cm-1 up to 1608 cm-1. Hall measurements in-situ further confirm the strong doping. We measured the electronic transport properties of cesium doped graphene at temperatures as low as 1.2 K and under magnetic fields up to 7 T. Weak-localization, magnetoresistance and Hall resistance are measured and analyzed. 1. Elias, D. C.; Nair, R. R.; Mohiuddin, T. M.; Morozov, S. V.; Blake, P.; Halsall, M. P.; Ferrari, A. C.; Boukhvalov, D. W.; Katsnelson, M. I.; Geim, A. K.; Novoselov, K. S., Control of graphene's properties by reversible hydrogenation: evidence for graphane. Science 2009, 323 (5914), 610-3.2. Weeks, C.; Hu, J.; Alicea, J.; Franz, M.; Wu, R., Engineering a Robust Quantum Spin Hall State in Graphene via Adatom Deposition. Physical Review X 2011, 1 (2).3. Hong, X.; Zou, K.; Wang, B.; Cheng, S. H.; Zhu, J., Evidence for spin-flip scattering and local moments in dilute fluorinated graphene. Phys Rev Lett 2012, 108 (22), 226602.4. Schedin, F.; Geim, A. K.; Morozov, S. V.; Hill, E. W.; Blake, P.; Katsnelson, M. I.; Novoselov, K. S., Detection of individual gas molecules adsorbed on graphene. Nat Mater 2007, 6 (9), 652-5.5. Profeta, G.; Calandra, M.; Mauri, F., Phonon-mediated superconductivity in graphene by lithium deposition. Nat Phys 2012, 8 (2), 131-134.6. Kühne, M.; Paolucci, F.; Popovic, J.; Ostrovsky, P. M.; Maier, J.; Smet, J. H., Ultrafast lithium diffusion in bilayer graphene. Nat Nanotechnol 2017, 12, 895.7. Fan, X.; Zheng, W. T.; Kuo, J. L.; Singh, D. J., Adsorption of single Li and the formation of small Li clusters on graphene for the anode of lithium-ion batteries. ACS Appl Mater Interfaces 2013, 5 (16), 7793-7.

Sample seal-and-drop device and methodology for high temperature oxide melt solution calorimetric measurements of PuO2

Thermodynamic properties of refractory materials, such as standard enthalpy of formation, heat content, and enthalpy of reaction, can be measured by high temperature calorimetry. In such experiments, a small sample pellet is dropped from room temperature into a calorimeter operating at high temperature (often 700 °C) with or without a molten salt solvent present in an inert crucible in the calorimeter chamber. However, for hazardous (radioactive, toxic, etc.) and/or air-sensitive (hygroscopic, sensitive to oxygen, pyrophoric, etc.) samples, it is necessary to utilize a sealed device to encapsulate and isolate the samples, crucibles, and solvent under a controlled atmosphere in order to prevent the materials from reactions and/or protect the personnel from hazardous exposure during the calorimetric experiments. We have developed a sample seal-and-drop device (calorimetric dropper) that can be readily installed onto the dropping tube of a calorimeter such as the Setaram AlexSYS Calvet-type high temperature calorimeter to fulfill two functions: (i) load hazardous or air-sensitive samples in an air-tight, sealed container and (ii) drop the samples into the calorimeter chamber using an "off-then-on" mechanism. As a case study, we used the calorimetric dropper for measurements of the enthalpy of drop solution of PuO2 in molten sodium molybdate (3Na2O·4MoO3) solvent at 700 °C. The obtained enthalpy of -52.21 ± 3.68 kJ/mol is consistent with the energetic systematics of other actinide oxides (UO2, ThO2, and NpO2). This capability has thus laid the foundation for thermodynamic studies of other Pu-bearing phases in the future.

Electronic and Magnetic Properties of Black Phosphorus

Black phosphorus (bP) has emerged as the next member in the graphene inspired two‐dimensional materials family. Its electronic and magnetic properties are studied herein using electron and nuclear magnetic resonance techniques (ESR and NMR) and microwave conductivity measurement. The latter is a unique technique to study conductivity on air sensitive samples. The ESR study indicates the absence of free charge carriers and no sign of paramagnetic defects are found. 31P NMR shows the presence of a characteristic Pake doublet structure due to the interaction between I = 1/2 nuclei. Microwave conductivity shows, in accordance with the ESR results, that black phosphorus behaves as a semiconductor and we identify extrinsic and intrinsic charge carrier contributions to the conductivity and extracted the sizes of the gaps. ESR measurement also yields that bP might find applications as a microwave absorbent.

Low-profile self-sealing sample transfer flexure box.

A flexural bearing mechanism has enabled the development of a self-sealing box for protecting air sensitive samples during transfer between glove boxes, micro-machining equipment, and microscopy equipment. The simplicity and self-actuating feature of this design makes it applicable to many devices that operate under vacuum conditions. The models used to design the flexural mechanism are presented in detail. The device has been tested in a Zeiss Merlin GEMINI II scanning electron microscope with Li3PS4 samples, showing effective isolation from air and corrosion prevention.

Low cost apparatus for rapid boiling point determination of small air sensitive samples under inert atmosphere

The boiling point is a characteristic property of substances and mixtures. We have developed a new low cost apparatus which uses standard Schlenk technique for measuring the boiling point of small samples (<0.2ml) under inert atmosphere.

Interferometrically stable, enclosed, spinning sample cell for spectroscopic experiments on air-sensitive samples.

In experiments with high photon flux, it is necessary to rapidly remove the sample from the beam and to delay re-excitation until the sample has returned to equilibrium. Rapid and complete sample exchange has been a challenge for air-sensitive samples and for vibration-sensitive experiments. Here, a compact spinning sample cell for air and moisture sensitive liquid and thin film samples is described. The principal parts of the cell are a copper gasket sealed enclosure, a 2.5 in. hard disk drive motor, and a reusable, chemically inert glass sandwich cell. The enclosure provides an oxygen and water free environment at the 1 ppm level, as demonstrated by multi-day tests with sodium benzophenone ketyl radical. Inside the enclosure, the glass sandwich cell spins at ≈70 Hz to generate tangential speeds of 7-12 m/s that enable complete sample exchange at 100 kHz repetition rates. The spinning cell is acoustically silent and compatible with a ±1 nm rms displacement stability interferometer. In order to enable the use of the spinning cell, we discuss centrifugation and how to prevent it, introduce the cycle-averaged resampling rate to characterize repetitive excitation, and develop a figure of merit for a long-lived photoproduct buildup.

Portable ultrahigh-vacuum sample storage system for polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy

A portable ultrahigh-vacuum sample storage system was designed and built to investigate the detailed geometric structures of mass-selected metal clusters on oxide substrates by polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy (PTRF-XAFS). This ultrahigh-vacuum (UHV) sample storage system provides the handover of samples between two different sample manipulating systems. The sample storage system is adaptable for public transportation, facilitating experiments using air-sensitive samples in synchrotron radiation or other quantum beam facilities. The samples were transferred by the developed portable UHV transfer system via a public transportation at a distance over 400 km. The performance of the transfer system was demonstrated by a successful PTRF-XAFS study of Pt4 clusters deposited on a TiO2(110) surface.

Thin-film encapsulation of the air-sensitive organic-based ferrimagnet vanadium tetracyanoethylene

The organic-based ferrimagnet vanadium tetracyanoethylene (V[TCNE]x∼2) has demonstrated potential for use in both microwave electronics and spintronics due to the combination of high temperature magnetic ordering (TC &amp;gt; 600 K), extremely sharp ferromagnetic resonance (peak to peak linewidth of 1 G), and low-temperature conformal deposition via chemical vapor deposition (deposition temperature of 50 °C). However, air-sensitivity leads to the complete degradation of the films within 2 h under ambient conditions, with noticeable degradation occurring within 30 min. Here, we demonstrate encapsulation of V[TCNE]x∼2 thin films using a UV-cured epoxy that increases film lifetime to over 710 h (30 days) as measured by the remanent magnetization. The saturation magnetization and Curie temperature decay more slowly than the remanence, and the coercivity is unchanged after 340 h (14 days) of air exposure. Fourier transform infrared spectroscopy indicates that the epoxy does not react with the film, and magnetometry measurements show that the presence of the epoxy does not degrade the magnetic properties. This encapsulation strategy directly enables a host of experimental protocols and investigations not previously feasible for air-sensitive samples and lays the foundation for the development of practical applications for this promising organic-based magnetic material.

Advanced Crystallographic Program at ChemMatCARS at Advanced Photon Source

ChemMatCARS, a state-of-the-art synchrotron-based national facility for Chemistry and Materials Science located at the Advanced Photon Source (APS), maintains dedicated advanced crystallographic programs for small molecule which include photo-crystallography, high resolution charge density studies, high pressure (&lt;10 GPa) chemical crystallography using a diamond anvil cell(DAC), ultra-low temperature crystallography using open flow Helium at ~10 K, and element-specific resonant diffraction and diffraction anomalous fine structure (DAFS) (tunable energy from 5 to 70 keV). High throughput micro-crystallography benefits from a new sample preparation environment and a fast data collection strategy to enable measurements on air-sensitive samples in fewer than 5 minutes. This work is typically done by cooling the sample with cryogenic open flow nitrogen or helium. These new capabilities will impact the development of new materials to meet emerging challenges in energy, environment and life sciences. This poster focuses on the above scientific research activities and provides information on how to apply for beam time.

Gas cell for in situ soft X-ray transmission-absorption spectroscopy of materials

A simple gas cell design, constructed primarily from commercially available components, enables in situ soft X-ray transmission-absorption spectroscopy of materials in contact with gas at ambient temperature. The cell has a minimum X-ray path length of 1 mm and can hold gas pressures up to ~300 Torr, and could support higher pressures with simple modifications. The design enables cycling between vacuum and gas environments without interrupting the X-ray beam, and can be fully sealed to allow for measurements of air-sensitive samples. The cell can attach to the downstream port of any appropriate synchrotron beamline, and offers a robust and versatile method for in situ measurements of certain materials. The construction and operation of the cell are discussed, as well as sample preparation and proper spectral analysis, illustrated by examples of spectral measurements. Potential areas for improvement and modification for specialized applications are also mentioned.