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Automatic equipment for sampling and preparing gases by dual column gas chromatography for subsequent mass spectral analysis of carbon isotopes during methane metabolism
Analyzing the phosphoproteome at nanoscale poses a significant challenge, mainly due to the substantial sample loss from non-specific surface adsorption during the enrichment of low stoichiometric phosphopeptides. Here, we describe a tandem tip-based phosphoproteomics sample preparation method capable of sequential sample cleanup and enrichment without the need for additional sample transfer, thereby minimizing sample loss. Integration of this method to our recently developed SOP (Surfactant-assisted One-Pot sample preparation) and iBASIL (improved Boosting to Amplify Signal with Isobaric Labeling) approaches creates a streamlined workflow, enabling sensitive, high-throughput nanoscale phosphoproteomics measurements.
Detailed understanding between microstructure evolution and mechanical properties is important for designing new high burnup nuclear fuels. In this presentation we discuss the use of picosecond ultrasonics to measure localize changes in mechanical properties of fuel surrogates. We develop measurement techniques that can be applied to investigate heterogeneous elastic properties caused by localize changes in chemistry, grain microstructure caused by recrystallization, and mechanical properties of small samples prepared using focused ion beam sample preparation. Emphasis is placed on understanding the relationship between microstructure and mechanical properties
The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.
Plant–microbe interactions are of rising interest in plant sustainability, biomass production, plant biology, and systems biology. These interactions have been a challenge to detect until recent advancements in mass spectrometry imaging. Plants and microbes interact in four main regions within the plant, the rhizosphere, endosphere, phyllosphere, and spermosphere. This mini review covers the challenges within investigations of plant and microbe interactions. We highlight the importance of sample preparation and comparisons among time-of-flight secondary ion mass spectroscopy (ToF-SIMS), matrix-assisted laser desorption/ionization (MALDI), laser desorption ionization (LDI/LDPI), and desorption electrospray ionization (DESI) techniques used for the analysis of these interactions. Using mass spectral imaging (MSI) to study plants and microbes offers advantages in understanding microbe and host interactions at the molecular level with single-cell and community communication information. More research utilizing MSI has emerged in the past several years. We first introduce the principles of major MSI techniques that have been employed in the research of microorganisms. An overview of proper sample preparation methods is offered as a prerequisite for successful MSI analysis. Traditionally, dried or cryogenically prepared, frozen samples have been used; however, they do not provide a true representation of the bacterial biofilms compared to living cell analysis and chemical imaging. New developments such as microfluidic devices that can be used under a vacuum are highly desirable for the application of MSI techniques, such as ToF-SIMS, because they have a subcellular spatial resolution to map and image plant and microbe interactions, including the potential to elucidate metabolic pathways and cell-to-cell interactions. Promising results due to recent MSI advancements in the past five years are selected and highlighted. The latest developments utilizing machine learning are captured as an important outlook for maximal output using MSI to study microorganisms.
Cu-ferrite nanoparticles were synthesized by co-precipitation method and were annealed at different temperatures ranging from 400 to l000°C in air for 4 hours. The as-prepared sample and the sample annealed at 400°C showed small peaks of cubic Cu-ferrite in X-ray diffraction studies. For the intermediate temperature 600°C, some additional peaks of α-Fe{sub 2}O{sub 3} were observed. As the annealing temperature increased further only tetragonal Cu-ferrite peaks were observed. In all the samples some traces of CuO was noted. Grain size was increased from 2lnm for the as prepared sample to 42nm for the sample annealed at l000°C. Spontaneous magnetization value was found to be very small for the as prepared sample and it was increased monotonically with the increase in annealing temperature. Maximum magnetization of 29.7emu/g was observed at 300K for the sample annealed at l000°C. The remanent magnetization was increased with the increase in annealing temperature up to 900°C and then decreased whereas for the coercivity a peak was observed for the sample annealed at 800°C. The highest coercivity of l402 Oe was observed at 300K for the sample annealed at 800°C. As the measurement temperature decreased from 300K to 60K, magnetization and coercivity values were increased. The observed magnetic behaviour may be understood on the basis of phase transformation, grain growth with the increase in annealing temperature and reduced thermal energy at low measurement temperature.
The Saltstone Production Facility (SPF) built two new Saltstone Disposal Units (SDU), SDU 3 and SDU 5, in 2013. The variable frequency drive (VFD) for the grout transfer hose pump tripped due to high current demand by the motor during the initial radioactive saltstone transfer to SDU 5B on 12/5/2013. This was not observed during clean cap processing on July 5, 2013 to SDU 3A, which is a slightly longer distance from the SPF than is SDU 5B. Saltstone Design Authority (SDA) is evaluating the grout pump performance and capabilities to transfer the grout processed in SPF to SDU 3/5. To assist in this evaluation, grout physical properties are required. At this time, there are no rheological data from the actual SPF so the properties of laboratory prepared samples using simulated salt solution or Tank 50 salt solution will be measured. The physical properties of grout prepared in the laboratory with de-ionized water (DI) and salt solutions were obtained at 0.60 and 0.59 water to premix (W/P) ratios, respectively. The yield stress of the DI grout was greater than any salt grout. The plastic viscosity of the DI grout was lower than all of the salt grouts (including salt grout with admixture). When these physical data were used to determine the pressure drop and fluid horsepower for steady state conditions, the salt grouts without admixture addition required a higher pressure drop and higher fluid horsepower to transport. When 0.00076 g Daratard 17/g premix was added, both the pressure drop and fluid horsepower were below that of the DI grout. Higher concentrations of Daratard 17 further reduced the pressure drop and fluid horsepower. The uncertainty in the single point Bingham Plastic parameters is + 4% of the reported values and is the bounding uncertainty. Two different mechanical agitator mixing protocols were followed for the simulant salt grout, one having a total mixing time of three minutes and the other having a time of 10 minutes. The Bingham Plastic parameters were essentially the same for the salt grout without admixture. When Daratard 17 was added, the Bingham Plastic yield stress increased for the 10 minute mix. The simulant salt used in this task had similar physical properties of the Tank 50 3Q13 salt grout and is recommended for future use, if the salt solution in Tank 50 does not change. The design basis physical properties used to size the pumps and mixers at SPF were obtained from DPST-85-312. The grouts characterized in this report are bounded by the design basis density and Bingham Plastic yield stress. The opposite is true for the plastic viscosity. Steady state pressure drop calculations were performed for the design basis values using the flow rate for the clean cap and salt grouts and they bound the pressure drop of the grouts characterized in this report. A comparison of the lab prepared samples to PI ProcessBook data, specifically average pressure drop, indicate that the lab prepared samples are more viscous in nature than what is processed in the facility. This difference could be due to the applied shear rates which could be lower in the lab as compared to the facility and that fact the SPF added flush water, making this comparison more difficult. A perfunctory review of the PI ProcessBook data was discussed. It may be possible that the frequency that the distributed control system alters the grout pump speed to maintain grout hopper volume can negatively affect the efficiency of the grout pump.
The ETF ammonia tolerant grout waste form was developed by the Vitreous State Laboratory (VSL) to stabilize ammonium and thereby prevent emission of ammonia vapor during solidification of an ammonium-rich, concentrated sodium sulfate aqueous waste stream generated at the Hanford Effluent Treatment Facility (ETF). VSL personnel did not observe expansion in samples prepared during the waste form development work. However, Savannah River National Laboratory (SRNL) personnel detected expansion, in a few ETF grout samples, up to ~ 20 percent vertical expansion, while preforming work scope to evaluate the effect of ETF brine compositional ranges on the precipitation and solidification processes. The initial work requests can be found in Washington River Protection Services (WRPS) Statement of Work (SOW, Requisitions #: 339922 Revisions 0 and 1, March 11, 2021, and November 2021, respectively. As a result of the waste form expansion observed by SRNL, additional evaluation was requested by WRPS SOW Requisitions #: 356730 Revision 0 and Revision 1, February 1, 2022, and July 11, 2022, respectively. The goal of these requests was to determine whether differences in the slags and / or in sample preparation protocols used by VSL and SRNL were the cause of the expansion observed in the SRNL samples. G. Chen, WRPS, arranged a materials exchange between VSL and SRNL and coordinated the VSL protocol(s) for grouting and curing 1L batches of Base Case ETF base case simulant. Materials were exchanged between VSL and SRNL. Both laboratories performed the VSL struvite precipitation-solidification protocol and cured samples for at least 28 days. Differences in VSL and SRNL slag compositions, mineralogy and particle size results in themselves or combined were determined to not be the cause of the expansion because all samples expanded regardless of whether the VSL or SRNL slags were used. The fundamental cause of the observed expansion could not be attributed to minor variations in the following: 1) chemistry of the slag and other reagents, 2) container wall thickness, 3) ambient bench top curing conditions at VSL and SRNL, 4) pH adjustments to 7 ± a few tenths of unit, nor 5) stirring time between the precipitation and solidification process steps. Additional observations include: grout samples prepared with VSL slag expanded less than those prepared with the SRNL slag and, based on a very limited sample set, some samples stirred for longer times expanded less than those stirred for 20 minutes.
Highlights: • The native fibrous outer and dense inner C-S-H structure are preserved by using low energy argon broad ion beam sectioning. • Possible artefacts of the preparation and imaging of hydrated alite are shown and discussed. • An approach for a semi automated pore analysis of the obtained high resolution images is demonstrated. Scanning electron microscopy (SEM) imaging is able to visualize micro- to nano-structures of cement and concrete. A prerequisite is that the sample preparation preserves the native structure of the specimen. In this study, argon broad ion beam (BIB) sectioning is compared to state-of-the-art sample preparation (resin embedding, polishing) for hydrated alite. Additionally, it is investigated if during BIB, sample cooling is beneficial to avoid deterioration of cement hydrates. The aim is to quantitatively measure pore size distributions in hardened alite pastes. Therefore, not only optimized sample preparation but also optimized imaging conditions are investigated. Finally, it is demonstrated that by image analysis pores down to a diameter of 5 nm in hydrated alite pastes can be quantitatively analysed.
In this study, thermoluminescence dosimetry material of carbon doped aluminium oxide by combustion method using Aluminium nitrate and Glycine. The Structure of the prepared Sample was carried out by XRD. The sample was nano crystalline in nature. Having hexagonal structure with unit cell parameters a=4.75Å, C=12.99Å. The surface morphology of the prepared nanopowder was carried out through (SEM). The morphology of the prepared sample is platelet structure and functional group analysis carried out through FT-IR Spectrum. The prepared sample was irradiated through γ-ray CO{sup 60} (100 Gy) was used as γ-ray source. The thermoluminescence glow curve of the irradiated sample showed an isolated peak at around 200°C. The result suggest the prepared nanopowder is suitable for medical radiation dosimetry.
In this work, solid solutions of Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (where x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0) ferrite nanoparticles were synthesized using the novel combustion method. A powder X-ray diffraction study confirms the formation of spinel-structured Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4}. Unusual increases in the lattice constant were observed from 8.358 to 8.435 Å for Zn substitution. Raman spectra show the change in local environment of tetrahedral and octahedral symmetry. Field emission scanning electron microscopy images show that the prepared samples are nanosized and there is not much difference observed in surface morphology. A magnetic study reveals that the prepared samples exhibit superparamagnetic properties with negligible coercivity and the saturation magnetizations initially increase from 31.12 emu g{sup −1} (x = 0) to 35.48 emu g{sup −1} (x = 0.2) and then decrease for further Zn substitution at 300 K. The zero-field-cooled and field-cooled magnetization studies confirm the superparamagnetic nature of prepared samples, and the observed blocking temperature decreases from 146.05 to 32.3 K. At 20 K, the measured hysteresis loop shows the coercivity and it gradually decreases from 810 to 152 Oe. The obtained results suggest that the prepared superparamagnetic Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} ferrite nanoparticles are a promising candidate material for biomedical applications.
M-type aluminum doped SrFe{sub 10}Al{sub 2}O{sub 19} were synthesized via co-precipitation method using cetyltrimethyl ammonium bromide (CTAB) as a surfactant. The effects of CTAB content (x = 0, 1, 3, and 9 wt. %) on the formation, structure, morphology, magnetic, and dielectric properties of the SrFe{sub 10}Al{sub 2}O{sub 19} nanoparticles were investigated. X-ray diffraction results show elimination of α-Fe{sub 2}O{sub 3} phase from samples prepared using CTAB. Morphological changes including grain and crystallite size was noticed with the increase in the CTAB content. With the increase in CTAB, powder particles grew in hexagonal plates. A linear increase in saturation magnetization, Ms, with CTAB content was observed from 56.5 emu/g at 0% CTAB to 66.4 emu/g at 9% CTAB. This is a net increase of 17.5% in Ms. The coercivity (Hc ∼ 5700 Oe) of sample reached maximum at 1% CTAB and reduced with further CTAB content reaching to a minimum value of 4488 Oe at 9% CTAB. A slight increase in Curie temperature (735 K) was also observed for samples synthesized using CTAB as compared to that of sample prepared in the absence of CTAB (729 K). Samples synthesized with CTAB show higher dielectric constants as compared to samples prepared without CTAB, while dielectric constant for all samples show decrease in value with the increase in frequency. These results imply that CTAB may act as a crystallization master, controlling the nucleation and growth of SrFe{sub 10}Al{sub 2}O{sub 19} crystal. The study delineates the scope of improving magnetic properties of ferrites without substitution of metal ions.
Yb{sup 3+},Er{sup 3+},Eu{sup 3+} triply-doped in YVO{sub 4} with varying molar ratio of Er/Eu were synthesized in a sol–gel method with a subsequent heat treatment for the first time. The optimal molar ratio of Er/Eu for the maximum energy transfer efficiency was 1/39. After molar ratio, the influences of different heat treatment temperatures were also researched and the maximal heat temperature was 1300 °C. Besides, the properties of YVO{sub 4}:Yb{sup 3+},Er{sup 3+},Eu{sup 3+} upconversion phosphors were investigated by X-ray diffraction, scanning electron microscopy and photo luminescent spectra, respectively. In sum, XRD results indicate the crystal structure of as-prepared samples, which is the tetragonal phase of YVO{sub 4} with no other diffraction peaks. SEM images show the morphology of as-prepared samples, which are granular-like nanoparticles. PL spectra demonstrate the upconversion luminescence of as-prepared samples, which emit strong green lights (at 525 nm, 550 nm) and slight red lights (at 590 nm, 615 nm, 695 nm) under the NIR irradiation at 980 nm. Two strong green emissions are attributed to the {sup 2}H{sub 11/2}→{sup 4}I{sub 15/2} and {sup 4}S{sub 3/2}→{sup 4}I{sub 15/2} transitions of Er{sup 3+} ions. Meanwhile, three slight red emissions are attributed to the {sup 5}D{sub 0}→{sup 7}F{sub 1}, {sup 5}D{sub 0}→{sup 7}F{sub 2} and {sup 5}D{sub 0}→{sup 7}F{sub 4} transitions of Eu{sup 3+} ions. All in all, the colorful emissions endow YVO{sub 4}:Yb{sup 3+},Er{sup 3+},Eu{sup 3+} phosphors great potential for some applications, such as display devices, bio-labeling and infrared detection.
Herein, we report on the preparation, structure, and magnetic characterization of FeCoCu nanowire arrays grown by DC electrodeposition inside self-assembled ordered nanopores of anodic aluminum oxide templates. A systematic study of their structure has been performed both in as-prepared samples and after annealing in the temperature range up to 800 °C, although particular attention has been paid to annealing at 700 °C after which maximum magnetic hardening is achieved. The obtained nanowires have a diameter of 40 nm and their Fe{sub 0.28}Co{sub 0.67}Cu{sub 0.05} composition was confirmed by energy dispersive X-ray spectroscopy (EDS). Focused ion-beam lamellas of two samples (as-prepared and annealed at 700 °C) were prepared for their imaging in the high-resolution transmission electron microscopy (HRTEM) perpendicularly to the electron beam, where the obtained EDS compositional mappings show a homogeneous distribution of the elements. X-ray diffraction analysis, and selected area electron diffraction (SAED) patterns confirm that nanowires exhibit a bcc cubic structure (space group Im-3m). In addition, bright-dark field images show that the nanowires have a polycrystalline structure that remains essentially the same after annealing, but some modifications were observed: (i) an overall increase and sharpening of recrystallized grains, and (ii) an apparent shrinkage of the nanowires diameter. Obtained SAED patterns also show strong textured components with determined <111> and <112> crystalline directions parallel to the wires growth direction. The presence of both directions was also confirmed in the HRTEM images doing Fourier transform analyses. Magnetic measurements show strong magnetic anisotropy with magnetization easy axis parallel to the nanowires in as-prepared and annealed samples. The magnetic properties are tuned by suitable thermal treatments so that, maximum enhanced coercivity (∼2.7 kOe) and normalized remanence (∼0.91 Ms) values are achieved after annealing at temperature of 700 °C. The contribution of the changes in the crystalline structure, induced by the heat treatment, to the magnetic hardening of the FeCoCu nanowires is discussed.
Abstract Synchrotron-based X-ray fluorescence microscopy is a flexible tool for identifying the distribution of trace elements in biological specimens across a broad range of sample sizes. The technique is not particularly limited by sample type and can be performed on ancient fossils, fixed or fresh tissue specimens, and in some cases even live tissue and live cells can be studied. The technique can also be expanded to provide chemical specificity to elemental maps, either at individual points of interest in a map or across a large field of view. While virtually any sample type can be characterized with X-ray fluorescence microscopy, common biological sample preparation methods (often borrowed from other fields, such as histology) can lead to unforeseen pitfalls, resulting in altered element distributions and concentrations. A general overview of sample preparation and data-acquisition methods for X-ray fluorescence microscopy is presented, along with outlining the general approach for applying this technique to a new field of investigation for prospective new users. Considerations for improving data acquisition and quality are reviewed as well as the effects of sample preparation, with a particular focus on soft tissues. The effects of common sample pretreatment steps as well as the underlying factors that govern which, and to what extent, specific elements are likely to be altered are reviewed along with common artifacts observed in X-ray fluorescence microscopy data.
The ETF ammonia tolerant grout waste form was developed by the Vitreous State Laboratory (VSL) to stabilize ammonium and thereby prevent emission of ammonia vapor during solidification of an ammonium-rich, concentrated sulfate aqueous waste stream generated at the Hanford Effluent Treatment Facility (ETF). VSL did not observe expansion in samples prepared during the waste form development work. However, Savannah River National Laboratory (SRNL) personnel did encounter expansion, in some cases up to 20+ volume percent expansion in ETF grout samples while preforming work scope to evaluate compositional ranges for ETF brine and of the precipitation and solidification reagent. The work requests can be found in Washington River Protection Services (WRPS) Statement of Work (SOW), Requisitions #: 339922 Revisions 0 and 1, March 11, 2021, and November 2021. Additional evaluation was requested by WRPS SOW Requisitions #: 356730, Revision 1, February 1, 2022, to determine whether differences in the slags or differences in sample preparation protocols used by VSL and SRNL were the cause of the expansion observed in the SRNL samples. G. Chen, WRPS, arranged a materials exchange between VSL and SRNL and coordinated the VSL protocol for grouting and curing 1L of Base Case ETF simulant. Materials were exchanged between VSL and SRNL and both laboratories performed the VSL struvite precipitation-solidification protocol and cured samples for at least 28 days. VSL and SRNL encountered expansion, at varying degrees, in all samples prepared under the material exchange and grouting protocol. Additional material exchange testing between VSL and SRNL and alternative materials evaluation to further investigate the causes of grout expansion and differentiate the effects of various dry materials, grouting procedures, and curing containers was requested by WRPS SOW Requisitions #: 356730, Revision 2, January 10, 2023. Pacific Northwest National Laboratory (PNNL) assembled and distributed materials to both laboratories for testing. Observations from this study indicated variations in MgO additions, water-to-dry mix (dm) ratios and curing containers did not correlate to ETF ammonia grout expansion. In comparison to previous work, SRNL observed the addition rate of NaOH to be a potential factor for the final pH in the struvite precipitation step. In the current testing NaOH was added in bulk (5-10 mL at one time) during the precipitation step. The resulting pH was 7.57-9.15 which is slightly higher than pH observed at a slower addition rate. Additional testing is needed to identify the presence and/or struvite stability in high-pH struvite precipitant ETF ammonia grout samples. Therefore, based on current data, it is unknown if NaOH addition rate is the fundamental cause of grout expansion.
We present a detailed study on the effect of strontium non-stoichiometry on the properties of double perovskite Sr{sub 2}FeMoO{sub 6} (SFMO). A citrate route has been used to prepare high quality polycrystalline samples with (2−x)Sr:Fe:Mo (x=0, 0.02, 0.04) and (2+x)Sr:Fe:Mo (x=0.02, 0.04, 0.10) cationic ratios. The strontium deficient samples exhibit a significant decrease in their values of saturation magnetization (Ms), Curie temperature (Tc) and magnetoresistance (MR) compared to the stoichiometric SFMO. On the other hand, the samples prepared with an excess of strontium, respectively those with x=0.02 and 0.04, show remarkably superior magneto–transport characteristics, despite of their increased level of Fe/Mo disorder and somewhat diminished magnetic properties compared to the stoichiometric SFMO. We also show that these samples exhibit superior MR values under low magnetic field and persisting up to temperatures as high as 400 K. - Graphical abstract: Evolution of the magnetization versus temperature under an applied magnetic field of 1000 Oe (left panel) and magnetoresistance versus applied magnetic field at 300 K (right panel) for strontium off-stoichiometric Sr{sub 2}FeMoO{sub 6} samples. - Highlights: • Strontium nonstoichiometric samples of Sr{sub 2}FeMoO{sub 6} are prepared by a citrate route. • The nonstoichiometric samples exhibit an increased Fe/Mo disorder in the structure. • We observed important changes in their magnetic and magnetoresistive properties. • Improved magnetoresistive properties for samples prepared with strontium excess.
The Analytical Laboratory at Idaho National Laboratory (INL) is a growing program with an emphasis on providing high quality results to customers, and an increasing focus on independent research. The Analytical Laboratory Counting Group has a number of capabilities: six gamma-ray counters, one gamma-ray sample changer, four gas flow proportional counter drawers, an auto-changing gas flow proportional counter, two liquid scintillation counters, and an alpha spectroscopy system. Other capabilities within the Analytical Laboratory include quadrupole inductively coupled plasma mass spectrometry (ICP-MS), high resolution ICP-MS, multi-collector ICP-MS, ICP atomic emission spectrometry (ICP-AES), gas mass spectrometry, thermal ionization mass spectrometry (TIMS), several glove boxes and fume hoods for sample preparation, and six interconnected hot cells for sample receipt and dissolution. In order to position the Analytical Laboratory as a world-class research institution, the Counting Group has recently begun making improvements to its analytical techniques, calibrations, standardization, and quality control procedures. A large part of this effort is to increase the level of documentation of instrument work. One project is to re-calibrate all of the gamma systems with newly purchased standards. One of the changes made in the purchase of the new standards was to lower the total activity so that the dead time of the calibration would more closely match the dead time of typical samples. Similarly, another planned project is to use new standards to re-calibration the gas flow proportional counters. Additional work has focused on testing and improving alpha spectroscopy sample preparation techniques. Plutonium separations have been tested to improve tracer recovery and to verify the separation technique in the presence of typical sample matrices. A final planned area of improvements has focused on liquid scintillation counting. One difficulty the Counting Group has encountered in liquid scintillation counting is an inflated gross alpha count relative to other analysis methods in the presence of high gross beta activity. Ideas include investigating the impact of choice of scintillation cocktail, as well as the effects of sample dilution.