A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

PubMed

Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

2017-03-01

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF AIR SAMPLES FOR GC/MS ANALYSIS OF PESTICIDES (BCO-L-11.0)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for extracting and preparing an air sample consisting of a polyurethane foam (PUF) plug and Teflon-coated glass fiber filter (Pallflex T60A20) for analysis of pesticides. This procedure covers sample preparation for samples t...

Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

NASA Technical Reports Server (NTRS)

Carden, J. L.; Browner, R.

1982-01-01

The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.28)

EPA Science Inventory

This SOP describes the extraction and preparation of a solid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are to...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DUST AND SOIL SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.14)

EPA Science Inventory

This SOP summarizes the method for extracting and preparing a dust or soil sample for analysis of neutral persistent organic pollutants. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DERMAL WIPE SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.16)

EPA Science Inventory

The method for extracting and preparing a dermal (hand) wipe sample for analysis of neutral persistent organic pollutants is summarized in this SOP. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING LIQUID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.29)

EPA Science Inventory

This SOP describes the extraction and preparation of a liquid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are t...

Soils element activities for the period October 1973--September 1974

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fowler, E.B.; Essington, E.H.; White, M.G.

Soils Element activities were conducted on behalf of the U. S. Atomic Energy Commission's Nevada Applied Ecology Group (NAEG) program to provide source term information for the other program elements and maintain continuous cognizance of program requirements for sampling, sample preparation, and analysis. Activities included presentation of papers; participation in workshops; analysis of soil, vegetation, and animal tissue samples for $sup 238$Pu, $sup 239-240$Pu, $sup 241$Am, $sup 137$Cs, $sup 60$Co, and gamma scan for routine and laboratory quality control purposes; preparation and analysis of animal tissue samples for NAEG laboratory certification; studies on a number of analytical, sample preparation, andmore » sample collection procedures; and contributions to the evaluation of procedures for calculation of specialized counting statistics. (auth)« less

Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

NASA Astrophysics Data System (ADS)

Stosnach, Hagen; Mages, Margarete

2009-04-01

In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

Miniaturized sample preparation needle: a versatile design for the rapid analysis of smoking-related compounds in hair and air samples.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Hayashida, Makiko; Jinno, Kiyokatsu

2007-05-09

Miniaturized needle extraction device has been developed as a versatile sample preparation device designed for the rapid and simple analysis of smoking-related compounds in smokers' hair samples and environmental tobacco smoke. Packed with polymeric particle, the resulting particle-packed needle was employed as a miniaturized sample preparation device for the analysis of typical volatile organic compounds in tobacco smoke. Introducing a bundle of polymer-coated filaments as the extraction medium, the needle was further applied as a novel sample preparation device containing simultaneous derivatization/extraction process of volatile aldehydes. Formaldehyde (FA) and acetaldehyde (AA) in smoker's breath during the smoking were successfully derivatized with two derivatization reagents in the polymer-coated fiber-packed needle device followed by the separation and determination in gas chromatography (GC). Smokers' hair samples were also packed into the needle, allowing the direct extraction of nicotine from the hair sample in a conventional GC injector. Optimizing the main experimental parameters for each technique, successful determination of several smoking-related compounds with these needle extraction methods has been demonstrated.

Analysis and comparison of focused ion beam milling and vibratory polishing sample surface preparation methods for porosity study of U-Mo plate fuel for research and test reactors.

PubMed

Westman, Bjorn; Miller, Brandon; Jue, Jan-Fong; Aitkaliyeva, Assel; Keiser, Dennis; Madden, James; Tucker, Julie D

2018-07-01

Uranium-Molybdenum (U-Mo) low enriched uranium (LEU) fuels are a promising candidate for the replacement of high enriched uranium (HEU) fuels currently in use in a high power research and test reactors around the world. Contemporary U-Mo fuel sample preparation uses focused ion beam (FIB) methods for analysis of fission gas porosity. However, FIB possess several drawbacks, including reduced area of analysis, curtaining effects, and increased FIB operation time and cost. Vibratory polishing is a well understood method for preparing large sample surfaces with very high surface quality. In this research, fission gas porosity image analysis results are compared between samples prepared using vibratory polishing and FIB milling to assess the effectiveness of vibratory polishing for irradiated fuel sample preparation. Scanning electron microscopy (SEM) imaging was performed on sections of irradiated U-Mo fuel plates and the micrographs were analyzed using a fission gas pore identification and measurement script written in MatLab. Results showed that the vibratory polishing method is preferentially removing material around the edges of the pores, causing the pores to become larger and more rounded, leading to overestimation of the fission gas porosity size. Whereas, FIB preparation tends to underestimate due to poor micrograph quality and surface damage leading to inaccurate segmentations. Despite the aforementioned drawbacks, vibratory polishing remains a valid method for porosity analysis sample preparation, however, improvements should be made to reduce the preferential removal of material surrounding pores in order to minimize the error in the porosity measurements. Copyright © 2018 Elsevier Ltd. All rights reserved.

Analysis of $sup 239$Pu and $sup 241$Am in NAEG large-sized bovine samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Major, W.J.; Lee, K.D.; Wessman, R.A.

Methods are described for the analysis of environmental levels of $sup 239$Pu and $sup 241$Am in large-sized bovine samples. Special procedure modifications to overcome the complexities of sample preparation and analyses and special techniques employed to prepare and analyze different types of bovine samples, such as muscle, blood, liver, and bone are discussed. (CH)

Sample preparation for the analysis of isoflavones from soybeans and soy foods.

PubMed

Rostagno, M A; Villares, A; Guillamón, E; García-Lafuente, A; Martínez, J A

2009-01-02

This manuscript provides a review of the actual state and the most recent advances as well as current trends and future prospects in sample preparation and analysis for the quantification of isoflavones from soybeans and soy foods. Individual steps of the procedures used in sample preparation, including sample conservation, extraction techniques and methods, and post-extraction treatment procedures are discussed. The most commonly used methods for extraction of isoflavones with both conventional and "modern" techniques are examined in detail. These modern techniques include ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction and microwave-assisted extraction. Other aspects such as stability during extraction and analysis by high performance liquid chromatography are also covered.

Effect Of Neodymium Substitution In Structural Characteristics Of Magnesium Ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thankachan, Smitha; Binu, P. J.; Xavier, Sheena

2011-10-20

The effect of Nd{sup 3+} substitution on the structural properties of Magnesium ferrite was studied in the series MgNd{sub x}Fe{sub 2-x}O{sub 4}, where x = 0 to 0.3 in steps of 0.05. The series was prepared by sol-gel technique which is one of the novel technique to prepare nanosized samples. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. XRD analysis reveals the prepared samples are single phasic till x = 0.2. From x0 = .25, a secondary phase of iron neodymium oxide appears along with the spinel phase. Particle size calculation shows the prepared samples aremore » in the 9nm to 11 nm regime. Lattice parameter was found to increase with concentration of Nd. XRD and FTIR analysis confirmed spinel structure of the prepared samples. XRF result shows the expected composition of prepared samples. The frequency dependence of the dielectric constant in the range 100 Hz--120MHz was also studied« less

Adaptation of Laser Microdissection Technique for the Study of a Spontaneous Metastatic Mammary Carcinoma Mouse Model by NanoString Technologies

PubMed Central

Saylor, Karen L.; Anver, Miriam R.; Salomon, David S.; Golubeva, Yelena G.

2016-01-01

Laser capture microdissection (LCM) of tissue is an established tool in medical research for collection of distinguished cell populations under direct microscopic visualization for molecular analysis. LCM samples have been successfully analyzed in a number of genomic and proteomic downstream molecular applications. However, LCM sample collection and preparation procedure has to be adapted to each downstream analysis platform. In this present manuscript we describe in detail the adaptation of LCM methodology for the collection and preparation of fresh frozen samples for NanoString analysis based on a study of a model of mouse mammary gland carcinoma and its lung metastasis. Our adaptation of LCM sample preparation and workflow to the requirements of the NanoString platform allowed acquiring samples with high RNA quality. The NanoString analysis of such samples provided sensitive detection of genes of interest and their associated molecular pathways. NanoString is a reliable gene expression analysis platform that can be effectively coupled with LCM. PMID:27077656

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{submore » 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.« less

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DUST AND SOIL SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.15)

EPA Science Inventory

The method for extracting and preparing a dust or soil sample for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the extraction, concentration, and derivatization of samples that are to be analyzed by gas chromatography/mass spectrometry.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING URINE SAMPLES FOR ANALYSIS OF HYDROXY POLYCYCLIC AROMATIC HYDROCARBONS, PENTACHLOROPHENOL AND 2,4-D (SOP-5.21)

EPA Science Inventory

The method for extracting and preparing urine samples for analysis of hydroxy-polycyclic aromatic hydrocarbons, pentachlorophenol and 2,4-D is summarized in this SOP. It covers the extraction, concentration and methylation of samples that are to be analyzed by gas chromatography/...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING DERMAL WIPE AND SURFACE WIPE SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.27)

EPA Science Inventory

The method for extracting and preparing a dermal or surface wipe sample for analysis of acidic persistent organic pollutants is summarized in this standard operating procedure. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mas...

Fluidics platform and method for sample preparation and analysis

DOEpatents

Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

2014-08-19

Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

Evaluation of sample preparation methods for the analysis of papaya leaf proteins through two-dimensional gel electrophoresis.

PubMed

Rodrigues, Silas Pessini; Ventura, José Aires; Zingali, R B; Fernandes, P M B

2009-01-01

A variety of sample preparation protocols for plant proteomic analysis using two-dimensional gel electrophoresis (2-DE) have been reported. However, they usually have to be adapted and further optimised for the analysis of plant species not previously studied. This work aimed to evaluate different sample preparation protocols for analysing Carica papaya L. leaf proteins through 2-DE. Four sample preparation methods were tested: (1) phenol extraction and methanol-ammonium acetate precipitation; (2) no precipitation fractionation; and the traditional trichloroacetic acid-acetone precipitation either (3) with or (4) without protein fractionation. The samples were analysed for their compatibility with SDS-PAGE (1-DE) and 2-DE. Fifteen selected protein spots were trypsinised and analysed by matrix-assisted laser desorption/ionisation time-of-flight tandem mass spectrometry (MALDI-TOF-MS/MS), followed by a protein search using the NCBInr database to accurately identify all proteins. Methods number 3 and 4 resulted in large quantities of protein with good 1-DE separation and were chosen for 2-DE analysis. However, only the TCA method without fractionation (no. 4) proved to be useful. Spot number and resolution advances were achieved, which included having an additional solubilisation step in the conventional TCA method. Moreover, most of the theoretical and experimental protein molecular weight and pI data had similar values, suggesting good focusing and, most importantly, limited protein degradation. The described sample preparation method allows the proteomic analysis of papaya leaves by 2-DE and mass spectrometry (MALDI-TOF-MS/MS). The methods presented can be a starting point for the optimisation of sample preparation protocols for other plant species.

Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples

DTIC Science & Technology

2015-11-13

P Wijewarnasuriya at the Army Research Lab to understand the bandd offsets of HgCdTe infrared detector structures. Especially when a sample is not...Final Report: Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples Report Title A used calibrated...structures i. G15-38 and G15-38 Quantum Dot ---------------------------- 16 Infrared Detector Samples ii. GSU13-MPD-GB1 Heterostructure

Automation of preparation of nonmetallic samples for analysis by atomic absorption and inductively coupled plasma spectrometry

NASA Technical Reports Server (NTRS)

Wittmann, A.; Willay, G.

1986-01-01

For a rapid preparation of solutions intended for analysis by inductively coupled plasma emission spectrometry or atomic absorption spectrometry, an automatic device called Plasmasol was developed. This apparatus used the property of nonwettability of glassy C to fuse the sample in an appropriate flux. The sample-flux mixture is placed in a composite crucible, then heated at high temperature, swirled until full dissolution is achieved, and then poured into a water-filled beaker. After acid addition, dissolution of the melt, and filling to the mark, the solution is ready for analysis. The analytical results obtained, either for oxide samples or for prereduced iron ores show that the solutions prepared with this device are undistinguished from those obtained by manual dissolutions done by acid digestion or by high temperature fusion. Preparation reproducibility and analytical tests illustrate the performance of Plasmasol.

Sampling hazelnuts for aflatoxin: uncertainty associated with sampling, sample preparation, and analysis.

PubMed

Ozay, Guner; Seyhan, Ferda; Yilmaz, Aysun; Whitaker, Thomas B; Slate, Andrew B; Giesbrecht, Francis

2006-01-01

The variability associated with the aflatoxin test procedure used to estimate aflatoxin levels in bulk shipments of hazelnuts was investigated. Sixteen 10 kg samples of shelled hazelnuts were taken from each of 20 lots that were suspected of aflatoxin contamination. The total variance associated with testing shelled hazelnuts was estimated and partitioned into sampling, sample preparation, and analytical variance components. Each variance component increased as aflatoxin concentration (either B1 or total) increased. With the use of regression analysis, mathematical expressions were developed to model the relationship between aflatoxin concentration and the total, sampling, sample preparation, and analytical variances. The expressions for these relationships were used to estimate the variance for any sample size, subsample size, and number of analyses for a specific aflatoxin concentration. The sampling, sample preparation, and analytical variances associated with estimating aflatoxin in a hazelnut lot at a total aflatoxin level of 10 ng/g and using a 10 kg sample, a 50 g subsample, dry comminution with a Robot Coupe mill, and a high-performance liquid chromatographic analytical method are 174.40, 0.74, and 0.27, respectively. The sampling, sample preparation, and analytical steps of the aflatoxin test procedure accounted for 99.4, 0.4, and 0.2% of the total variability, respectively.

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the... PCB remediation waste at the cleanup site, or must be the same kind of material as that waste. For...

Recent advances in applications of nanomaterials for sample preparation.

PubMed

Xu, Linnan; Qi, Xiaoyue; Li, Xianjiang; Bai, Yu; Liu, Huwei

2016-01-01

Sample preparation is a key step for qualitative and quantitative analysis of trace analytes in complicated matrix. Along with the rapid development of nanotechnology in material science, numerous nanomaterials have been developed with particularly useful applications in analytical chemistry. Benefitting from their high specific areas, increased surface activities, and unprecedented physical/chemical properties, the potentials of nanomaterials for rapid and efficient sample preparation have been exploited extensively. In this review, recent progress of novel nanomaterials applied in sample preparation has been summarized and discussed. Both nanoparticles and nanoporous materials are evaluated for their unusual performance in sample preparation. Various compositions and functionalizations extended the applications of nanomaterials in sample preparations, and distinct size and shape selectivity was generated from the diversified pore structures of nanoporous materials. Such great variety make nanomaterials a kind of versatile tools in sample preparation for almost all categories of analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

PubMed

Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

PubMed

Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

2014-04-01

Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

Potential artifacts associated with historical preparation of joint compound samples and reported airborne asbestos concentrations.

PubMed

Brorby, G P; Sheehan, P J; Berman, D W; Bogen, K T; Holm, S E

2011-05-01

Airborne samples collected in the 1970s for drywall workers using asbestos-containing joint compounds were likely prepared and analyzed according to National Institute of Occupational Safety and Health Method P&CAM 239, the historical precursor to current Method 7400. Experimentation with a re-created, chrysotile-containing, carbonate-based joint compound suggested that analysis following sample preparation by the historical vs. current method produces different fiber counts, likely because of an interaction between the different clearing and mounting chemicals used and the carbonate-based joint compound matrix. Differences were also observed during analysis using Method 7402, depending on whether acetic acid/dimethylformamide or acetone was used during preparation to collapse the filter. Specifically, air samples of sanded chrysotile-containing joint compound prepared by the historical method yielded fiber counts significantly greater (average of 1.7-fold, 95% confidence interval: 1.5- to 2.0-fold) than those obtained by the current method. In addition, air samples prepared by Method 7402 using acetic acid/dimethylformamide yielded fiber counts that were greater (2.8-fold, 95% confidence interval: 2.5- to 3.2-fold) than those prepared by this method using acetone. These results indicated (1) there is an interaction between Method P&CAM 239 preparation chemicals and the carbonate-based joint compound matrix that reveals fibers that were previously bound in the matrix, and (2) the same appeared to be true for Method 7402 preparation chemicals acetic acid/dimethylformamide. This difference in fiber counts is the opposite of what has been reported historically for samples of relatively pure chrysotile dusts prepared using the same chemicals. This preparation artifact should be considered when interpreting historical air samples for drywall workers prepared by Method P&CAM 239. Copyright © 2011 JOEH, LLC

Quantitative and qualitative measure of intralaboratory two-dimensional protein gel reproducibility and the effects of sample preparation, sample load, and image analysis.

PubMed

Choe, Leila H; Lee, Kelvin H

2003-10-01

We investigate one approach to assess the quantitative variability in two-dimensional gel electrophoresis (2-DE) separations based on gel-to-gel variability, sample preparation variability, sample load differences, and the effect of automation on image analysis. We observe that 95% of spots present in three out of four replicate gels exhibit less than a 0.52 coefficient of variation (CV) in fluorescent stain intensity (% volume) for a single sample run on multiple gels. When four parallel sample preparations are performed, this value increases to 0.57. We do not observe any significant change in quantitative value for an increase or decrease in sample load of 30% when using appropriate image analysis variables. Increasing use of automation, while necessary in modern 2-DE experiments, does change the observed level of quantitative and qualitative variability among replicate gels. The number of spots that change qualitatively for a single sample run in parallel varies from a CV = 0.03 for fully manual analysis to CV = 0.20 for a fully automated analysis. We present a systematic method by which a single laboratory can measure gel-to-gel variability using only three gel runs.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF AIR SAMPLES FOR GC/MS ANALYSIS OF PESTICIDE AND PAH (BCO-L-27.0)

EPA Science Inventory

The purpose of this SOP is to describe methods for extracting and preparing an air sample consisting of a quartz fiber filter (Pallflex) and an XAD-2 cartridge for analysis of pesticides and polyaromatic hydrocarbons (PAHs). It covers the preparation of samples that are to be an...

Simultaneous derivatization/preconcentration of volatile aldehydes with a miniaturized fiber-packed sample preparation device designed for gas chromatographic analysis.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Jinno, Kiyokatsu

2006-10-01

A novel in-needle sample preparation device has been developed for the determination of volatile aldehydes in gaseous samples. The needle device is designed for the gas chromatographic (GC) analysis of aldehydes and ketones commonly found in typical in-house environments. In order to prepare the extraction device, a bundle of polymer-coated filaments was longitudinally packed into a specially designed needle. Derivatization reactions were prompted by 2,4-dinitrophenylhydrazine (NDPH) included in the needle, and so the aldehydes and ketones were derivatized to the corresponding hydrazones and extracted with the extraction needle. A reproducible extraction needle preparation process was established, along with a repeatable derivatization/extraction process that ensures the successful determination of aldehydes. The storage performance of the extraction needle was also evaluated at room temperature for three days. The results demonstrate the successful application of the fiber-packed extraction device to the preparation of a gaseous sample of aldehydes, and the future possibility of applying the extraction device to the analysis of in-house environments.

Sensory profile and acceptability for pitanga (Eugenia uniflora L.) nectar with different sweeteners.

PubMed

Freitas, Mírian Luisa Faria; Dutra, Mariana Borges de Lima; Bolini, Helena Maria André

2016-12-01

The objective of this study was to evaluate the sensory properties and acceptability of pitanga nectar samples prepared with sucrose and different sweeteners (sucralose, aspartame, stevia with 40% rebaudioside A, stevia with 95% rebaudioside A, neotame, and a 2:1 cyclamate/saccharin blend). A total of 13 assessors participated in a quantitative descriptive analysis and evaluated the samples in relation to the descriptor terms. The acceptability test was carried out by 120 fruit juice consumers. The results of the quantitative descriptive analysis of pitanga nectar showed that samples prepared with sucralose, aspartame, and the 2:1 cyclamate/saccharin blend had sensory profiles similar to that of the sample prepared with sucrose. Consumers' most accepted samples were prepared with sucrose, sucralose, aspartame, and neotame. The sweeteners that have the greatest potential to replace sucrose in pitanga nectar are sucralose and aspartame. © The Author(s) 2016.

[Standard sample preparation method for quick determination of trace elements in plastic].

PubMed

Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

2011-08-01

Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

Unattended reaction monitoring using an automated microfluidic sampler and on-line liquid chromatography.

PubMed

Patel, Darshan C; Lyu, Yaqi Fara; Gandarilla, Jorge; Doherty, Steve

2018-04-03

In-process sampling and analysis is an important aspect of monitoring kinetic profiles and impurity formation or rejection, both in development and during commercial manufacturing. In pharmaceutical process development, the technology of choice for a substantial portion of this analysis is high-performance liquid chromatography (HPLC). Traditionally, the sample extraction and preparation for reaction characterization have been performed manually. This can be time consuming, laborious, and impractical for long processes. Depending on the complexity of the sample preparation, there can be variability introduced by different analysts, and in some cases, the integrity of the sample can be compromised during handling. While there are commercial instruments available for on-line monitoring with HPLC, they lack capabilities in many key areas. Some do not provide integration of the sampling and analysis, while others afford limited flexibility in sample preparation. The current offerings provide a limited number of unit operations available for sample processing and no option for workflow customizability. This work describes development of a microfluidic automated program (MAP) which fully automates the sample extraction, manipulation, and on-line LC analysis. The flexible system is controlled using an intuitive Microsoft Excel based user interface. The autonomous system is capable of unattended reaction monitoring that allows flexible unit operations and workflow customization to enable complex operations and on-line sample preparation. The automated system is shown to offer advantages over manual approaches in key areas while providing consistent and reproducible in-process data. Copyright © 2017 Elsevier B.V. All rights reserved.

Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.

2007-12-01

The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includesmore » an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.« less

Quantitation of heat-shock proteins in clinical samples using mass spectrometry.

PubMed

Kaur, Punit; Asea, Alexzander

2011-01-01

Mass spectrometry (MS) is a powerful analytical tool for proteomics research and drug and biomarker discovery. MS enables identification and quantification of known and unknown compounds by revealing their structural and chemical properties. Proper sample preparation for MS-based analysis is a critical step in the proteomics workflow because the quality and reproducibility of sample extraction and preparation for downstream analysis significantly impact the separation and identification capabilities of mass spectrometers. The highly expressed proteins represent potential biomarkers that could aid in diagnosis, therapy, or drug development. Because the proteome is so complex, there is no one standard method for preparing protein samples for MS analysis. Protocols differ depending on the type of sample, source, experiment, and method of analysis. Molecular chaperones play significant roles in almost all biological functions due to their capacity for detecting intracellular denatured/unfolded proteins, initiating refolding or denaturation of such malfolded protein sequences and more recently for their role in the extracellular milieu as chaperokines. In this chapter, we describe the latest techniques for quantitating the expression of molecular chaperones in human clinical samples.

Methodological considerations for implementation of lymphocyte subset analysis in a clinical reference laboratory.

PubMed

Muirhead, K A; Wallace, P K; Schmitt, T C; Frescatore, R L; Franco, J A; Horan, P K

1986-01-01

As the diagnostic utility of lymphocyte subset analysis has been recognized in the clinical research laboratory, a wide variety of reagents and cell preparation, staining and analysis methods have also been described. Methods that are perfectly suitable for analysis of smaller sample numbers in the biological or clinical research setting are not always appropriate and/or applicable in the setting of a high volume clinical reference laboratory. We describe here some of the specific considerations involved in choosing a method for flow cytometric analysis which minimizes sample preparation and data analysis time while maximizing sample stability, viability, and reproducibility. Monoclonal T- and B-cell reagents from three manufacturers were found to give equivalent results for a reference population of healthy individuals. This was true whether direct or indirect immunofluorescence staining was used and whether cells were prepared by Ficoll-Hypaque fractionation (FH) or by lysis of whole blood. When B cells were enumerated using a polyclonal anti-immunoglobulin reagent, less cytophilic immunoglobulin staining was present after lysis than after FH preparation. However, both preparation methods required additional incubation at 37 degrees C to obtain results concordant with monoclonal B-cell reagents. Standard reagents were chosen on the basis of maximum positive/negative separation and the availability of appropriate negative controls. The effects of collection medium and storage conditions on sample stability and reproducibility of subset analysis were also assessed. Specimens collected in heparin and stored at room temperature in buffered medium gave reproducible results for 3 days after specimen collection, using either FH or lysis as the preparation method. General strategies for instrument optimization, quality control, and biohazard containment are also discussed.

Modified electrokinetic sample injection method in chromatography and electrophoresis analysis

DOEpatents

Davidson, J. Courtney; Balch, Joseph W.

2001-01-01

A sample injection method for horizontal configured multiple chromatography or electrophoresis units, each containing a number of separation/analysis channels, that enables efficient introduction of analyte samples. This method for loading when taken in conjunction with horizontal microchannels allows much reduced sample volumes and a means of sample stacking to greatly reduce the concentration of the sample. This reduction in the amount of sample can lead to great cost savings in sample preparation, particularly in massively parallel applications such as DNA sequencing. The essence of this method is in preparation of the input of the separation channel, the physical sample introduction, and subsequent removal of excess material. By this method, sample volumes of 100 nanoliter to 2 microliters have been used successfully, compared to the typical 5 microliters of sample required by the prior separation/analysis method.

Forensic Analysis of Human DNA from Samples Contamined with Bioweapons Agents

DTIC Science & Technology

2011-10-01

Forensic analysis of human DNA from samples contaminated with bioweapons agents Jason Timbers Kathryn Wright Royal Canadian Mounted...Police Forensic Science and Identification Service Prepared By: Royal Canadian Mounted Police RCMP Forensic Science Identification Services... Royal Canadian Mounted Police Forensic Science and Identification Service Prepared By: Royal Canadian Mounted Police RCMP Forensic Science

Preparation, certification and interlaboratory analysis of workplace air filters spiked with high-fired beryllium oxide.

PubMed

Oatts, Thomas J; Hicks, Cheryl E; Adams, Amy R; Brisson, Michael J; Youmans-McDonald, Linda D; Hoover, Mark D; Ashley, Kevin

2012-02-01

Occupational sampling and analysis for multiple elements is generally approached using various approved methods from authoritative government sources such as the National Institute for Occupational Safety and Health (NIOSH), the Occupational Safety and Health Administration (OSHA) and the Environmental Protection Agency (EPA), as well as consensus standards bodies such as ASTM International. The constituents of a sample can exist as unidentified compounds requiring sample preparation to be chosen appropriately, as in the case of beryllium in the form of beryllium oxide (BeO). An interlaboratory study was performed to collect analytical data from volunteer laboratories to examine the effectiveness of methods currently in use for preparation and analysis of samples containing calcined BeO powder. NIST SRM(®) 1877 high-fired BeO powder (1100 to 1200 °C calcining temperature; count median primary particle diameter 0.12 μm) was used to spike air filter media as a representative form of beryllium particulate matter present in workplace sampling that is known to be resistant to dissolution. The BeO powder standard reference material was gravimetrically prepared in a suspension and deposited onto 37 mm mixed cellulose ester air filters at five different levels between 0.5 μg and 25 μg of Be (as BeO). Sample sets consisting of five BeO-spiked filters (in duplicate) and two blank filters, for a total of twelve unique air filter samples per set, were submitted as blind samples to each of 27 participating laboratories. Participants were instructed to follow their current process for sample preparation and utilize their normal analytical methods for processing samples containing substances of this nature. Laboratories using more than one sample preparation and analysis method were provided with more than one sample set. Results from 34 data sets ultimately received from the 27 volunteer laboratories were subjected to applicable statistical analyses. The observed performance data show that sample preparations using nitric acid alone, or combinations of nitric and hydrochloric acids, are not effective for complete extraction of Be from the SRM 1877 refractory BeO particulate matter spiked on air filters; but that effective recovery can be achieved by using sample preparation procedures utilizing either sulfuric or hydrofluoric acid, or by using methodologies involving ammonium bifluoride with heating. Laboratories responsible for quantitative determination of Be in workplace samples that may contain high-fired BeO should use quality assurance schemes that include BeO-spiked sampling media, rather than solely media spiked with soluble Be compounds, and should ensure that methods capable of quantitative digestion of Be from the actual material present are used.

Detection of Acetone Processing of Castor Bean Mash for Forensic Investigation of Ricin Preparation Methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kreuzer-Martin, Helen W.; Wahl, Jon H.; Metoyer, Candace N.

The toxic protein ricin is of concern as a potential biological threat agent (BTA) Recently, several samples of ricin have been seized in connection with biocriminal activity. Analytical methods are needed that enable federal investigators to determine how the samples were prepared, to match seized samples to potential source materials, and to identify samples that may have been prepared by the same method using the same source materials. One commonly described crude ricin preparation method is acetone extraction of crushed castor beans. Here we describe the use of solid-phase microextraction and headspace analysis of crude ricin preparation samples to determinemore » whether they were processed by acetone extraction. In all cases, acetone-extracted bean mash could be distinguished from un-extracted mash or mash extracted with other organic solvents. Statistical analysis showed that storage in closed containers for up to 109 days had no effect on acetone signal intensity. Signal intensity in acetone-extracted mash decreased during storage in open containers, but extracted mash could still be distinguished from un-extracted mash after 94 days.« less

Structural morphology, upconversion luminescence and optical thermometric sensing behavior of Y2O3:Er(3+)/Yb(3+) nano-crystalline phosphor.

PubMed

Joshi, C; Dwivedi, A; Rai, S B

2014-08-14

Infrared-to-visible upconverting rare earths Er(3+)/Yb(3+) co-doped Y2O3 nano-crystalline phosphor samples have been prepared by solution combustion method followed by post-heat treatment at higher temperatures. A slight increase in average crystallite size has been found on calcinations verified by X-ray analysis. Transmission electron microscopy (TEM) confirms the nano-crystalline nature of the as-prepared and calcinated samples. Fourier transform infrared (FTIR) analysis shows the structural changes in as-prepared and calcinated samples. Upconversion and downconversion emission recorded using 976 and 532 nm laser sources clearly demonstrates a better luminescence properties in the calcinated samples as compared to as-prepared sample. Upconversion emission has been quantified in terms of standard chromaticity diagram (CIE) showing a shift in overall upconversion emission of as-prepared and calcinated samples. Temperature sensing behaviour of this material has also been investigated by measurement of fluorescence intensity ratio (FIR) of various signals in green emission in the temperature range of 315 to 555 K under 976 nm laser excitation. Copyright © 2014 Elsevier B.V. All rights reserved.

How Confocal Is Confocal Raman Microspectroscopy on the Skin? Impact of Microscope Configuration and Sample Preparation on Penetration Depth Profiles.

PubMed

Lunter, Dominique Jasmin

2016-01-01

The aim of the study was to elucidate the effect of sample preparation and microscope configuration on the results of confocal Raman microspectroscopic evaluation of the penetration of a pharmaceutical active into the skin (depth profiling). Pig ear skin and a hydrophilic formulation containing procaine HCl were used as a model system. The formulation was either left on the skin during the measurement, or was wiped off or washed off prior to the analysis. The microscope configuration was varied with respect to objectives and pinholes used. Sample preparation and microscope configuration had a tremendous effect on the results of depth profiling. Regarding sample preparation, the best results could be observed when the formulation was washed off the skin prior to the analysis. Concerning microscope configuration, the use of a 40 × 0.6 numerical aperture (NA) objective in combination with a 25-µm pinhole or a 100 × 1.25 NA objective in combination with a 50-µm pinhole was found to be advantageous. Complete removal of the sample from the skin before the analysis was found to be crucial. A thorough analysis of the suitability of the chosen microscope configuration should be performed before acquiring concentration depth profiles. © 2016 S. Karger AG, Basel.

Evaluation of a Fast and Simple Sample Preparation Method for Polybrominated Diphenyl Ether (PBDE) Flame Retardants and Dichlorodiphenyltrichloroethane (DDT) Pesticides in Fish for Analysis by ELISA Compared with GC-MS/MS.

PubMed

Sapozhnikova, Yelena; Simons, Tawana; Lehotay, Steven J

2015-05-13

A simple, fast, and cost-effective sample preparation method, previously developed and validated for the analysis of organic contaminants in fish using low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS), was evaluated for the analysis of polybrominated diphenyl ethers (PBDEs) and dichlorodiphenyltrichloroethane (DDT) pesticides using enzyme-linked immunosorbent assay (ELISA). The sample preparation technique was based on the quick, easy, cheap, rugged, effective, and safe (QuEChERS) approach with filter-vial dispersive solid phase extraction (d-SPE). Incurred PBDEs and DDTs were analyzed in three types of fish with 3-10% lipid content: Pacific croaker, salmon, and National Institute of Standards and Technology (NIST) Standard Reference Material 1947 (Lake Michigan fish tissue). LPGC-MS/MS and ELISA results were in agreement: 108-111 and 65-82% accuracy ELISA versus LPGC-MS/MS results for PBDEs and DDTs, respectively. Similar detection limits were achieved for ELISA and LPGC-MS/MS. Matrix effects (MEs) were significant (e.g., -60%) for PBDE measurement in ELISA, but not a factor in the case of DDT pesticides. This study demonstrated that the sample preparation method can be adopted for semiquantitative screening analysis of fish samples by commercial kits for PBDEs and DDTs.

Current trends and challenges in sample preparation for metallic nanoparticles analysis in daily products and environmental samples: A review

NASA Astrophysics Data System (ADS)

De la Calle, Inmaculada; Menta, Mathieu; Séby, Fabienne

2016-11-01

Due to the increasing use of nanoparticles (NPs) in consumer products, it becomes necessary to develop different strategies for their detection, identification, characterization and quantification in a wide variety of samples. Since the analysis of NPs in consumer products and environmental samples is particularly troublesome, a detailed description of challenges and limitations is given here. This review mainly focuses on sample preparation procedures applied for the mostly used techniques for metallic and metal oxide NPs characterization in consumer products and most outstanding publications of biological and environmental samples (from 2006 to 2015). We summarize the procedures applied for total metal content, extraction/separation and/or preconcentration of NPs from the matrix, separation of metallic NPs from their ions or from larger particles and NPs' size fractionation. Sample preparation procedures specifically for microscopy are also described. Selected applications in cosmetics, food, other consumer products, biological tissues and environmental samples are presented. Advantages and inconveniences of those procedures are considered. Moreover, selected simplified schemes for NPs sample preparation, as well as usual techniques applied are included. Finally, promising directions for further investigations are discussed.

Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

PubMed Central

Geller, Joseph D.; Engle, Paul D.

2002-01-01

There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very important, and, under certain conditions, may even be the limiting factor in the analytical uncertainty budget. This paper considers preparing samples to get known geometries. It will not address the analysis of samples with irregular, unprepared surfaces or unknown geometries. PMID:27446757

Sample treatments prior to capillary electrophoresis-mass spectrometry.

PubMed

Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Angel; Cifuentes, Alejandro

2007-06-15

Sample preparation is a crucial part of chemical analysis and in most cases can become the bottleneck of the whole analytical process. Its adequacy is a key factor in determining the success of the analysis and, therefore, careful selection and optimization of the parameters controlling sample treatment should be carried out. This work revises the different strategies that have been developed for sample preparation prior to capillary electrophoresis-mass spectrometry (CE-MS). Namely the present work presents an exhaustive and critical revision of the different samples treatments used together with on-line CE-MS including works published from January 2000 to July 2006.

Recent advances of mesoporous materials in sample preparation.

PubMed

Zhao, Liang; Qin, Hongqiang; Wu, Ren'an; Zou, Hanfa

2012-03-09

Sample preparation has been playing an important role in the analysis of complex samples. Mesoporous materials as the promising adsorbents have gained increasing research interest in sample preparation due to their desirable characteristics of high surface area, large pore volume, tunable mesoporous channels with well defined pore-size distribution, controllable wall composition, as well as modifiable surface properties. The aim of this paper is to review the recent advances of mesoporous materials in sample preparation with emphases on extraction of metal ions, adsorption of organic compounds, size selective enrichment of peptides/proteins, specific capture of post-translational peptides/proteins and enzymatic reactor for protein digestion. Copyright © 2011 Elsevier B.V. All rights reserved.

The role of sample preparation in interpretation of trace element concentration variability in moss bioindication studies

USGS Publications Warehouse

Migaszewski, Z.M.; Lamothe, P.J.; Crock, J.G.; Galuszka, A.; Dolegowska, S.

2011-01-01

Trace element concentrations in plant bioindicators are often determined to assess the quality of the environment. Instrumental methods used for trace element determination require digestion of samples. There are different methods of sample preparation for trace element analysis, and the selection of the best method should be fitted for the purpose of a study. Our hypothesis is that the method of sample preparation is important for interpretation of the results. Here we compare the results of 36 element determinations performed by ICP-MS on ashed and on acid-digested (HNO3, H2O2) samples of two moss species (Hylocomium splendens and Pleurozium schreberi) collected in Alaska and in south-central Poland. We found that dry ashing of the moss samples prior to analysis resulted in considerably lower detection limits of all the elements examined. We also show that this sample preparation technique facilitated the determination of interregional and interspecies differences in the chemistry of trace elements. Compared to the Polish mosses, the Alaskan mosses displayed more positive correlations of the major rock-forming elements with ash content, reflecting those elements' geogenic origin. Of the two moss species, P. schreberi from both Alaska and Poland was also highlighted by a larger number of positive element pair correlations. The cluster analysis suggests that the more uniform element distribution pattern of the Polish mosses primarily reflects regional air pollution sources. Our study has shown that the method of sample preparation is an important factor in statistical interpretation of the results of trace element determinations. ?? 2010 Springer-Verlag.

Nearly 1000 Protein Identifications from 50 ng of Xenopus laevis Zygote Homogenate Using Online Sample Preparation on a Strong Cation Exchange Monolith Based Microreactor Coupled with Capillary Zone Electrophoresis.

PubMed

Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J

2016-01-05

A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method.

Electrical and magnetic properties of nano-sized magnesium ferrite

NASA Astrophysics Data System (ADS)

T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.

2015-02-01

Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.

Cost Analysis of Various Low Pathogenic Avian Influenza Surveillance Systems in the Dutch Egg Layer Sector

PubMed Central

Rutten, Niels; Gonzales, José L.; Elbers, Armin R. W.; Velthuis, Annet G. J.

2012-01-01

Background As low pathogenic avian influenza viruses can mutate into high pathogenic viruses the Dutch poultry sector implemented a surveillance system for low pathogenic avian influenza (LPAI) based on blood samples. It has been suggested that egg yolk samples could be sampled instead of blood samples to survey egg layer farms. To support future decision making about AI surveillance economic criteria are important. Therefore a cost analysis is performed on systems that use either blood or eggs as sampled material. Methodology/Principal Findings The effectiveness of surveillance using egg or blood samples was evaluated using scenario tree models. Then an economic model was developed that calculates the total costs for eight surveillance systems that have equal effectiveness. The model considers costs for sampling, sample preparation, sample transport, testing, communication of test results and for the confirmation test on false positive results. The surveillance systems varied in sampled material (eggs or blood), sampling location (farm or packing station) and location of sample preparation (laboratory or packing station). It is shown that a hypothetical system in which eggs are sampled at the packing station and samples prepared in a laboratory had the lowest total costs (i.e. € 273,393) a year. Compared to this a hypothetical system in which eggs are sampled at the farm and samples prepared at a laboratory, and the currently implemented system in which blood is sampled at the farm and samples prepared at a laboratory have 6% and 39% higher costs respectively. Conclusions/Significance This study shows that surveillance for avian influenza on egg yolk samples can be done at lower costs than surveillance based on blood samples. The model can be used in future comparison of surveillance systems for different pathogens and hazards. PMID:22523543

Sample collection and preparation of biofluids and extracts for gas chromatography-mass spectrometry.

PubMed

Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Kharbatia, Najeh M

2015-01-01

To maximize the utility of gas chromatography-mass spectrometry (GC-MS) in metabonomics research, all stages of the experimental design should be standardized, including sample collection, storage, preparation, and sample separation. Moreover, the prerequisite for any GC-MS analysis is that a compound must be volatile and thermally stable if it is to be analyzed using this technique. Since many metabolites are nonvolatile and polar in nature, they are not readily amenable to analysis by GC-MS and require initial chemical derivatization of the polar functional groups in order to reduce the polarity and to increase the thermal stability and volatility of the analytes. In this chapter, an overview is presented of the optimum approach to sample collection, storage, and preparation for gas chromatography-mass spectrometry-based metabonomics with particular focus on urine samples as example of biofluids.

Validated Test Method 5030C: Purge-and-Trap for Aqueous Samples

EPA Pesticide Factsheets

This method describes a purge-and-trap procedure for the analysis of volatile organic compoundsin aqueous samples & water miscible liquid samples. It also describes the analysis of high concentration soil and waste sample extracts prepared in Method 5035.

Microfluidic Sample Preparation for Diagnostic Cytopathology

PubMed Central

Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino

2014-01-01

The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972

Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

PubMed Central

Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

2014-01-01

In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

NASA Astrophysics Data System (ADS)

Chandra, Subhash

2008-12-01

Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2+) revealed local secondary ion signal enhancements correlated with the water image signals of 19(H 3O) +. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells provided a rule-of-thumb criterion for the validation of sample preparation. The fractured freeze-dried cells allowed 3-D SIMS imaging and localization of 13C 15N labeled molecules and therapeutic drugs containing an elemental tag. Examples are shown to demonstrate that both diffusible elements and molecules are prone to artifact-induced relocation at subcellular scale if the sample preparation is compromised. The sample preparation is problem dependent and may vary widely between the diverse sample types of biological systems and the type of instrument used for SIMS analysis. The sample preparation, however, must be validated so that SIMS can be applied with confidence in biology and medicine.

Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

PubMed

Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

2011-01-01

To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

EPA Science Inventory

An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

Recent trends in sorption-based sample preparation and liquid chromatography techniques for food analysis.

PubMed

V Soares Maciel, Edvaldo; de Toffoli, Ana Lúcia; Lanças, Fernando Mauro

2018-04-20

The accelerated rising of the world's population increased the consumption of food, thus demanding more rigors in the control of residue and contaminants in food-based products marketed for human consumption. In view of the complexity of most food matrices, including fruits, vegetables, different types of meat, beverages, among others, a sample preparation step is important to provide more reliable results when combined with HPLC separations. An adequate sample preparation step before the chromatographic analysis is mandatory in obtaining higher precision and accuracy in order to improve the extraction of the target analytes, one of the priorities in analytical chemistry. The recent discovery of new materials such as ionic liquids, graphene-derived materials, molecularly imprinted polymers, restricted access media, magnetic nanoparticles, and carbonaceous nanomaterials, provided high sensitivity and selectivity results in an extensive variety of applications. These materials, as well as their several possible combinations, have been demonstrated to be highly appropriate for the extraction of different analytes in complex samples such as food products. The main characteristics and application of these new materials in food analysis will be presented and discussed in this paper. Another topic discussed in this review covers the main advantages and limitations of sample preparation microtechniques, as well as their off-line and on-line combination with HPLC for food analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automated Drug Identification for Urban Hospitals

NASA Technical Reports Server (NTRS)

Shirley, Donna L.

1971-01-01

Many urban hospitals are becoming overloaded with drug abuse cases requiring chemical analysis for identification of drugs. In this paper, the requirements for chemical analysis of body fluids for drugs are determined and a system model for automated drug analysis is selected. The system as modeled, would perform chemical preparation of samples, gas-liquid chromatographic separation of drugs in the chemically prepared samples, infrared spectrophotometric analysis of the drugs, and would utilize automatic data processing and control for drug identification. Requirements of cost, maintainability, reliability, flexibility, and operability are considered.

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

NASA Astrophysics Data System (ADS)

Lari, L.; Dudkiewicz, A.

2014-06-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) of skin: Aspects of sample preparation.

PubMed

de Macedo, Cristiana Santos; Anderson, David M; Schey, Kevin L

2017-11-01

MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) allows molecular analysis of biological materials making possible the identification and localization of molecules in tissues, and has been applied to address many questions on skin pathophysiology, as well as on studies about drug absorption and metabolism. Sample preparation for MALDI IMS is the most important part of the workflow, comprising specimen collection and preservation, tissue embedding, cryosectioning, washing, and matrix application. These steps must be carefully optimized for specific analytes of interest (lipids, proteins, drugs, etc.), representing a challenge for skin analysis. In this review, critical parameters for MALDI IMS sample preparation of skin samples will be described. In addition, specific applications of MALDI IMS of skin samples will be presented including wound healing, neoplasia, and infection. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of coke beverages by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; von Bohlen, Alex; Friedrich K, E. Josue; Redrejo, M. J.

2018-07-01

The influence of the organic content, sample preparation process and the morphology of the depositions of two types of Coke beverage, traditional and light Coke, have been investigated by mean of Total-reflection X-ray Fluorescence (TXRF) spectrometry. Strong distortions of the nominal concentration values, up to 128% for P, have been detected in the analysis of traditional Coke by different preparation methods. These differences have been correlated with the edge X-ray energies of the elements analyzed being more pronounced for the lighter elements. The influence of the organic content (mainly sugar) was evaluated comparing traditional and light Coke analytical TXRF results. Three sample preparation methods have been evaluated as follows: direct TXRF analysis of the sample only adding internal standard, TXRF analysis after open vessel acid digestion and TXRF analysis after high pressure and temperature microwave-assisted acid digestion. Strong correlations were detected between quantitative results, methods of preparation and energies of the X-ray absorption edges of quantified elements. In this way, a decay behavior for the concentration differences between preparation methods and the energies of the X-ray absorption edges of each element were observed. The observed behaviors were modeled with exponential decay functions obtaining R2 correlation coefficients from 0.989 to 0.992. The strong absorption effect observed, and even possible matrix effect, can be explained by the inherent high organic content of the evaluated samples and also by the morphology and average thickness of the TXRF depositions observed. As main conclusion of this work, the analysis of light elements in samples with high organic content by TXRF, i.e. medical, biological, food or any other organic matrixes should be taken carefully. In any case, the direct analysis is not recommended and a previous microwave-assisted acid digestion, or similar, is mandatory, for the correct elemental quantification by TXRF.

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, Carl A.; Johnson, Wayne F.; Walker, William A.

1988-01-01

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises (1) a whole blood sample disc, (2) a serum sample disc, (3) a sample preparation rotor, and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc in capillary tubes filled by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analytical rotor for analysis by conventional methods.

An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins

PubMed Central

Cigić, Irena Kralj; Prosen, Helena

2009-01-01

Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass spectrometric detection, while in the field of sample preparation various solid-phase extraction approaches are discussed. However, an overview of other analytical and sample preparation methods less often used is also given. Finally, different matrices where mycotoxins have to be determined are discussed with the emphasis on their specific characteristics important for the analysis (human food and beverages, animal feed, biological samples, environmental samples). Various issues important for accurate qualitative and quantitative analyses are critically discussed: sampling and choice of representative sample, sample preparation and possible bias associated with it, specificity of the analytical method and critical evaluation of results. PMID:19333436

Impact of Oriented Clay Particles on X-Ray Spectroscopy Analysis

NASA Astrophysics Data System (ADS)

Lim, A. J. M. S.; Syazwani, R. N.; Wijeyesekera, D. C.

2016-07-01

Understanding the engineering properties of the mineralogy and microfabic of clayey soils is very complex and thus very difficult for soil characterization. Micromechanics of soils recognize that the micro structure and mineralogy of clay have a significant influence on its engineering behaviour. To achieve a more reliable quantitative evaluation of clay mineralogy, a proper sample preparation technique for quantitative clay mineral analysis is necessary. This paper presents the quantitative evaluation of elemental analysis and chemical characterization of oriented and random oriented clay particles using X-ray spectroscopy. Three different types of clays namely marine clay, bentonite and kaolin clay were studied. The oriented samples were prepared by placing the dispersed clay in water and left to settle on porous ceramic tiles by applying a relatively weak suction through a vacuum pump. Images form a Scanning Electron Microscope (SEM) was also used to show the comparison between the orientation patterns of both the sample preparation techniques. From the quantitative analysis of the X-ray spectroscopy, oriented sampling method showed more accuracy in identifying mineral deposits, because it produced better peak intensity on the spectrum and more mineral content can be identified compared to randomly oriented samples.

The effects of sample preparation on measured concentrations of eight elements in edible tissues of fish from streams contaminated by lead mining

USGS Publications Warehouse

Schmitt, Christopher J.; Finger, Susan E.

1987-01-01

The influence of sample preparation on measured concentrations of eight elements in the edible tissues of two black basses (Centrarchidae), two catfishes (Ictaluridae), and the black redhorse,Moxostoma duquesnei (Catostomidae) from two rivers in southeastern Missouri contaminated by mining and related activities was investigated. Concentrations of Pb, Cd, Cu, Zn, Fe, Mn, Ba, and Ca were measured in two skinless, boneless samples of axial muscle from individual fish prepared in a clean room. One sample (normally-processed) was removed from each fish with a knife in a manner typically used by investigators to process fish for elemental analysis and presumedly representative of methods employed by anglers when preparing fish for home consumption. A second sample (clean-processed) was then prepared from each normally-processed sample by cutting away all surface material with acid-cleaned instruments under ultraclean conditions. The samples were analyzed as a single group by atomic absorption spectrophotometry. Of the elements studied, only Pb regularly exceeded current guidelines for elemental contaminants in foods. Concentrations were high in black redhorse from contaminated sites, regardless of preparation method; for the other fishes, whether or not Pb guidelines were exceeded depended on preparation technique. Except for Mn and Ca, concentrations of all elements measured were significantly lower in cleanthan in normally-processed tissue samples. Absolute differences in measured concentrations between clean- and normally-processed samples were most evident for Pb and Ba in bass and catfish and for Cd and Zn in redhorse. Regardless of preparation method, concentrations of Pb, Ca, Mn, and Ba in individual fish were closely correlated; samples that were high or low in one of these four elements were correspondingly high or low in the other three. In contrast, correlations between Zn, Fe, and Cd occurred only in normallyprocessed samples, suggesting that these correlations resulted from high concentrations on the surfaces of some samples. Concentrations of Pb and Ba in edible tissues of fish from contaminated sites were highly correlated with Ca content, which was probably determined largely by the amount of tissue other than muscle in the sample because fish muscle contains relatively little Ca. Accordingly, variation within a group of similar samples can be reduced by normalizing Pb and Ba concentrations to a standard Ca concentration. When sample size (N) is large, this can be accomplished statistically by analysis of covariance; whenN is small, molar ratios of [Pb]/[Ca] and [Ba]/[Ca] can be computed. Without such adjustments, unrealistically large Ns are required to yield statistically reliable estimates of Pb concentrations in edible tissues. Investigators should acknowledge that reported concentrations of certain elements are only estimates, and that regardless of the care exercised during the collection, preparation, and analysis of samples, results should be interpreted with the awareness that contamination from external sources may have occurred.

The effects of crosslinkers on physical, mechanical, and cytotoxic properties of gelatin sponge prepared via in-situ gas foaming method as a tissue engineering scaffold.

PubMed

Poursamar, S Ali; Lehner, Alexander N; Azami, Mahmoud; Ebrahimi-Barough, Somayeh; Samadikuchaksaraei, Ali; Antunes, A P M

2016-06-01

In this study porous gelatin scaffolds were prepared using in-situ gas foaming, and four crosslinking agents were used to determine a biocompatible and effective crosslinker that is suitable for such a method. Crosslinkers used in this study included: hexamethylene diisocyanate (HMDI), poly(ethylene glycol) diglycidyl ether (epoxy), glutaraldehyde (GTA), and genipin. The prepared porous structures were analyzed using Fourier Transform Infrared Spectroscopy (FT-IR), thermal and mechanical analysis as well as water absorption analysis. The microstructures of the prepared samples were analyzed using Scanning Electron Microscopy (SEM). The effects of the crosslinking agents were studied on the cytotoxicity of the porous structure indirectly using MTT analysis. The affinity of L929 mouse fibroblast cells for attachment on the scaffold surfaces was investigated by direct cell seeding and DAPI-staining technique. It was shown that while all of the studied crosslinking agents were capable of stabilizing prepared gelatin scaffolds, there are noticeable differences among physical and mechanical properties of samples based on the crosslinker type. Epoxy-crosslinked scaffolds showed a higher capacity for water absorption and more uniform microstructures than the rest of crosslinked samples, whereas genipin and GTA-crosslinked scaffolds demonstrated higher mechanical strength. Cytotoxicity analysis showed the superior biocompatibility of the naturally occurring genipin in comparison with other synthetic crosslinking agents, in particular relative to GTA-crosslinked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A robust and fast method of sampling and analysis of delta13C of dissolved inorganic carbon in ground waters.

PubMed

Spötl, Christoph

2005-09-01

The stable carbon isotopic composition of dissolved inorganic carbon (delta13C(DIC)) is traditionally determined using either direct precipitation or gas evolution methods in conjunction with offline gas preparation and measurement in a dual-inlet isotope ratio mass spectrometer. A gas evolution method based on continuous-flow technology is described here, which is easy to use and robust. Water samples (100-1500 microl depending on the carbonate alkalinity) are injected into He-filled autosampler vials in the field and analysed on an automated continuous-flow gas preparation system interfaced to an isotope ratio mass spectrometer. Sample analysis time including online preparation is 10 min and overall precision is 0.1 per thousand. This method is thus fast and can easily be automated for handling large sample batches.

Sample preparation: a critical step in the analysis of cholesterol oxidation products.

PubMed

Georgiou, Christiana A; Constantinou, Michalis S; Kapnissi-Christodoulou, Constantina P

2014-02-15

In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity. Copyright © 2013 Elsevier Ltd. All rights reserved.

Urea free and more efficient sample preparation method for mass spectrometry based protein identification via combining the formic acid-assisted chemical cleavage and trypsin digestion.

PubMed

Wu, Shuaibin; Yang, Kaiguang; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2011-10-30

A formic acid (FA)-assisted sample preparation method was presented for protein identification via mass spectrometry (MS). Detailedly, an aqueous solution containing 2% FA and dithiothreitol was selected to perform protein denaturation, aspartic acid (D) sites cleavage and disulfide linkages reduction simultaneously at 108°C for 2h. Subsequently, FA wiped off via vacuum concentration. Finally, iodoacetamide (IAA) alkylation and trypsin digestion could be performed ordinally. A series of model proteins (BSA, β-lactoglobulin and apo-Transferrin) were treated respectively using such method, followed by matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS) analysis. The identified peptide number was increased by ∼ 80% in comparison with the conventional urea-assisted sample preparation method. Moreover, BSA identification was achieved efficiently down to femtomole (25 ± 0 sequence coverage and 16 ± 1 peptides) via such method. In contrast, there were not peptides identified confidently via the urea-assisted method before desalination via the C18 zip tip. The absence of urea in this sample preparation method was an advantage for the more favorable digestion and MALDI-TOF MS analysis. The performances of two methods for the real sample (rat liver proteome) were also compared, followed by a nanoflow reversed-phase liquid chromatography with electrospray ionization tandem mass spectrometry system analysis. As a result, 1335 ± 43 peptides were identified confidently (false discovery rate <1%) via FA-assisted method, corresponding to 295 ± 12 proteins (of top match=1 and requiring 2 unique peptides at least). In contrast, there were only 1107 ± 16 peptides (corresponding to 231 ± 10 proteins) obtained from the conventional urea-assisted method. It was serving as a more efficient protein sample preparation method for researching specific proteomes better, and providing assistance to develop other proteomics analysis methods, such as, peptide quantitative analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Optimization for Peptide Sample Preparation for Urine Peptidomics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan

2014-02-25

Analysis of native or endogenous peptides in biofluids can provide valuable insights into disease mechanisms. Furthermore, the detected peptides may also have utility as potential biomarkers for non-invasive monitoring of human diseases. The non-invasive nature of urine collection and the abundance of peptides in the urine makes analysis by high-throughput ‘peptidomics’ methods , an attractive approach for investigating the pathogenesis of renal disease. However, urine peptidomics methodologies can be problematic with regards to difficulties associated with sample preparation. The urine matrix can provide significant background interference in making the analytical measurements that it hampers both the identification of peptides andmore » the depth of the peptidomics read when utilizing LC-MS based peptidome analysis. We report on a novel adaptation of the standard solid phase extraction (SPE) method to a modified SPE (mSPE) approach for improved peptide yield and analysis sensitivity with LC-MS based peptidomics in terms of time, cost, clogging of the LC-MS column, peptide yield, peptide quality, and number of peptides identified by each method. Expense and time requirements were comparable for both SPE and mSPE, but more interfering contaminants from the urine matrix were evident in the SPE preparations (e.g., clogging of the LC-MS columns, yellowish background coloration of prepared samples due to retained urobilin, lower peptide yields) when compared to the mSPE method. When we compared data from technical replicates of 4 runs, the mSPE method provided significantly improved efficiencies for the preparation of samples from urine (e.g., mSPE peptide identification 82% versus 18% with SPE; p = 8.92E-05). Additionally, peptide identifications, when applying the mSPE method, highlighted the biology of differential activation of urine peptidases during acute renal transplant rejection with distinct laddering of specific peptides, which was obscured for most proteins when utilizing the conventional SPE method. In conclusion, the mSPE method was found to be superior to the conventional, standard SPE method for urine peptide sample preparation when applying LC-MS peptidomics analysis due to the optimized sample clean up that provided improved experimental inference from the confidently identified peptides.« less

An automation-assisted generic approach for biological sample preparation and LC-MS/MS method validation.

PubMed

Zhang, Jie; Wei, Shimin; Ayres, David W; Smith, Harold T; Tse, Francis L S

2011-09-01

Although it is well known that automation can provide significant improvement in the efficiency of biological sample preparation in quantitative LC-MS/MS analysis, it has not been widely implemented in bioanalytical laboratories throughout the industry. This can be attributed to the lack of a sound strategy and practical procedures in working with robotic liquid-handling systems. Several comprehensive automation assisted procedures for biological sample preparation and method validation were developed and qualified using two types of Hamilton Microlab liquid-handling robots. The procedures developed were generic, user-friendly and covered the majority of steps involved in routine sample preparation and method validation. Generic automation procedures were established as a practical approach to widely implement automation into the routine bioanalysis of samples in support of drug-development programs.

14C sample preparation for AMS microdosing studies at Lund University using online combustion and septa-sealed vials

NASA Astrophysics Data System (ADS)

Sydoff, Marie; Stenström, Kristina

2010-04-01

The Department of Physics at Lund University is participating in a European Union project called EUMAPP (European Union Microdose AMS Partnership Programme), in which sample preparation and accelerator mass spectrometry (AMS) measurements of biological samples from microdosing studies have been made. This paper describes a simplified method of converting biological samples to solid graphite for 14C analysis with AMS. The method is based on online combustion of the samples, and reduction of CO 2 in septa-sealed vials. The septa-sealed vials and disposable materials are used to eliminate sample cross-contamination. Measurements of ANU and Ox I standards show deviations of 2% and 3%, respectively, relative to reference values. This level of accuracy is sufficient for biological samples from microdosing studies. Since the method has very few handling steps from sample to graphite, the risk of failure during the sample preparation process is minimized, making the method easy to use in routine preparation of samples.

Evaluation of automated sample preparation, retention time locked gas chromatography-mass spectrometry and data analysis methods for the metabolomic study of Arabidopsis species.

PubMed

Gu, Qun; David, Frank; Lynen, Frédéric; Rumpel, Klaus; Dugardeyn, Jasper; Van Der Straeten, Dominique; Xu, Guowang; Sandra, Pat

2011-05-27

In this paper, automated sample preparation, retention time locked gas chromatography-mass spectrometry (GC-MS) and data analysis methods for the metabolomics study were evaluated. A miniaturized and automated derivatisation method using sequential oximation and silylation was applied to a polar extract of 4 types (2 types×2 ages) of Arabidopsis thaliana, a popular model organism often used in plant sciences and genetics. Automation of the derivatisation process offers excellent repeatability, and the time between sample preparation and analysis was short and constant, reducing artifact formation. Retention time locked (RTL) gas chromatography-mass spectrometry was used, resulting in reproducible retention times and GC-MS profiles. Two approaches were used for data analysis. XCMS followed by principal component analysis (approach 1) and AMDIS deconvolution combined with a commercially available program (Mass Profiler Professional) followed by principal component analysis (approach 2) were compared. Several features that were up- or down-regulated in the different types were detected. Copyright © 2011 Elsevier B.V. All rights reserved.

Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhandari, Deepak; Van Berkel, Gary J

2012-01-01

The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45more » min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.« less

Improved chip design for integrated solid-phase microextraction in on-line proteomic sample preparation.

PubMed

Bergkvist, Jonas; Ekström, Simon; Wallman, Lars; Löfgren, Mikael; Marko-Varga, György; Nilsson, Johan; Laurell, Thomas

2002-04-01

A recently introduced silicon microextraction chip (SMEC), used for on-line proteomic sample preparation, has proved to facilitate the process of protein identification by sample clean up and enrichment of peptides. It is demonstrated that a novel grid-SMEC design improves the operating characteristics for solid-phase microextraction, by reducing dispersion effects and thereby improving the sample preparation conditions. The structures investigated in this paper are treated both numerically and experimentally. The numerical approach is based on finite element analysis of the microfluidic flow in the microchip. The analysis is accomplished by use of the computational fluid dynamics-module FLOTRAN in the ANSYS software package. The modeling and analysis of the previously reported weir-SMEC design indicates some severe drawbacks, that can be reduced by changing the microextraction chip geometry to the grid-SMEC design. The overall analytical performance was thereby improved and also verified by experimental work. Matrix-assisted laser desorption/ionization mass spectra of model peptides extracted from both the weir-SMEC and the new grid-SMEC support the numerical analysis results. Further use of numerical modeling and analysis of the SMEC structures is also discussed and suggested in this work.

Thermoluminescence property of nano scale Al{sub 2}O{sub 3}: C by combustion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bharthasaradhi, R.; Nehru, L. C.

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 samplemore » showed an isolated peak at around 200°C. The result suggest the prepared nanopowder is suitable for medical radiation dosimetry.« less

La 2-xSr xCuO 4-δ superconducting samples prepared by the wet-chemical method

NASA Astrophysics Data System (ADS)

Loose, A.; Gonzalez, J. L.; Lopez, A.; Borges, H. A.; Baggio-Saitovitch, E.

2009-10-01

In this work, we report on the physical properties of good-quality polycrystalline superconducting samples of La 2-xSr xCu 1-yZn yO 4-δ ( y=0, 0.02) prepared by a wet-chemical method, focusing on the temperature dependence of the critical current. Using the wet-chemical method, we were able to produce samples with improved homogeneity compared to the solid-state method. A complete set of samples with several carrier concentrations, ranging from the underdoped (strontium concentration x≈0.05) to the highly overdoped ( x≈0.25) region, were prepared and investigated. The X-ray diffraction analysis, zero-field cooling magnetization and electrical resistivity measurements were reported on earlier. The structural parameters of the prepared samples seem to be slightly modified by the preparation method and their critical temperatures were lower than reported in the literature. The temperature dependence of the critical current was explained by a theoretical model which took the granular structure of the samples into account.

Transport Properties of ZnSe- ITO Hetero Junction

NASA Astrophysics Data System (ADS)

Ichibakase, Tsuyoshi

In this report, ITO(Indium Tin Oxide) was used on the glass substrates as the transparent electrode, and ZnSe layer was prepared by the vacuum deposition on this ITO. Then, the electrical characteristics of this sample were investigated by mans of the electric current transport analysis. The sample that ZnSe was prepared as 3.4 μm in case of ITO-ZnSe sample, has high density level at the junction surface. The ITO-ZnSe junction has two type of diffusion current. However, the ITO-ZnSe sample that ZnSe layer was prepared as 0.1 μm can be assumed as the ohmic contact, and ITO-ZnSe(0.1μm) -CdTe sample shows the avalanche breakdown, and it is considered that the avalanche breakdown occurs in CdTe layer. It is difficult to occur the avalanche breakdown, if ZnSe-CdTe junction has high-density level and CdTe layer has high-density defect. Hence, the ZnSe-CdTe sample that CdTe layer was prepared on ITO-ZnSe(0.1μm) substrate has not high-density level at the junction surface, and the CdTe layer with little lattice imperfection can be prepared. It found that ITO-ZnSe(0.1μm) substrate is available for the II-VI compounds semiconductor device through above analysis result.

Standardization of a traditional polyherbo-mineral formulation - Brahmi vati.

PubMed

Mishra, Amrita; Mishra, Arun K; Ghosh, Ashoke K; Jha, Shivesh

2013-01-01

The present study deals with standardization of an in-house standard preparation and three marketed samples of Brahmi vati, which is a traditional medicine known to be effective in mental disorders, convulsions, weak memory, high fever and hysteria. Preparation and standardization have been done by following modern scientific quality control procedures for raw material and the finished products. The scanning electron microscopic (SEM) analysis showed the reduction of metals and minerals (particle size range 2-5 µm) which indicates the proper preparation of bhasmas, the important ingredient of Brahmi vati. Findings of EDX analysis of all samples of Brahmi vati suggested the absence of Gold, an important constituent of Brahmi vati in two marketed samples. All the samples of Brahmi vati were subjected to quantitative estimation of Bacoside A (marker compound) by HPTLC technique. Extraction of the samples was done in methanol and the chromatograms were developed in Butanol: Glacial acetic acid: water (4.5:0.5:5 v/v) and detected at 225nm. The regression analysis of calibration plots of Bacoside A exhibited linear relationship in the concentration range of 50-300 ng, while the % recovery was found to be 96.06% w/w, thus proving the accuracy and precision of the analysis. The Bacoside A content in the in-house preparation was found to be higher than that of the commercial samples. The proposed HPTLC method was found to be rapid, simple and accurate for quantitative estimation of Bacoside A in different formulations. The results of this study could be used as a model data in the standardization of Brahmi vati.

Preparation and Characterization of Natural Rubber/Organophilic Clay Nanocomposites

NASA Astrophysics Data System (ADS)

Gonzales-Fernandes, M.; Esper, F. J.; Silva-Valenzuela, M. G.; Martín-Cortés, G. R.; Valenzuela-Diaz, F. R.; Wiebeck, H.

Natural rubber/organophilic clay nanocomposites were prepared and characterized. A brown bentonite from Paraiba's State, Brazil was modified with a sodium salt and treated with quaternary ammonium salt hexadecyltrimethyl ammonium chloride. The clay in its natural state, after cation exchange with sodium and after organophilization was characterized by XRD, IR, SEM, thermal analysis. Nanocomposite samples were prepared containing 10 resin percent of organophilic clay. The vulcanized samples were analyzed by XRD, SEM. The nanocomposites obtained showed improvement in their mechanical properties in comparison with samples without clay.

Determination of benzylpenicillin in pharmaceuticals by capillary zone electrophoresis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoyt, A.M. Jr.; Sepaniak, M.J.

A rapid and direct method is described for the determination of benzylpenicillin (penicillin G) in pharmaceutical preparations. The method involves very little sample preparation and total analysis time for duplicate results is less 30 minutes per sample. The method takes advantage of the speed and separating power of capillary zone electrophoresis (CZE). Detection of penicillin is by absorption at 228 nm. An internal standard is employed to reduce sample injection error. The method was applied successfully to both tablets and injectable preparations. 14 refs., 5 figs., 3 tabs.

Comparison of sample preparation techniques and data analysis for the LC-MS/MS-based identification of proteins in human follicular fluid.

PubMed

Lehmann, Roland; Schmidt, André; Pastuschek, Jana; Müller, Mario M; Fritzsche, Andreas; Dieterle, Stefan; Greb, Robert R; Markert, Udo R; Slevogt, Hortense

2018-06-25

The proteomic analysis of complex body fluids by liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis requires the selection of suitable sample preparation techniques and optimal parameter settings in data analysis software packages to obtain reliable results. Proteomic analysis of follicular fluid, as a representative of a complex body fluid similar to serum or plasma, is difficult as it contains a vast amount of high abundant proteins and a variety of proteins with different concentrations. However, the accessibility of this complex body fluid for LC-MS/MS analysis is an opportunity to gain insights into the status, the composition of fertility-relevant proteins including immunological factors or for the discovery of new diagnostic and prognostic markers for, for example, the treatment of infertility. In this study, we compared different sample preparation methods (FASP, eFASP and in-solution digestion) and three different data analysis software packages (Proteome Discoverer with SEQUEST, Mascot and MaxQuant with Andromeda) combined with semi- and full-tryptic databank search options to obtain a maximum coverage of the follicular fluid proteome. We found that the most comprehensive proteome coverage is achieved by the eFASP sample preparation method using SDS in the initial denaturing step and the SEQUEST-based semi-tryptic data analysis. In conclusion, we have developed a fractionation-free methodical workflow for in depth LC-MS/MS-based analysis for the standardized investigation of human follicle fluid as an important representative of a complex body fluid. Taken together, we were able to identify a total of 1392 proteins in follicular fluid. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

A Coordinated Focused Ion Beam/Ultramicrotomy Technique for Serial Sectioning of Hayabusa Particles and Other Returned Samples

NASA Technical Reports Server (NTRS)

Berger, E. L.; Keller, L. P.

2014-01-01

Recent sample return missions, such as NASA's Stardust mission to comet 81P/Wild 2 and JAXA's Hayabusa mission to asteroid 25143 Itokawa, have returned particulate samples (typically 5-50 µm) that pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on how the samples are prepared for analysis. This also holds true for other extraterrestrial materials, including interplanetary dust particles, micrometeorites and lunar regolith grains. Traditionally, particulate samples have been prepared using microtomy techniques (e.g., [1]). However, for hard mineral particles ?20 µm, microtome thin sections are compromised by severe chatter and sample loss. For these difficult samples, we have developed a hybrid technique that combines traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for the in situ investigation of grain surfaces and interiors. Using this method, we have increased the number of FIB-SEM prepared sections that can be recovered from a particle with dimensions on the order of tens of µms. These sections can be subsequently analyzed using a variety of electron beam techniques. Here, we demonstrate this sample preparation technique on individual lunar regolith grains in order to study their space-weathered surfaces. We plan to extend these efforts to analyses of individual Hayabusa samples.

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992–2010

USGS Publications Warehouse

Martin, Jeffrey D.; Eberle, Michael; Nakagaki, Naomi

2011-01-01

This report updates a previously published water-quality dataset of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through September 2010 at stream-water sites of the U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) Program and the National Stream Quality Accounting Network (NASQAN) were compiled, reviewed, selected, and prepared for trend analysis. The principal steps in data review for trend analysis were to (1) identify analytical schedule, (2) verify sample-level coding, (3) exclude inappropriate samples or results, (4) review pesticide detections per sample, (5) review high pesticide concentrations, and (6) review the spatial and temporal extent of NAWQA pesticide data and selection of analytical methods for trend analysis. The principal steps in data preparation for trend analysis were to (1) select stream-water sites for trend analysis, (2) round concentrations to a consistent level of precision for the concentration range, (3) identify routine reporting levels used to report nondetections unaffected by matrix interference, (4) reassign the concentration value for routine nondetections to the maximum value of the long-term method detection level (maxLT-MDL), (5) adjust concentrations to compensate for temporal changes in bias of recovery of the gas chromatography/mass spectrometry (GCMS) analytical method, and (6) identify samples considered inappropriate for trend analysis. Samples analyzed at the USGS National Water Quality Laboratory (NWQL) by the GCMS analytical method were the most extensive in time and space and, consequently, were selected for trend analysis. Stream-water sites with 3 or more water years of data with six or more samples per year were selected for pesticide trend analysis. The selection criteria described in the report produced a dataset of 21,988 pesticide samples at 212 stream-water sites. Only 21,144 pesticide samples, however, are considered appropriate for trend analysis.

Elimination of ``memory`` from sample handling and inlet system of a mass spectrometer

DOEpatents

Chastgner, P.

1991-05-08

This paper describes a method for preparing the sample handling and inlet system of a mass spectrometer for analysis of a subsequent sample following analysis of a previous sample comprising the flushing of the system interior with supercritical CO{sub 2} and venting the interior. The method eliminates the effect of system ``memory`` on the subsequent analysis, especially following persistent samples such as xenon and krypton.

Methods for Determining Particle Size Distributions from Nuclear Detonations.

DTIC Science & Technology

1987-03-01

Debris . . . 30 IV. Summary of Sample Preparation Method . . . . 35 V. Set Parameters for PCS ... ........... 39 VI. Analysis by Vendors...54 XV. Results From Brookhaven Analysis Using The Method of Cumulants ... ........... . 54 XVI. Results From Brookhaven Analysis of Sample...R-3 Using Histogram Method ......... .55 XVII. Results From Brookhaven Analysis of Sample R-8 Using Histogram Method ........... 56 XVIII.TEM Particle

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Dielectrophoresis-Based Sample Handling in General-Purpose Programmable Diagnostic Instruments

PubMed Central

Gascoyne, Peter R. C.; Vykoukal, Jody V.

2009-01-01

As the molecular origins of disease are better understood, the need for affordable, rapid, and automated technologies that enable microscale molecular diagnostics has become apparent. Widespread use of microsystems that perform sample preparation and molecular analysis could ensure that the benefits of new biomedical discoveries are realized by a maximum number of people, even those in environments lacking any infrastructure. While progress has been made in developing miniaturized diagnostic systems, samples are generally processed off-device using labor-intensive and time-consuming traditional sample preparation methods. We present the concept of an integrated programmable general-purpose sample analysis processor (GSAP) architecture where raw samples are routed to separation and analysis functional blocks contained within a single device. Several dielectrophoresis-based methods that could serve as the foundation for building GSAP functional blocks are reviewed including methods for cell and particle sorting, cell focusing, cell ac impedance analysis, cell lysis, and the manipulation of molecules and reagent droplets. PMID:19684877

Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review.

PubMed

Tankiewicz, Maciej; Fenik, Jolanta; Biziuk, Marek

2011-10-30

The intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to monitor pesticide residues in the environment with the aid of all accessible analytical methods. The analysis of samples for the presence of pesticides is problematic, because of the laborious and time-consuming operations involved in preparing samples for analysis, which themselves may be a source of additional contaminations and errors. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solventless and solvent-minimized techniques are coming into use. This paper discusses the most commonly used over the last 15 years sample preparation techniques for monitoring organophosphorus and organonitrogen pesticides residue in water samples. Furthermore, a significant trend in sample preparation, in accordance with the principles of 'Green Chemistry' is the simplification, miniaturization and automation of analytical techniques. In view of this aspect, several novel techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. The paper describes extraction techniques requiring the use of solvents - liquid-liquid extraction (LLE) and its modifications, membrane extraction techniques, hollow fibre-protected two-phase solvent microextraction, liquid phase microextraction based on the solidification of a floating organic drop (LPME-SFO), solid-phase extraction (SPE) and single-drop microextraction (SDME) - as well as solvent-free techniques - solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The advantages and drawbacks of these techniques are also discussed, and some solutions to their limitations are proposed. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

PubMed

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

Movement of moisture in refrigerated cheese samples transferred to room temperature.

PubMed

Emmons, D B; Bradley, R L; Campbell, C; Sauvé, J P

2001-01-01

When cheese samples refrigerated at 4 degrees C in 120 mL plastic tubs were transferred to room temperature at 23 degrees C, moisture began to move from the warmer surface to the cooler interior; the difference after 1 h was 0.2-0.4%. Others had observed that moisture moved from the interior of warmer blocks of cheese to the cooler surface during cooling at the end of cheese manufacture. In loosely packed cheese prepared for analysis, part of the moisture movement may have been due to evaporation from the warmer surface and condensation on the cooler cheese. It is recommended that cheese be prepared for analysis immediately before weighing. Cheese samples that have been refrigerated, as in interlaboratory trials, should also be remixed or prepared again.

Simultaneous quantitation of 14 active components in Yinchenhao decoction by using ultra high performance liquid chromatography with diode array detection: Method development and ingredient analysis of different commonly prepared samples.

PubMed

Yi, YaXiong; Zhang, Yong; Ding, Yue; Lu, Lu; Zhang, Tong; Zhao, Yuan; Xu, XiaoJun; Zhang, YuXin

2016-11-01

We developed a novel quantitative analysis method based on ultra high performance liquid chromatography coupled with diode array detection for the simultaneous determination of the 14 main active components in Yinchenhao decoction. All components were separated on an Agilent SB-C18 column by using a gradient solvent system of acetonitrile/0.1% phosphoric acid solution at a flow rate of 0.4 mL/min for 35 min. Subsequently, linearity, precision, repeatability, and accuracy tests were implemented to validate the method. Furthermore, the method has been applied for compositional difference analysis of 14 components in eight normal-extraction Yinchenhao decoction samples, accompanied by hierarchical clustering analysis and similarity analysis. The result that all samples were divided into three groups based on different contents of components demonstrated that extraction methods of decocting, refluxing, ultrasonication and extraction solvents of water or ethanol affected component differentiation, and should be related to its clinical applications. The results also indicated that the sample prepared by patients in the family by using water extraction employing a casserole was almost same to that prepared using a stainless-steel kettle, which is mostly used in pharmaceutical factories. This research would help patients to select the best and most convenient method for preparing Yinchenhao decoction. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative Analysis of Therapeutic Drugs in Dried Blood Spot Samples by Paper Spray Mass Spectrometry: An Avenue to Therapeutic Drug Monitoring

NASA Astrophysics Data System (ADS)

Manicke, Nicholas Edward; Abu-Rabie, Paul; Spooner, Neil; Ouyang, Zheng; Cooks, R. Graham

2011-09-01

A method is presented for the direct quantitative analysis of therapeutic drugs from dried blood spot samples by mass spectrometry. The method, paper spray mass spectrometry, generates gas phase ions directly from the blood card paper used to store dried blood samples without the need for complex sample preparation and separation; the entire time for preparation and analysis of blood samples is around 30 s. Limits of detection were investigated for a chemically diverse set of some 15 therapeutic drugs; hydrophobic and weakly basic drugs, such as sunitinib, citalopram, and verapamil, were found to be routinely detectable at approximately 1 ng/mL. Samples were prepared by addition of the drug to whole blood. Drug concentrations were measured quantitatively over several orders of magnitude, with accuracies within 10% of the expected value and relative standard deviation (RSD) of around 10% by prespotting an internal standard solution onto the paper prior to application of the blood sample. We have demonstrated that paper spray mass spectrometry can be used to quantitatively measure drug concentrations over the entire therapeutic range for a wide variety of drugs. The high quality analytical data obtained indicate that the technique may be a viable option for therapeutic drug monitoring.

Post-irradiation-examination of irradiated fuel outside the hot cell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dawn E. Janney; Adam B. Robinson; Thomas P. O'Holleran

Because of their high radioactivity, irradiated fuels are commonly examined in a hot cell. However, the Idaho National Laboratory (INL) has recently investigated irradiated U-Mo-Al metallic fuel from the Reduced Enrichment for Research and Test Reactors (RERTR) project using a conventional unshielded scanning electron microscope outside a hot cell. This examination was possible because of a two-step sample-preparation approach in which a small volume of fuel was isolated in a hot cell and shielding was introduced during later stages of sample preparation. The resulting sample contained numerous sample-preparation artifacts but allowed analysis of microstructures from selected areas.

Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives.

PubMed

Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna; Chidambara, Vinayaka Aaydha; Wolff, Anders; Bang, Dang Duong; Sun, Yi

2017-05-15

Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions. MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given. Copyright © 2017 Elsevier B.V. All rights reserved.

Protein identification and quantification from riverbank grape, Vitis riparia: Comparing SDS-PAGE and FASP-GPF techniques for shotgun proteomic analysis.

PubMed

George, Iniga S; Fennell, Anne Y; Haynes, Paul A

2015-09-01

Protein sample preparation optimisation is critical for establishing reproducible high throughput proteomic analysis. In this study, two different fractionation sample preparation techniques (in-gel digestion and in-solution digestion) for shotgun proteomics were used to quantitatively compare proteins identified in Vitis riparia leaf samples. The total number of proteins and peptides identified were compared between filter aided sample preparation (FASP) coupled with gas phase fractionation (GPF) and SDS-PAGE methods. There was a 24% increase in the total number of reproducibly identified proteins when FASP-GPF was used. FASP-GPF is more reproducible, less expensive and a better method than SDS-PAGE for shotgun proteomics of grapevine samples as it significantly increases protein identification across biological replicates. Total peptide and protein information from the two fractionation techniques is available in PRIDE with the identifier PXD001399 (http://proteomecentral.proteomexchange.org/dataset/PXD001399). © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

PubMed

Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

2016-02-01

Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

Recombinant Intrinsically Disordered Proteins for NMR: Tips and Tricks.

PubMed

Calçada, Eduardo O; Korsak, Magdalena; Kozyreva, Tatiana

2015-01-01

The growing recognition of the several roles that intrinsically disordered proteins play in biology places an increasing importance on protein sample availability to allow the characterization of their structural and dynamic properties. The sample preparation is therefore the limiting step to allow any biophysical method being able to characterize the properties of an intrinsically disordered protein and to clarify the links between these properties and the associated biological functions. An increasing array of tools has been recruited to help prepare and characterize the structural and dynamic properties of disordered proteins. This chapter describes their sample preparation, covering the most common drawbacks/barriers usually found working in the laboratory bench. We want this chapter to be the bedside book of any scientist interested in preparing intrinsically disordered protein samples for further biophysical analysis.

Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method

NASA Astrophysics Data System (ADS)

Wang, Shifa; Li, Danming; Xiao, Yuhua; Dang, Wenqiang; Feng, Jie

2017-10-01

A modified polyacrylamide gel route was used to prepare SrFe12O19 magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe12O19 magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm-1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe12O19 magnetic nanoparticles are uniform with the mean particle size of 60 nm. VSM measurement shows that the maximum magnetic energy product (BH)max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.

Comparison of Dilution, Filtration, and Microwave Digestion Sample Pretreatments in Elemental Profiling of Wine by ICP-MS.

PubMed

Godshaw, Joshua; Hopfer, Helene; Nelson, Jenny; Ebeler, Susan E

2017-09-25

Wine elemental composition varies by cultivar, geographic origin, viticultural and enological practices, and is often used for authenticity validation. Elemental analysis of wine by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging due to the potential for non-spectral interferences and plasma instability arising from organic matrix components. Sample preparation mitigates these interferences, however, conflicting recommendations of best practices in ICP-MS analysis of wine have been reported. This study compared direct dilution, microwave-assisted acid digestion, and two filtration sample pretreatments, acidification prior to filtration and filtration followed by acidification, in elemental profiling of one white and three red table wines by ICP-MS. Of 43 monitored isotopes, 37 varied by sample preparation method, with significantly higher results of 17 isotopes in the microwave-digested samples. Both filtration treatments resulted in lower results for 11 isotopes compared to the other methods. Finally, isotope dilution determination of copper based on natural abundances and the 63 Cu: 65 Cu instrument response ratio agreed with external calibration and confirmed a significant sample preparation effect. Overall, microwave digestion did not compare favorably, and direct dilution was found to provide the best compromise between ease of use and result accuracy and precision, although all preparation strategies were able to differentiate the wines.

Time of flight secondary ion mass spectrometry of bone—Impact of sample preparation and measurement conditions

PubMed Central

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-01-01

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein. PMID:26253108

Time of flight secondary ion mass spectrometry of bone-Impact of sample preparation and measurement conditions.

PubMed

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-06-07

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein.

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

DOE PAGES

Adamic, M. L.; Lister, T. E.; Dufek, E. J.; ...

2015-03-25

This paper presents an evaluation of an alternate method for preparing environmental samples for 129I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Furthermore, precipitated silver iodide samples are usually mixed with niobium or silver powdermore » prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.« less

Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

DOEpatents

Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM

2011-07-26

There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

GUM Analysis for TIMS Isotopic Ratios in BEP0 Graphite Qualification Samples, Round 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gerlach, David C.; Heasler, Patrick G.; Reid, Bruce D.

In May 2007, one set of three samples from NBL were addressed to Steve Petersen for TIMS analysis, and included BEP0 samples numbered 27008, 30986, and 50846. All cores were trimmed by tooling, and lightly cleaned by CO2 pellet blasting. Small discs were cut from the second set of samples for SIMS analysis, with the remainder of each used for TIMS preparation.

Trace-element analysis of 1000 environmental samples per year using instrumental neutron activation analysis

NASA Technical Reports Server (NTRS)

Sheibley, D. W.

1974-01-01

The technology and methods developed at the Plum Brook Reactor to analyze 1000 samples per year and report data on as many as 56 elements are described. The manpower for the complete analysis of 20 to 24 samples per week required only 3 to 3.5 hours per sample. The solutions to problems encountered in sample preparation, irradiation, and counting are discussed. The automation of data reduction is described. Typical data on various sample matrices are presented.

A comparison between DART-MS and DSA-MS in the forensic analysis of writing inks.

PubMed

Drury, Nicholas; Ramotowski, Robert; Moini, Mehdi

2018-05-23

Ambient ionization mass spectrometry is gaining momentum in forensic science laboratories because of its high speed of analysis, minimal sample preparation, and information-rich results. One such application of ambient ionization methodology includes the analysis of writing inks from questioned documents where colorants of interest may not be soluble in common solvents, rendering thin layer chromatography (TLC) and separation-mass spectrometry methods such as LC/MS (-MS) impractical. Ambient ionization mass spectrometry uses a variety of ionization techniques such as penning ionization in Direct Analysis in Real Time (DART), and atmospheric pressure chemical ionization in Direct Sample Analysis (DSA), and electrospray ionization in Desorption Electrospray Ionization (DESI). In this manuscript, two of the commonly used ambient ionization techniques are compared: Perkin Elmer DSA-MS and IonSense DART in conjunction with a JEOL AccuTOF MS. Both technologies were equally successful in analyzing writing inks and produced similar spectra. DSA-MS produced less background signal likely because of its closed source configuration; however, the open source configuration of DART-MS provided more flexibility for sample positioning for optimum sensitivity and thereby allowing smaller piece of paper containing writing ink to be analyzed. Under these conditions, the minimum sample required for DART-MS was 1mm strokes of ink on paper, whereas DSA-MS required a minimum of 3mm. Moreover, both techniques showed comparable repeatability. Evaluation of the analytical figures of merit, including sensitivity, linear dynamic range, and repeatability, for DSA-MS and DART-MS analysis is provided. To the forensic context of the technique, DART-MS was applied to the analysis of United States Secret Service ink samples directly on a sampling mesh, and the results were compared with DSA-MS of the same inks on paper. Unlike analysis using separation mass spectrometry, which requires sample preparation, both DART-MS and DSA-MS successfully analyzed writing inks with minimal sample preparation. Copyright © 2018 Elsevier B.V. All rights reserved.

Study of the temperature dependent transport properties in nanocrystalline lithium lanthanum titanate for lithium ion batteries

NASA Astrophysics Data System (ADS)

Abhilash, K. P.; Christopher Selvin, P.; Nalini, B.; Somasundaram, K.; Sivaraj, P.; Chandra Bose, A.

2016-04-01

The nano-crystalline Li0.5La0.5TiO3 (LLTO) was prepared as an electrolyte material for lithium-ion batteries by the sol-gel method. The prepared LLTO material is characterized by structural, morphological and electrical characterizations. The LLTO shows the cubic perovskite structure with superlattice formation. The uniform distribution of LLTO particles has been analyzed by the SEM and TEM analysis of the sample. Impedance measurements at various temperatures were carried out and the temperature dependent conductivity of as prepared LLTO nanopowders at different temperatures from room temperature to 448 K has been analyzed. The transport mechanism has been analyzed using the dielectric and modulus analysis of the sample. Maximum grain conductivity of the order of 10-3 S cm-1 has been obtained for the sample at higher temperatures.

PLE in the analysis of plant compounds. Part I. The application of PLE for HPLC analysis of caffeine in green tea leaves.

PubMed

Dawidowicz, Andrzej L; Wianowska, Dorota

2005-04-29

A broad spectrum of sample preparation methods is currently used for the isolation of pharmacologically active compounds from plant and herbal materials. The paper compares the effectiveness of infusion, microwave assisted solvent extraction (MASE), matrix solid-phase dispersion (MSPD) and pressurised liquid extraction (PLE) as sample preparation methods for the isolation of caffeine from green tea leaves. The effect of PLE variables, such as extraction temperature, pressure and time, on the yield of caffeine from the investigated matrix is discussed. The obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly lower efficacy for caffeine isolation from green tea leaves. The evaluation of PLE conditions leads to the conclusion that elevated pressure applied in the PLE process is the factor hindering the extraction.

Phosphonium-based ionic liquids and uses

DOEpatents

Del Sesto, Rico E; Koppisch, Andrew T; Lovejoy, Katherine S; Purdy, Geraldine M

2014-12-30

Phosphonium-based room temperature ionic liquids ("RTILs") were prepared. They were used as matrices for Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry and also for preparing samples of dyes for analysis.

Use of direct versus indirect preparation data for assessing risk associated with airborne exposures at asbestos-contaminated sites.

PubMed

Goldade, Mary Patricia; O'Brien, Wendy Pott

2014-01-01

At asbestos-contaminated sites, exposure assessment requires measurement of airborne asbestos concentrations; however, the choice of preparation steps employed in the analysis has been debated vigorously among members of the asbestos exposure and risk assessment communities for many years. This study finds that the choice of preparation technique used in estimating airborne amphibole asbestos exposures for risk assessment is generally not a significant source of uncertainty. Conventionally, the indirect preparation method has been less preferred by some because it is purported to result in false elevations in airborne asbestos concentrations, when compared to direct analysis of air filters. However, airborne asbestos sampling in non-occupational settings is challenging because non-asbestos particles can interfere with the asbestos measurements, sometimes necessitating analysis via indirect preparation. To evaluate whether exposure concentrations derived from direct versus indirect preparation techniques differed significantly, paired measurements of airborne Libby-type amphibole, prepared using both techniques, were compared. For the evaluation, 31 paired direct and indirect preparations originating from the same air filters were analyzed for Libby-type amphibole using transmission electron microscopy. On average, the total Libby-type amphibole airborne exposure concentration was 3.3 times higher for indirect preparation analysis than for its paired direct preparation analysis (standard deviation = 4.1), a difference which is not statistically significant (p = 0.12, two-tailed, Wilcoxon signed rank test). The results suggest that the magnitude of the difference may be larger for shorter particles. Overall, neither preparation technique (direct or indirect) preferentially generates more precise and unbiased data for airborne Libby-type amphibole concentration estimates. The indirect preparation method is reasonable for estimating Libby-type amphibole exposure and may be necessary given the challenges of sampling in environmental settings. Relative to the larger context of uncertainties inherent in the risk assessment process, uncertainties associated with the use of airborne Libby-type amphibole exposure measurements derived from indirect preparation analysis are low. Use of exposure measurements generated by either direct or indirect preparation analyses is reasonable to estimate Libby-type Amphibole exposures in a risk assessment.

Chemical fingerprinting of Arabidopsis using Fourier transform infrared (FT-IR) spectroscopic approaches.

PubMed

Gorzsás, András; Sundberg, Björn

2014-01-01

Fourier transform infrared (FT-IR) spectroscopy is a fast, sensitive, inexpensive, and nondestructive technique for chemical profiling of plant materials. In this chapter we discuss the instrumental setup, the basic principles of analysis, and the possibilities for and limitations of obtaining qualitative and semiquantitative information by FT-IR spectroscopy. We provide detailed protocols for four fully customizable techniques: (1) Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS): a sensitive and high-throughput technique for powders; (2) attenuated total reflectance (ATR) spectroscopy: a technique that requires no sample preparation and can be used for solid samples as well as for cell cultures; (3) microspectroscopy using a single element (SE) detector: a technique used for analyzing sections at low spatial resolution; and (4) microspectroscopy using a focal plane array (FPA) detector: a technique for rapid chemical profiling of plant sections at cellular resolution. Sample preparation, measurement, and data analysis steps are listed for each of the techniques to help the user collect the best quality spectra and prepare them for subsequent multivariate analysis.

Nuclear radiation cleanup and uranium prospecting

DOEpatents

Mariella, Jr., Raymond P.; Dardenne, Yves M.

2016-02-02

Apparatus, systems, and methods for nuclear radiation cleanup and uranium prospecting include the steps of identifying an area; collecting samples; sample preparation; identification, assay, and analysis; and relating the samples to the area.

Nuclear radiation cleanup and uranium prospecting

DOEpatents

Mariella, Jr., Raymond P.; Dardenne, Yves M.

2017-01-03

Apparatus, systems, and methods for nuclear radiation cleanup and uranium prospecting include the steps of identifying an area; collecting samples; sample preparation; identification, assay, and analysis; and relating the samples to the area.

Laboratory Spectrometer for Wear Metal Analysis of Engine Lubricants.

DTIC Science & Technology

1986-04-01

analysis, the acid digestion technique for sample pretreatment is the best approach available to date because of its relatively large sample size (1000...microliters or more). However, this technique has two major shortcomings limiting its application: (1) it requires the use of hydrofluoric acid (a...accuracy. Sample preparation including filtration or acid digestion may increase analysis times by 20 minutes or more. b. Repeatability In the analysis

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, C.A.; Johnson, W.F.; Walker, W.A.

1985-08-05

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises: (1) a whole blood sample disc; (2) a serum sample disc; (3) a sample preparation rotor; and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analyticaly rotor for conventional methods. 5 figs.

Cytological preparations for molecular analysis: A review of technical procedures, advantages and limitations for referring samples for testing.

PubMed

da Cunha Santos, G; Saieg, M A; Troncone, G; Zeppa, P

2018-04-01

Minimally invasive procedures such as endobronchial ultrasound-guided transbronchial needle aspiration (EBUS-TBNA) must yield not only good quality and quantity of material for morphological assessment, but also an adequate sample for analysis of molecular markers to guide patients to appropriate targeted therapies. In this context, cytopathologists worldwide should be familiar with minimum requirements for refereeing cytological samples for testing. The present manuscript is a review with comprehensive description of the content of the workshop entitled Cytological preparations for molecular analysis: pre-analytical issues for EBUS TBNA, presented at the 40th European Congress of Cytopathology in Liverpool, UK. The present review emphasises the advantages and limitations of different types of cytology substrates used for molecular analysis such as archival smears, liquid-based preparations, archival cytospin preparations and FTA (Flinders Technology Associates) cards, as well as their technical requirements/features. These various types of cytological specimens can be successfully used for an extensive array of molecular studies, but the quality and quantity of extracted nucleic acids rely directly on adequate pre-analytical assessment of those samples. In this setting, cytopathologists must not only be familiar with the different types of specimens and associated technical procedures, but also correctly handle the material provided by minimally invasive procedures, ensuring that there is sufficient amount of material for a precise diagnosis and correct management of the patient through personalised care. © 2018 John Wiley & Sons Ltd.

Comprehensive analysis of structure and temperature, frequency and concentration-dependent dielectric properties of lithium-substituted cobalt ferrites (Li x Co1- x Fe2O4)

NASA Astrophysics Data System (ADS)

Anjum, Safia; Nisa, Mehru; Sabah, Aneeqa; Rafique, M. S.; Zia, Rehana

2017-08-01

This paper has been dedicated to the synthesis and characterization of a series of lithium-substituted cobalt ferrites Li x Co1- x Fe2O4 ( x = 0, 0.2, 0.4, 0.6, 0.8, 1). These samples have been prepared using simple ball milling machine through powder metallurgy route. The structural analysis is carried out using X-ray diffractometer and their 3D vitalization is simulated using diamond software. The frequency and temperature-dependent dielectric properties of prepared samples have been measured using inductor capacitor resistor (LCR) meter. The structural analysis confirms that all the prepared samples have inverse cubic spinel structure. It is also revealed that the crystallite size and lattice parameter decrease with the increasing concentration of lithium (Li+1) ions, it is due to the smaller ionic radii of lithium ions. The comprehensive analysis of frequency, concentration and temperature-dependent dielectric properties of prepared samples is described in this paper. It is observed that the dielectric constant and tangent loss have decreased and conductivity increased as the frequency increases. It is also revealed that the dielectric constant, tangent loss and AC conductivity increase as the concentration of lithium increases due to its lower electronegativity value. Temperature plays a vital role in enhancing the dielectric constant, tangent loss and AC conductivity because the mobility of ions increases as the temperature increases.

System Would Acquire Core and Powder Samples of Rocks

NASA Technical Reports Server (NTRS)

Bar-Cohen, Yoseph; Randolph, James; Bao, Xiaoqi; Sherrit, Stewart; Ritz, Chuck; Cook, Greg

2006-01-01

A system for automated sampling of rocks, ice, and similar hard materials at and immediately below the surface of the ground is undergoing development. The system, denoted a sample preparation, acquisition, handling, and delivery (SPAHD) device, would be mounted on a robotic exploratory vehicle that would traverse the terrain of interest on the Earth or on a remote planet. The SPAHD device would probe the ground to obtain data for optimization of sampling, prepare the surface, acquire samples in the form(s) of cores and/or powdered cuttings, and deliver the samples to a selected location for analysis and/or storage.

A new graphite preparation line for AMS 14C dating in the Zagreb Radiocarbon Laboratory

NASA Astrophysics Data System (ADS)

Krajcar Bronić, I.; Horvatinčić, N.; Sironić, A.; Obelić, B.; Barešić, J.; Felja, I.

2010-04-01

The new line for preparation of graphite samples for 14C dating by AMS has been constructed in the Zagreb Radiocarbon Laboratory. The performance of the rig and sample preparation procedure has been validated by preparing graphites from various reference materials of known 14C activity. The yield of the graphitization was good and the measured fraction of modern carbon ( Fm) values have not significantly deviated from the expected ones. Detailed analysis of measured Fm values indicates a slight bias to more positive values and should be carefully investigated.

Optimization of Sample Preparation processes of Bone Material for Raman Spectroscopy.

PubMed

Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

2018-03-30

Raman spectroscopy has recently been investigated for use in the calculation of postmortem interval from skeletal material. The fluorescence generated by samples, which affects the interpretation of Raman data, is a major limitation. This study compares the effectiveness of two sample preparation techniques, chemical bleaching and scraping, in the reduction of fluorescence from bone samples during testing with Raman spectroscopy. Visual assessment of Raman spectra obtained at 1064 nm excitation following the preparation protocols indicates an overall reduction in fluorescence. Results demonstrate that scraping is more effective at resolving fluorescence than chemical bleaching. The scraping of skeletonized remains prior to Raman analysis is a less destructive method and allows for the preservation of a bone sample in a state closest to its original form, which is beneficial in forensic investigations. It is recommended that bone scraping supersedes chemical bleaching as the preferred method for sample preparation prior to Raman spectroscopy. © 2018 American Academy of Forensic Sciences.

Nucleotide composition analysis of tRNA from leukemia patient cell samples and human cell lines.

PubMed Central

Agris, P F

1975-01-01

A technique developed for analysis of less than microgram quantities of tRNA has been applied to the study of human leukemia. Leucocytes from peripheal blood and bone marrow samples of six, untreated leukemia patients and cells of five different established human cell lines were maintained for 18 hours in media containing (32P)-phosphate. Incorporation of radioactive phosphate into the cells from the patient samples was slightly less than that of the cell lines. Likewise, incorporation of (32P)-phosphate into the tRNA of the patient samples (approximately 5 x 106 DPM/mug tRNA) was also less then that incorporated into the tRNA of the cell lines. The major and minor nucleotide compositions of the unfractionated tRNA preparations from each patient sample and each cell line were determined and compared. Similarities and differences in the major and minor nucleotide compositions of the tRNA preparations are discussed with reference to types of leukemia and the importance of patient sample analysis versus analysis of cultured human cells. PMID:1057159

Purification of pharmaceutical preparations using thin-layer chromatography to obtain mass spectra with Direct Analysis in Real Time and accurate mass spectrometry.

PubMed

Wood, Jessica L; Steiner, Robert R

2011-06-01

Forensic analysis of pharmaceutical preparations requires a comparative analysis with a standard of the suspected drug in order to identify the active ingredient. Purchasing analytical standards can be expensive or unattainable from the drug manufacturers. Direct Analysis in Real Time (DART™) is a novel, ambient ionization technique, typically coupled with a JEOL AccuTOF™ (accurate mass) mass spectrometer. While a fast and easy technique to perform, a drawback of using DART™ is the lack of component separation of mixtures prior to ionization. Various in-house pharmaceutical preparations were purified using thin-layer chromatography (TLC) and mass spectra were subsequently obtained using the AccuTOF™- DART™ technique. Utilizing TLC prior to sample introduction provides a simple, low-cost solution to acquiring mass spectra of the purified preparation. Each spectrum was compared against an in-house molecular formula list to confirm the accurate mass elemental compositions. Spectra of purified ingredients of known pharmaceuticals were added to an in-house library for use as comparators for casework samples. Resolving isomers from one another can be accomplished using collision-induced dissociation after ionization. Challenges arose when the pharmaceutical preparation required an optimized TLC solvent to achieve proper separation and purity of the standard. Purified spectra were obtained for 91 preparations and included in an in-house drug standard library. Primary standards would only need to be purchased when pharmaceutical preparations not previously encountered are submitted for comparative analysis. TLC prior to DART™ analysis demonstrates a time efficient and cost saving technique for the forensic drug analysis community. Copyright © 2011 John Wiley & Sons, Ltd. Copyright © 2011 John Wiley & Sons, Ltd.

Caffeine content of beverages as consumed.

PubMed Central

Gilbert, R. M.; Marshman, J. A.; Schwieder, M.; Berg, R.

1976-01-01

Quantitative analysis of beverages prepared at home by staff of the Addiction Research Foundation revealed a lower and much more variable caffeine content of both tea and coffee than had been reported in earlier studies, most of which were based on analysis of laboratory-prepared beverages. Median caffeine concentration of 37 home-prepared samples of tea was 27 mg per cup (range, 8 to 91 mg); for 46 coffee samples the median concentration was 74 mg per cup (range, 29 to 176 mg). If tea and coffee as drunk contain less caffeine than generally supposed, the potency of caffeine may be greater than commonly realized, as may the relative caffeine content of certain commercial preparations, including chocolate and colas. The substantial variation in caffeine content emphasizes the need to establish actual caffeine intake in clinical, epidemiologic and experimental investigations of caffeine effects. PMID:1032351

Results and analysis of saltstone cores taken from saltstone disposal unit cell 2A

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reigel, M. M.; Hill, K. A.

2016-03-01

As part of an ongoing Performance Assessment (PA) Maintenance Plan, Savannah River Remediation (SRR) has developed a sampling and analyses strategy to facilitate the comparison of field-emplaced samples (i.e., saltstone placed and cured in a Saltstone Disposal Unit (SDU)) with samples prepared and cured in the laboratory. The primary objectives of the Sampling and Analyses Plan (SAP) are; (1) to demonstrate a correlation between the measured properties of laboratory-prepared, simulant samples (termed Sample Set 3), and the field-emplaced saltstone samples (termed Sample Set 9), and (2) to validate property values assumed for the Saltstone Disposal Facility (SDF) PA modeling. Themore » analysis and property data for Sample Set 9 (i.e. six core samples extracted from SDU Cell 2A (SDU2A)) are documented in this report, and where applicable, the results are compared to the results for Sample Set 3. Relevant properties to demonstrate the aforementioned objectives include bulk density, porosity, saturated hydraulic conductivity (SHC), and radionuclide leaching behavior.« less

Improved analysis of Monascus pigments based on their pH-sensitive UV-Vis absorption and reactivity properties.

PubMed

Shi, Kan; Chen, Gong; Pistolozzi, Marco; Xia, Fenggeng; Wu, Zhenqiang

2016-09-01

Monascus pigments, a mixture of azaphilones mainly composed of red, orange and yellow pigments, are usually prepared in aqueous ethanol and analysed by ultraviolet-visible (UV-Vis) spectroscopy. The pH of aqueous ethanol used during sample preparation and analysis has never been considered a key parameter to control; however, this study shows that the UV-Vis spectra and colour characteristics of the six major pigments are strongly influenced by the pH of the solvent employed. In addition, the increase of solvent pH results in a remarkable increase of the amination reaction of orange pigments with amino compounds, and at higher pH (≥ 6.0) a significant amount of orange pigment derivatives rapidly form. The consequent impact of these pH-sensitive properties on pigment analysis is further discussed. Based on the presented results, we propose that the sample preparation and analysis of Monascus pigments should be uniformly performed at low pH (≤ 2.5) to avoid variations of UV-Vis spectra and the creation of artefacts due to the occurrence of amination reactions, and ensure an accurate analysis that truly reflects pigment characteristics in the samples.

EPA Air Method, Toxic Organics - 15 (TO-15): Determination of Volatile Organic Compounds (VOCs) in Air Collected in Specially-Prepared Canisters and Analyzed by Gas Chromatography/Mass Spectrometry (GC/MS)

EPA Pesticide Factsheets

Method T)-15 describes procedures for for preparation and analysis of air samples containing volatile organic compounds collected in specially-prepared canisters, using gas chromatography-mass spectrometry.

Structural and optical properties of Cu2ZnSnS4 synthesized by ultrasonic assisted sol-gel method

NASA Astrophysics Data System (ADS)

Rajwar, Birendra Kumar; Sharma, Shailendra Kumar

2018-05-01

Cu2ZnSnS4 (CZTS) nanocrystals were synthesized by a simple ultrasonic assisted sol-gel method using two different solvents. Structure and purity of the phase formed were investigated using X-ray diffraction (XRD) and Raman measurements. The average crystallite size were estimated by using Scherrer's formula and found to be 2.09 and 7.15 nm. Raman study reveals the kesterite-phase of prepared samples. The influence of solvent in the morphologies of prepared samples was investigated by field emission scanning electron microscopy (FESEM). Ultraviolet-visible-near-infrared absorption measurement was carried out to calculate the optical band gap of samples. Oxidation state of the constitute elements of as-prepared samples were investigated by X-ray photoelectron spectroscopy (XPS) analysis and the results are in good agreement with the literature. The surface area and pore volume were estimated after analysis of nitrogen adsorption-desorption isotherm curves and found to be 16.5 m2/gm and 0.01 cm3/gm respectively.

An overview of the main foodstuff sample preparation technologies for tetracycline residue determination.

PubMed

Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo

2018-05-15

Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

DOE PAGES

Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund; ...

2018-03-28

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Polished sample preparing and backscattered electron imaging and of fly ash-cement paste

NASA Astrophysics Data System (ADS)

Feng, Shuxia; Li, Yanqi

2018-03-01

In recent decades, the technology of backscattered electron imaging and image analysis was applied in more and more study of mixed cement paste because of its special advantages. Test accuracy of this technology is affected by polished sample preparation and image acquisition. In our work, effects of two factors in polished sample preparing and backscattered electron imaging were investigated. The results showed that increasing smoothing pressure could improve the flatness of polished surface and then help to eliminate interference of morphology on grey level distribution of backscattered electron images; increasing accelerating voltage was beneficial to increase gray difference among different phases in backscattered electron images.

Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry.

PubMed

Kruve, Anneli; Künnapas, Allan; Herodes, Koit; Leito, Ivo

2008-04-11

Three sample preparation methods: Luke method (AOAC 985.22), QuEChERS (quick, easy, cheap, effective, rugged and safe) and matrix solid-phase dispersion (MSPD) were applied to different fruits and vegetables for analysis of 14 pesticide residues by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC/ESI/MS). Matrix effect, recovery and process efficiency of the sample preparation methods applied to different fruits and vegetables were compared. The Luke method was found to produce least matrix effect. On an average the best recoveries were obtained with the QuEChERS method. MSPD gave unsatisfactory recoveries for some basic pesticide residues. Comparison of matrix effects for different apple varieties showed high variability for some residues. It was demonstrated that the amount of co-extracting compounds that cause ionization suppression of aldicarb depends on the apple variety as well as on the sample preparation method employed.

Improvements in soft gelatin capsule sample preparation for USP-based simethicone FTIR analysis.

PubMed

Hargis, Amy D; Whittall, Linda B

2013-02-23

Due to the absence of a significant chromophore, Simethicone raw material and finished product analysis is achieved using a FTIR-based method that quantifies the polydimethylsiloxane (PDMS) component of the active ingredient. The method can be found in the USP monographs for several dosage forms of Simethicone-containing pharmaceutical products. For soft gelatin capsules, the PDMS assay values determined using the procedure described in the USP method were variable (%RSDs from 2 to 9%) and often lower than expected based on raw material values. After investigation, it was determined that the extraction procedure used for sample preparation was causing loss of material to the container walls due to the hydrophobic nature of PDMS. Evaluation revealed that a simple dissolution of the gelatin capsule fill in toluene provided improved assay results (%RSDs≤0.5%) as well as a simplified and rapid sample preparation. Copyright © 2012 Elsevier B.V. All rights reserved.

Importance of tissue preparation methods in FTIR micro-spectroscopical analysis of biological tissues: 'traps for new users'.

PubMed

Zohdi, Vladislava; Whelan, Donna R; Wood, Bayden R; Pearson, James T; Bambery, Keith R; Black, M Jane

2015-01-01

Fourier Transform Infrared (FTIR) micro-spectroscopy is an emerging technique for the biochemical analysis of tissues and cellular materials. It provides objective information on the holistic biochemistry of a cell or tissue sample and has been applied in many areas of medical research. However, it has become apparent that how the tissue is handled prior to FTIR micro-spectroscopic imaging requires special consideration, particularly with regards to methods for preservation of the samples. We have performed FTIR micro-spectroscopy on rodent heart and liver tissue sections (two spectroscopically very different biological tissues) that were prepared by desiccation drying, ethanol substitution and formalin fixation and have compared the resulting spectra with that of fully hydrated freshly excised tissues. We have systematically examined the spectra for any biochemical changes to the native state of the tissue caused by the three methods of preparation and have detected changes in infrared (IR) absorption band intensities and peak positions. In particular, the position and profile of the amide I, key in assigning protein secondary structure, changes depending on preparation method and the lipid absorptions lose intensity drastically when these tissues are hydrated with ethanol. Indeed, we demonstrate that preserving samples through desiccation drying, ethanol substitution or formalin fixation significantly alters the biochemical information detected using spectroscopic methods when compared to spectra of fresh hydrated tissue. It is therefore imperative to consider tissue preparative effects when preparing, measuring, and analyzing samples using FTIR spectroscopy.

Non-Contact Conductivity Measurement for Automated Sample Processing Systems

NASA Technical Reports Server (NTRS)

Beegle, Luther W.; Kirby, James P.

2012-01-01

A new method has been developed for monitoring and control of automated sample processing and preparation especially focusing on desalting of samples before analytical analysis (described in more detail in Automated Desalting Apparatus, (NPO-45428), NASA Tech Briefs, Vol. 34, No. 8 (August 2010), page 44). The use of non-contact conductivity probes, one at the inlet and one at the outlet of the solid phase sample preparation media, allows monitoring of the process, and acts as a trigger for the start of the next step in the sequence (see figure). At each step of the muti-step process, the system is flushed with low-conductivity water, which sets the system back to an overall low-conductivity state. This measurement then triggers the next stage of sample processing protocols, and greatly minimizes use of consumables. In the case of amino acid sample preparation for desalting, the conductivity measurement will define three key conditions for the sample preparation process. First, when the system is neutralized (low conductivity, by washing with excess de-ionized water); second, when the system is acidified, by washing with a strong acid (high conductivity); and third, when the system is at a basic condition of high pH (high conductivity). Taken together, this non-contact conductivity measurement for monitoring sample preparation will not only facilitate automation of the sample preparation and processing, but will also act as a way to optimize the operational time and use of consumables

Results of the first provisional technical secretariat interlaboratory comparison test

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stuff, J.R.; Hoffland, L.

1995-06-01

The principal task of this laboratory in the first Provisional Technical Secretariat (PTS) Interlaboratory Comparison Test was to verify and test the extraction and preparation procedures outlined in the Recommended Operating Procedures for Sampling and Analysis in the Verification of Chemical Disarmament in addition to our laboratory extraction methods and our laboratory analysis methods. Sample preparation began on 16 May 1994 and analysis was completed on 12 June 1994. The analytical methods used included NMR ({sup 1}H and {sup 31}P) GC/AED, GC/MS (EI and methane CI), GC/IRD, HPLC/IC, HPLC/TSP/MS, MS/MS(Electrospray), and CZE.

The Successful Diagnosis and Typing of Systemic Amyloidosis Using A Microwave-Assisted Filter-Aided Fast Sample Preparation Method and LC/MS/MS Analysis

PubMed Central

Zou, Lili; Shen, Kaini; Zhong, Dingrong; Zhou, Daobin; Sun, Wei; Li, Jian

2015-01-01

Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove contaminants with a 10-kDa cutoff ultrafiltration unit and can accelerate the digestion process with the assistance of a microwave. Additionally, two parameters (P- and D-scores) based on the exponentially modified protein abundance index were developed to define the existence of amyloid deposits and those causative proteins with the greatest abundance. Using our protocol, twenty cases of systemic amyloidosis that were well-typed according to clinical diagnostic standards (training group) and another twenty-four cases without subtype diagnoses (validation group) were analyzed. Using this approach, sample preparation could be completed within four hours. We successfully subtyped 100% of the cases in the training group, and the diagnostic success rate in the validation group was 91.7%. This maFASP-aided proteomic protocol represents an efficient approach for amyloid diagnosis and subtyping, particularly for serum-contaminated samples. PMID:25984759

Assessment of Sample Preparation Bias in Mass Spectrometry-Based Proteomics.

PubMed

Klont, Frank; Bras, Linda; Wolters, Justina C; Ongay, Sara; Bischoff, Rainer; Halmos, Gyorgy B; Horvatovich, Péter

2018-04-17

For mass spectrometry-based proteomics, the selected sample preparation strategy is a key determinant for information that will be obtained. However, the corresponding selection is often not based on a fit-for-purpose evaluation. Here we report a comparison of in-gel (IGD), in-solution (ISD), on-filter (OFD), and on-pellet digestion (OPD) workflows on the basis of targeted (QconCAT-multiple reaction monitoring (MRM) method for mitochondrial proteins) and discovery proteomics (data-dependent acquisition, DDA) analyses using three different human head and neck tissues (i.e., nasal polyps, parotid gland, and palatine tonsils). Our study reveals differences between the sample preparation methods, for example, with respect to protein and peptide losses, quantification variability, protocol-induced methionine oxidation, and asparagine/glutamine deamidation as well as identification of cysteine-containing peptides. However, none of the methods performed best for all types of tissues, which argues against the existence of a universal sample preparation method for proteome analysis.

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.12)

EPA Science Inventory

The method is for extracting an indoor and outdoor air sample consisting of a quartz fiber filter and an XAD-2 cartridge for analysis of neutral persistent organic pollutants. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF PESTICIDES FROM SURFACE WIPE SAMPLES (BCO-L-13.0)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for extracting and preparing a sill surface wipe sample for gas chromatography/mass spectrometry (GC/MS) analysis of pesticides. This procedure is also used for the pre-shipment analysis of sill wipe samples for materials sui...

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS

PubMed Central

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-01-01

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed—aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended. PMID:25791294

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS.

PubMed

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-03-19

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed-aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended.

Automation of dimethylation after guanidination labeling chemistry and its compatibility with common buffers and surfactants for mass spectrometry-based shotgun quantitative proteome analysis.

PubMed

Lo, Andy; Tang, Yanan; Chen, Lu; Li, Liang

2013-07-25

Isotope labeling liquid chromatography-mass spectrometry (LC-MS) is a major analytical platform for quantitative proteome analysis. Incorporation of isotopes used to distinguish samples plays a critical role in the success of this strategy. In this work, we optimized and automated a chemical derivatization protocol (dimethylation after guanidination, 2MEGA) to increase the labeling reproducibility and reduce human intervention. We also evaluated the reagent compatibility of this protocol to handle biological samples in different types of buffers and surfactants. A commercially available liquid handler was used for reagent dispensation to minimize analyst intervention and at least twenty protein digest samples could be prepared in a single run. Different front-end sample preparation methods for protein solubilization (SDS, urea, Rapigest™, and ProteaseMAX™) and two commercially available cell lysis buffers were evaluated for compatibility with the automated protocol. It was found that better than 94% desired labeling could be obtained in all conditions studied except urea, where the rate was reduced to about 92% due to carbamylation on the peptide amines. This work illustrates the automated 2MEGA labeling process can be used to handle a wide range of protein samples containing various reagents that are often encountered in protein sample preparation for quantitative proteome analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

A High-Performance Liquid Chromatography-Based Screening Method for the Analysis of Atrazine, Alachlor, and Ten of Their Transformation Products

USGS Publications Warehouse

Schroyer, B.R.; Capel, P.D.

1996-01-01

A high-performance liquid Chromatography (HPLC) method is presented for the for the fast, quantitative analysis of the target analytes in water and in low organic-carbon, sandy soils that are known to be contaminated with the parent herbicides. Speed and ease of sample preparation was prioritized above minimizing detection limits. Soil samples were extracted using 80:20 methanol:water (volume:volume). Water samples (50 ??L) were injected directly into the HPLC without prior preparation. Method quantification limits for soil samples (10 g dry weight) and water samples ranged from 20 to 110 ng/g and from 20 to 110 ??g/L for atrazine and its transformation products and from 80 to 320 ng/g and from 80 to 320 ??g/L for alachlor and its transformation products, respectively.

Photo-, sono- and sonophotocatalytic degradation of methylene blue using Fe3O4/ZrO2 composites catalysts

NASA Astrophysics Data System (ADS)

Kristianto, Y.; Taufik, A.; Saleh, R.

2017-07-01

In the present work, magnetite material Fe3O4/ZrO2 with various molar ratios was prepared by the two-step method (sol-gel followed by the ultrasonic-assisted method). The as-prepared samples were fairly characterized by various characterization methods, such as X-ray Diffraction (XRD), Vibrating Sample Magnetometer (VSM), Fourier Transform Infrared (FT-IR) and Thermal Gravimetric Analysis (TGA). The catalytic performance of the as-prepared samples was evaluated based on the degradation of methylene blue under UV light, ultrasound and combination of UV and ultrasound irradiation. The results revealed that the sample with Fe3O4:ZrO2 molar ratio of 0.5:1 showed the best catalytic performance under UV, ultrasound and UV + ultrasound irradiation. The degradation of methylene blue follows the order: sonophotocatalytic > sonocatalytic > photocatalytic. In addition, the effect of various scavengers has also been studied. Furthermore, all prepared samples could be used as a convenient recyclable catalyst.

Infrared spectroscopy and upconversion luminescence behaviour of erbium doped yttrium (III) oxide phosphor

NASA Astrophysics Data System (ADS)

Dubey, Vikas; Tiwari, Ratnesh; Tamrakar, Raunak Kumar; Rathore, Gajendra Singh; Sharma, Chitrakant; Tiwari, Neha

2014-11-01

The paper reports upconversion luminescence behaviour and infra-red spectroscopic pattern of erbium doped yttrium (III) oxide phosphor. Sample was synthesized by solid state reaction method with variable concentration or erbium (0.5-2.5 mol%). The conventional solid state method is suitable for large scale production and eco-friendly method. The prepared sample was characterized by X-ray diffraction (XRD) technique. From structural analysis by XRD technique shows cubic structure of prepared sample with variable concentration of erbium and no impurity phase were found when increase the concentration of Er3+. Particle size was calculated by Scherer's formula and it varies from 67 nm to 120 nm. The surface morphology of prepared phosphor was determined by field emission gun scanning electron microscopy (FEGSEM) technique. The surface morphology of the sample shows good connectivity with grains as well as some agglomerates formation occurs in sample. The functional group analysis was done by Fourier transform infra-red technique (FTIR) analysis which confirm the formation of Y2O3:Er3+ phosphor was prepared. The results indicated that the Y2O3:Er3+ phosphors might have high upconversion efficiency because of their low vibrational energy. Under 980 nm laser excitation sample shows intense green emission at 555 nm and orange emission at 590 nm wavelength. For green emission transition occurs 2H11/2 → 4I15/2, 4S3/2 → 4I15/2 for upconversion emissions. Excited state absorption and energy transfer process were discussed as possible upconversion mechanisms. The near infrared luminescence spectra was recorded. The upconversion luminescence intensity increase with increasing the concentration or erbium up to 2 mol% after that luminescence intensity decreases due to concentration quenching occurs. Spectrophotometric determinations of peaks are evaluated by Commission Internationale de I'Eclairage (CIE) technique. From CIE technique the dominant peak of from PL spectra shows intense green emission so the prepared phosphor is may be useful for green light emitting diode (GLED) application.

Hydrogen concentration analysis in clinopyroxene using proton-proton scattering analysis

NASA Astrophysics Data System (ADS)

Weis, Franz A.; Ros, Linus; Reichart, Patrick; Skogby, Henrik; Kristiansson, Per; Dollinger, Günther

2018-02-01

Traditional methods to measure water in nominally anhydrous minerals (NAMs) are, for example, Fourier transformed infrared (FTIR) spectroscopy or secondary ion mass spectrometry (SIMS). Both well-established methods provide a low detection limit as well as high spatial resolution yet may require elaborate sample orientation or destructive sample preparation. Here we analyze the water content in erupted volcanic clinopyroxene phenocrysts by proton-proton scattering and reproduce water contents measured by FTIR spectroscopy. We show that this technique provides significant advantages over other methods as it can provide a three-dimensional distribution of hydrogen within a crystal, making the identification of potential inclusions possible as well as elimination of surface contamination. The sample analysis is also independent of crystal structure and orientation and independent of matrix effects other than sample density. The results are used to validate the accuracy of wavenumber-dependent vs. mineral-specific molar absorption coefficients in FTIR spectroscopy. In addition, we present a new method for the sample preparation of very thin crystals suitable for proton-proton scattering analysis using relatively low accelerator potentials.

NEW COLUMN SEPARATION METHOD FOR EMERGENCY URINE SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S; Brian Culligan, B

2007-08-28

The Savannah River Site Environmental Bioassay Lab participated in the 2007 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2007. A new rapid column separation method was applied directly to the NRIP 2007 emergency urine samples, with only minimal sample preparation to reduce preparation time. Calcium phosphate precipitation, previously used to pre-concentrate actinides and Sr-90 in NRIP 2006 urine and water samples, was not used for the NRIP 2007 urine samples. Instead, the raw urine was acidified and passed directly through the stacked resin columns (TEVA+TRU+SR Resins) to separate the actinides andmore » strontium from the NRIP urine samples more quickly. This improvement reduced sample preparation time for the NRIP 2007 emergency urine analyses significantly. This approach works well for small volume urine samples expected during an emergency response event. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and strontium-90 analyses for NRIP 2007 urine samples.« less

A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis.

PubMed

Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M

2006-01-01

A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

Using Microwave Sample Decomposition in Undergraduate Analytical Chemistry

NASA Astrophysics Data System (ADS)

Griff Freeman, R.; McCurdy, David L.

1998-08-01

A shortcoming of many undergraduate classes in analytical chemistry is that students receive little exposure to sample preparation in chemical analysis. This paper reports the progress made in introducing microwave sample decomposition into several quantitative analysis experiments at Truman State University. Two experiments being performed in our current laboratory rotation include closed vessel microwave decomposition applied to the classical gravimetric determination of nickel and the determination of sodium in snack foods by flame atomic emission spectrometry. A third lab, using open-vessel microwave decomposition for the Kjeldahl nitrogen determination is now ready for student trial. Microwave decomposition reduces the time needed to complete these experiments and significantly increases the student awareness of the importance of sample preparation in quantitative chemical analyses, providing greater breadth and realism in the experiments.

A comparison of freeze-drying and oven-drying preparation methods for bulk and compound-specific carbon stable isotope analyses: examples using the benthic macroinvertebrates Stenopsyche marmorata and Epeorus latifolium.

PubMed

Akamatsu, Fumikazu; Suzuki, Yaeko; Kato, Yoshikazu; Yoshimizu, Chikage; Tayasu, Ichiro

2016-01-15

Carbon stable isotope analysis of bulk samples and fatty acids is an established method for tracing carbon flow pathways and reconstructing trophic interactions, but there is no consensus on which sample drying method should be used for sample preparation. The aim of this study was to determine if freeze-drying and oven-drying treatments used to prepare samples of the benthic macroinvertebrates Stenopsyche marmorata and Epeorus latifolium for bulk and fatty-acid-specific carbon stable isotope analysis yield different isotopic ratio values. Five individuals each from two species were split in half; one half was freeze-dried and the other half was oven-dried. The samples were ground and the δ(13)C values of the bulk samples and eight fatty acids were measured following combustion using an isotope ratio mass spectrometer coupled to an elemental analyzer or gas chromatography system. The mean difference in the bulk and fatty acid δ(13)C values between freeze-dried and oven-dried samples was small (≤0.1‰ in both cases), although relatively large variations were observed in individual fatty-acid-specific δ(13)C values (maximum of ≤0.9 ‰). There were no significant differences in either bulk sample or fatty-acid-specific δ(13)C values between freeze-dried or oven-dried samples of the same species. Freeze-drying and oven-drying are equally acceptable methods for preparing freshly caught S. marmorata and E. latifolium samples for bulk and fatty-acid-specific carbon stable isotope analyses. Copyright © 2015 John Wiley & Sons, Ltd.

Associations among school characteristics and foodservice practices in a nationally representative sample of United States schools.

PubMed

Thomson, Jessica L; Tussing-Humphreys, Lisa M; Martin, Corby K; LeBlanc, Monique M; Onufrak, Stephen J

2012-01-01

Determine school characteristics associated with healthy/unhealthy food service offerings or healthy food preparation practices. Secondary analysis of cross-sectional data. Nationally representative sample of public and private elementary, middle, and high schools. Data from the 2006 School Health Policies and Practices Study Food Service School Questionnaire, n = 526 for Healthy and Unhealthy Offerings analysis; n = 520 for Healthy Preparation analysis. Scores for healthy/unhealthy foodservice offerings and healthy food preparation practices. Multivariable regression to determine significant associations among school characteristics and offerings/preparation practices. Public schools and schools participating in the United States Department of Agriculture (USDA) Team Nutrition reported more healthy offerings and preparation than private or nonparticipating schools, respectively. Elementary schools reported fewer unhealthy offerings than middle or high schools; middle schools reported fewer unhealthy offerings than high schools. Schools requiring foodservice managers to have a college education reported more healthy preparation, whereas those requiring completion of a foodservice training program reported fewer unhealthy offerings and more healthy preparation than schools without these requirements. Results suggest the school nutrition environment may be improved by requiring foodservice managers to hold a nutrition-related college degree and/or successfully pass a foodservice training program, and by participating in a school-based nutrition program, such as USDA Team Nutrition. Copyright © 2012 Society for Nutrition Education and Behavior. All rights reserved.

Methods of biological fluids sample preparation - biogenic amines, methylxanthines, water-soluble vitamins.

PubMed

Płonka, Joanna

2015-01-01

In recent years demands on the amount of information that can be obtained from the analysis of a single sample have increased. For time and economic reasons it is necessary to examine at the same time larger number of compounds, and compounds from different groups. This can best be seen in such areas as clinical analysis. In many diseases, the best results for patients are obtained when treatment fits the individual characteristics of the patient. Dosage monitoring is important at the beginning of therapy and in the full process of treatment. In the treatment of many diseases biogenic amines (dopamine, serotonin) and methylxanthines (theophylline, theobromine, caffeine) play an important role. They are used as drugs separately or in combination with others to support and strengthen the action of other drugs - for example, the combination of caffeine and paracetamol. Vitamin supplementation may be also an integral part of the treatment process. Specification of complete sample preparation parameters for extraction of the above compounds from biological matrices has been reviewed. Particular attention was given to the preparation stage and extraction methods. This review provides universal guidance on establishing a common procedures across laboratories to facilitate the preparation and analysis of all discussed compounds. Copyright © 2014 John Wiley & Sons, Ltd.

Green Aspects of Techniques for the Determination of Currently Used Pesticides in Environmental Samples

PubMed Central

Stocka, Jolanta; Tankiewicz, Maciej; Biziuk, Marek; Namieśnik, Jacek

2011-01-01

Pesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in the environment is a particular danger. It is therefore crucial to monitor pesticide residues using all available analytical methods. The analysis of environmental samples for the presence of pesticides is very difficult: the processes involved in sample preparation are labor-intensive and time-consuming. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solvent-less and solvent-minimized techniques are becoming popular. The application of Green Chemistry principles to sample preparation is primarily leading to the miniaturization of procedures and the use of solvent-less techniques, and these are discussed in the paper. PMID:22174632

Analysis of pure and malachite green doped polysulfone sample using FT-IR technique

NASA Astrophysics Data System (ADS)

Nayak, Rashmi J.; Khare, P. K.; Nayak, J. G.

2018-05-01

The sample of pure and malachite green doped Polysulfone in the form of foil was prepared by isothermal immersion technique. For the preparation of pure sample 4 gm of Polysulfone was dissolved in 50 ml of Dimethyl farmamide (DMF) solvent, while for the preparation of doped sample 10 mg, 50 mg and 100 mg Malachite Green was mixed with 4 gm of Polysulfone respectively. For the study of structural characterization of these pure and doped sample, Fourier Transform Infra-Red Spectroscopy (FT-IR) technique was used. This study shows that the intensity of transmittance decreases as the ratio of doping increases in pure polysulfone. The reduction in intensity of transmittance is clearly apparent in the present case more over the bands were broader which indicates towards charge transfer interaction between the donar and acceptor molecule.

Study of sample preparation for quantitative analysis of amino acids in human sweat by liquid chromatography-tandem mass spectrometry.

PubMed

Delgado-Povedano, M M; Calderón-Santiago, M; Priego-Capote, F; Luque de Castro, M D

2016-01-01

The determination of physiological levels of amino acids is important to aid in the diagnosis and treatment of several diseases and nutritional status of individuals. Amino acids are frequently determined in biofluids such as blood (serum or plasma) and urine; however, there are less common biofluids with different concentration profiles of amino acids that could be of interest. One of these biofluids is sweat that can be obtained in a non-invasive manner and is characterized by low complex composition. The analysis of amino acids in human sweat requires the development of sample preparation strategies according to the sample matrix and small collected volume. The influence of sample preparation on the quantitative analysis of amino acids in sweat by LC-MS/MS has been assessed through a comparison between two strategies: dilution of sweat and centrifugal microsolid-phase extraction (c-μSPE). In both cases, several dilution factors were assayed for in-depth knowledge of the matrix effects, and the use of c-μSPE provided the best results in terms of accuracy. The behavior of the target analytes was a function of the dilution factor, thus providing a pattern for sample preparation that depended on the amino acid to be determined. The concentration of amino acids in sweat ranges between 6.20 ng mL(-1) (for homocysteine) and 259.77 µg mL(-1) (for serine) with precision, expressed as relative standard deviation, within 1.1-21.4%. Copyright © 2015 Elsevier B.V. All rights reserved.

Analyzing Immunoglobulin Repertoires

PubMed Central

Chaudhary, Neha; Wesemann, Duane R.

2018-01-01

Somatic assembly of T cell receptor and B cell receptor (BCR) genes produces a vast diversity of lymphocyte antigen recognition capacity. The advent of efficient high-throughput sequencing of lymphocyte antigen receptor genes has recently generated unprecedented opportunities for exploration of adaptive immune responses. With these opportunities have come significant challenges in understanding the analysis techniques that most accurately reflect underlying biological phenomena. In this regard, sample preparation and sequence analysis techniques, which have largely been borrowed and adapted from other fields, continue to evolve. Here, we review current methods and challenges of library preparation, sequencing and statistical analysis of lymphocyte receptor repertoire studies. We discuss the general steps in the process of immune repertoire generation including sample preparation, platforms available for sequencing, processing of sequencing data, measurable features of the immune repertoire, and the statistical tools that can be used for analysis and interpretation of the data. Because BCR analysis harbors additional complexities, such as immunoglobulin (Ig) (i.e., antibody) gene somatic hypermutation and class switch recombination, the emphasis of this review is on Ig/BCR sequence analysis. PMID:29593723

Sampling of Atmospheric Precipitation and Deposits for Analysis of Atmospheric Pollution

PubMed Central

Skarżyńska, K.; Polkowska, Ż; Namieśnik, J.

2006-01-01

This paper reviews techniques and equipment for collecting precipitation samples from the atmosphere (fog and cloud water) and from atmospheric deposits (dew, hoarfrost, and rime) that are suitable for the evaluation of atmospheric pollution. It discusses the storage and preparation of samples for analysis and also presents bibliographic information on the concentration ranges of inorganic and organic compounds in the precipitation and atmospheric deposit samples. PMID:17671615

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

NASA Astrophysics Data System (ADS)

Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; von Reden, Karl; Nosams

2000-10-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 μg) of carbon. The capability to mass-produce small samples for 14C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC).

Preparation and validation of gross alpha/beta samples used in EML`s quality assessment program

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scarpitta, S.C.

1997-10-01

A set of water and filter samples have been incorporated into the existing Environmental Measurements Laboratory`s (EML) Quality Assessment Program (QAP) for gross alpha/beta determinations by participating DOE laboratories. The participating laboratories are evaluated by comparing their results with the EML value. The preferred EML method for measuring water and filter samples, described in this report, uses gas flow proportional counters with 2 in. detectors. Procedures for sample preparation, quality control and instrument calibration are presented. Liquid scintillation (LS) counting is an alternative technique that is suitable for quantifying both the alpha ({sup 241}Am, {sup 230}Th and {sup 238}Pu) andmore » beta ({sup 90}Sr/{sup 90}Y) activity concentrations in the solutions used to prepare the QAP water and air filter samples. Three LS counting techniques (Cerenkov, dual dpm and full spectrum analysis) are compared. These techniques may be used to validate the activity concentrations of each component in the alpha/beta solution before the QAP samples are actually prepared.« less

Novel sample preparation technique with needle-type micro-extraction device for volatile organic compounds in indoor air samples.

PubMed

Ueta, Ikuo; Mizuguchi, Ayako; Fujimura, Koji; Kawakubo, Susumu; Saito, Yoshihiro

2012-10-09

A novel needle-type sample preparation device was developed for the effective preconcentration of volatile organic compounds (VOCs) in indoor air before gas chromatography-mass spectrometry (GC-MS) analysis. To develop a device for extracting a wide range of VOCs typically found in indoor air, several types of particulate sorbents were tested as the extraction medium in the needle-type extraction device. To determine the content of these VOCs, air samples were collected for 30min with the packed sorbent(s) in the extraction needle, and the extracted VOCs were thermally desorbed in a GC injection port by the direct insertion of the needle. A double-bed sorbent consisting of a needle packed with divinylbenzene and activated carbon particles exhibited excellent extraction and desorption performance and adequate extraction capacity for all the investigated VOCs. The results also clearly demonstrated that the proposed sample preparation method is a more rapid, simpler extraction/desorption technique than traditional sample preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation of hair for measurement of elements by inductively coupled plasma-mass spectrometry (ICP-MS).

PubMed

Puchyr, R F; Bass, D A; Gajewski, R; Calvin, M; Marquardt, W; Urek, K; Druyan, M E; Quig, D

1998-06-01

The preparation of hair for the determination of elements is a critical component of the analysis procedure. Open-beaker, closed-vessel microwave, and flowthrough microwave digestion are methods that have been used for sample preparation and are discussed. A new digestion method for use with inductively coupled plasma-mass spectrometry (ICP-MS) has been developed. The method uses 0.2 g of hair and 3 mL of concentrated nitric acid in an atmospheric pressure-low-temperature microwave digestion (APLTMD) system. This preparation method is useful in handling a large numbers of samples per day and may be adapted to hair sample weights ranging from 0.08 to 0.3 g. After digestion, samples are analyzed by ICP-MS to determine the concentration of Li, Be, B, Na, Mg, Al, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Se, Rb, Sr, Zr, Mo, Pd, Ag, Cd, Sn, Sb, I, Cs, Ba, Pt, Au, Hg, Tl, Pb, Bi, Th, and U. Benefits of the APLTMD include reduced contamination and sample handling, and increased precision, reliability, and sample throughput.

Characterization Data Package for Containerized Sludge Samples Collected from Engineered Container SCS-CON-210

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fountain, Matthew S.; Fiskum, Sandra K.; Baldwin, David L.

This data package contains the K Basin sludge characterization results obtained by Pacific Northwest National Laboratory during processing and analysis of four sludge core samples collected from Engineered Container SCS-CON-210 in 2010 as requested by CH2M Hill Plateau Remediation Company. Sample processing requirements, analytes of interest, detection limits, and quality control sample requirements are defined in the KBC-33786, Rev. 2. The core processing scope included reconstitution of a sludge core sample distributed among four to six 4-L polypropylene bottles into a single container. The reconstituted core sample was then mixed and subsampled to support a variety of characterization activities. Additionalmore » core sludge subsamples were combined to prepare a container composite. The container composite was fractionated by wet sieving through a 2,000 micron mesh and a 500-micron mesh sieve. Each sieve fraction was sampled to support a suite of analyses. The core composite analysis scope included density determination, radioisotope analysis, and metals analysis, including the Waste Isolation Pilot Plant Hazardous Waste Facility Permit metals (with the exception of mercury). The container composite analysis included most of the core composite analysis scope plus particle size distribution, particle density, rheology, and crystalline phase identification. A summary of the received samples, core sample reconstitution and subsampling activities, container composite preparation and subsampling activities, physical properties, and analytical results are presented. Supporting data and documentation are provided in the appendices. There were no cases of sample or data loss and all of the available samples and data are reported as required by the Quality Assurance Project Plan/Sampling and Analysis Plan.« less

Determination of Cu Environments in the Cyanobacterium Anabaena flos-aquae by X-Ray Absorption Spectroscopy

PubMed Central

Kretschmer, X. C.; Meitzner, G.; Gardea-Torresdey, J. L.; Webb, R.

2004-01-01

Whole cells and peptidoglycan isolated from cell walls of the cyanobacterium Anabaena flos-aquae were lyophilized and used at pH 2 and pH 5 in Cu(II) binding studies. X-ray absorption spectra measured at the Cu K-edge were used to determine the oxidation states and chemical environments of Cu species in the whole-cell and peptidoglycan samples. In the whole-cell samples, most of the Cu retained at both pH values was coordinated by phosphate ligands. The whole-cell fractions contained significant concentrations of Cu(I) as well as Cu(II). An X-ray absorption near-edge spectrum analysis suggested that Cu(I) was coordinated by amine and thiol ligands. An analysis of the peptidoglycan fractions found that more Cu was adsorbed by the peptidoglycan fraction prepared at pH 5, due to increased chelation by amine and carboxyl ligands. The peptidoglycan fractions, also referred to as the cell wall fractions, contained little or no Cu(I). The Cu loading level was 30 times higher in the cell wall sample prepared at pH 5 than in the sample prepared at pH 2. Amine and bidentate carboxyl ligands had similar relative levels of importance in cell wall peptidoglycan samples prepared at both pH values, but phosphate coordination was insignificant. PMID:14766554

An evaluation of a reagentless method for the determination of total mercury in aquatic life

USGS Publications Warehouse

Haynes, Sekeenia; Gragg, Richard D.; Johnson, Elijah; Robinson, Larry; Orazio, Carl E.

2006-01-01

Multiple treatment (i.e., drying, chemical digestion, and oxidation) steps are often required during preparation of biological matrices for quantitative analysis of mercury; these multiple steps could potentially lead to systematic errors and poor recovery of the analyte. In this study, the Direct Mercury Analyzer (Milestone Inc., Monroe, CT) was utilized to measure total mercury in fish tissue by integrating steps of drying, sample combustion and gold sequestration with successive identification using atomic absorption spectrometry. We also evaluated the differences between the mercury concentrations found in samples that were homogenized and samples with no preparation. These results were confirmed with cold vapor atomic absorbance and fluorescence spectrometric methods of analysis. Finally, total mercury in wild captured largemouth bass (n = 20) were assessed using the Direct Mercury Analyzer to examine internal variability between mercury concentrations in muscle, liver and brain organs. Direct analysis of total mercury measured in muscle tissue was strongly correlated with muscle tissue that was homogenized before analysis (r = 0.81, p < 0.0001). Additionally, results using this integrated method compared favorably (p < 0.05) with conventional cold vapor spectrometry with atomic absorbance and fluorescence detection methods. Mercury concentrations in brain were significantly lower than concentrations in muscle (p < 0.001) and liver (p < 0.05) tissues. This integrated method can measure a wide range of mercury concentrations (0-500 ??g) using small sample sizes. Total mercury measurements in this study are comparative to the methods (cold vapor) commonly used for total mercury analysis and are devoid of laborious sample preparation and expensive hazardous waste. ?? Springer 2006.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Direct analysis of triterpenes from high-salt fermented cucumbers using infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI)

USDA-ARS?s Scientific Manuscript database

High-salt samples present a challenge to mass spectrometry (MS) analysis, particularly when electrospray ionization (ESI) is used, requiring extensive sample preparation steps such as desalting, extraction, and purification. In this study, infrared matrix-assisted laser desorption electrospray ioniz...

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope.

PubMed

Fang, Yurui; Zhang, Zhenglong; Sun, Mengtao

2016-03-01

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10(-7) Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 × 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR PREPARATION OF CALIBRATION AND SURROGATE RECOVERY SOLUTIONS FOR GC/MS ANALYSIS OF PESTICIDES (BCO-L-21.1)

EPA Science Inventory

The purpose of this SOP is to describe procedures for preparing calibration curve solutions used for gas chromatography/mass spectrometry (GC/MS) analysis of chlorpyrifos, diazinon, malathion, DDT, DDE, DDD, a-chlordane, and g-chlordane in dust, soil, air, and handwipe sample ext...

A simple non-enzymatic method for the preparation of white spot syndrome virus (WSSV) DNA from the haemolymph of Marsupenaeus japonicus using FTA matrix cards.

PubMed

Sudhakaran, R; Mekata, T; Kono, T; Supamattaya, K; Linh, N T H; Suzuki, Y; Sakai, M; Itami, T

2009-07-01

White spot syndrome virus (WSSV) is an important shrimp pathogen responsible for large economic losses for the shrimp culture industry worldwide. The nucleic acids of the virus must be adequately preserved and transported from the field to the laboratory before molecular diagnostic analysis is performed. Here, we developed a new method to isolate WSSV-DNA using Flinders Technology Associates filter paper (FTA matrix card; Whatman) without centrifugation or hazardous steps involved. FTA technology is a new method allowing the simple collection, shipment and archiving of nucleic acids from haemolymph samples providing DNA protection against nucleases, oxidation, UV damage, microbial and fungal attack. DNA samples prepared from 10-fold dilutions of moribund shrimp haemolymph using FTA matrix cards were analysed using semi-quantitative and quantitative polymerase chain reaction (PCR) and were compared with two commercially available DNA isolation methods, the blood GenomicPrep Mini Spin Kit (GE Healthcare) and the DNAzol (Invitrogen). Sequence analysis was performed for the DNA samples prepared using the various isolation procedures and no differences in the sequence among these methods were identified. Results based on the initial copy number of DNA prepared from the GenomicPrep Mini Spin Kit are a little more sensitive than the DNA prepared from FTA matrix cards, whereas the DNAzol method is not suitable for blood samples. Our data shows the efficiency of retention capacity of WSSV-DNA samples from impregnated FTA matrix cards. Matrix cards were easy to store and ship for long periods of time. They provide ease of handling and are a reliable alternative for sample collection and for molecular detection and characterization of WSSV isolates.

Thermoluminescence glow curve analysis and CGCD method for erbium doped CaZrO{sub 3} phosphor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tiwari, Ratnesh, E-mail: 31rati@gmail.com; Chopra, Seema

2016-05-06

The manuscript report the synthesis, thermoluminescence study at fixed concentration of Er{sup 3+} (1 mol%) doped CaZrO{sub 3} phosphor. The phosphors were prepared by modified solid state reaction method. The powder sample was characterized by thermoluminescence (TL) glow curve analysis. In TL glow curve the optimized concentration in 1mol% for UV irradiated sample. The kinetic parameters were calculated by computerized glow curve deconvolution (CGCD) techniaue. Trapping parameters gives the information of dosimetry loss in prepared phosphor and its usability in environmental monitoring and for personal monitoring. CGCD is the advance tool for analysis of complicated TL glow curves.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Flexible nano- and microliter injections on a single liquid chromatography-mass spectrometry system: Minimizing sample preparation and maximizing linear dynamic range.

PubMed

Lubin, Arnaud; Sheng, Sheng; Cabooter, Deirdre; Augustijns, Patrick; Cuyckens, Filip

2017-11-17

Lack of knowledge on the expected concentration range or insufficient linear dynamic range of the analytical method applied are common challenges for the analytical scientist. Samples that are above the upper limit of quantification are typically diluted and reanalyzed. The analysis of undiluted highly concentrated samples can cause contamination of the system, while the dilution step is time consuming and as the case for any sample preparation step, also potentially leads to precipitation, adsorption or degradation of the analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Sample preparation techniques for the determination of natural 15N/14N variations in amino acids by gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS).

PubMed

Hofmann, D; Gehre, M; Jung, K

2003-09-01

In order to identify natural nitrogen isotope variations of biologically important amino acids four derivatization reactions (t-butylmethylsilylation, esterification with subsequent trifluoroacetylation, acetylation and pivaloylation) were tested with standard mixtures of 17 proteinogenic amino acids and plant (moss) samples using GC-C-IRMS. The possible fractionation of the nitrogen isotopes, caused for instance by the formation of multiple reaction products, was investigated. For biological samples, the esterification of the amino acids with subsequent trifluoroacetylation is recommended for nitrogen isotope ratio analysis. A sample preparation technique is described for the isotope ratio mass spectrometric analysis of amino acids from the non-protein (NPN) fraction of terrestrial moss. 14N/15N ratios from moss (Scleropodium spec.) samples from different anthropogenically polluted areas were studied with respect to ecotoxicologal bioindication.

A ricin forensic profiling approach based on a complex set of biomarkers.

PubMed

Fredriksson, Sten-Åke; Wunschel, David S; Lindström, Susanne Wiklund; Nilsson, Calle; Wahl, Karen; Åstot, Crister

2018-08-15

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1-PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods and robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

Effect of sample preparation procedure for the determination of As, Sb and Se in fruit juices by HG-ICP-OES.

PubMed

Welna, Maja; Szymczycha-Madeja, Anna

2014-09-15

Various sample preparation procedures for the simultaneous determination of As, Sb and Se in fruit juices by hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES) were examined. Applicability of total wet digestion with HNO3/H2O2, partial decomposition (solubilisation in aqua regia), 1:1 dilution with 2% (v/v) HNO3 and direct analysis were evaluated. Hydrides were generated in the reaction of an acidified sample with NaBH4 after pre-reduction with KI-ascorbic acid for total As and Sb, and boiling with HCl for total Se. Best results, i.e. limits of detection (LODs) of 0.51-0.73 ng mL(-1), precision (RSD) within 1.7-3.6% and recoveries for spiked samples between 101% and 106% were found using aqua regia treatment. This procedure simplifying and improving sample preparation step prior to As, Sb and Se measurements in fruit juices by HG-ICP-OES, thus could be adequate for the routine analysis in terms of the quality control of these drinks. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Determination of LF-VD refining furnace slag by X ray fluorescence spectrometry].

PubMed

Kan, Bin; Cheng, Jian-ping; Song, Zu-feng

2004-10-01

Eight components, i.e. TFe, CaO, MgO, Al2O3, SiO2, TiO2, MnO and P2O5 in refining furnace slag were determined by X ray fluorescence spectrometer. Because the content of CaO was high, the authors selected 12 national and departmental grade slag standard samples and prepared a series of synthetic standard samples by adding spectrally pure reagents to them. The calibration curve is suitable to the sample analysis of CaO, MgO and SiO2 with widely varying range. Meanwhile, the points on the curve are even. The samples were prepared at high temperature by adding Li2B4O7 as flux. The experiments for the selection of the sample preparation conditions about strip reagents, melting temperature and dulition ratio were carried out. The matrix effects on absorption and enhancement were corrected by means of PH model and theoretical alpha coefficient. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

Hair analysis for cocaine: factors in laboratory contamination studies and their relevance to proficiency sample preparation and hair testing practices.

PubMed

Hill, Virginia; Cairns, Thomas; Schaffer, Michael

2008-03-21

Hair samples were contaminated by rubbing with cocaine (COC) followed by sweat application, multiple shampoo treatments and storage. The samples were then washed with isopropanol for 15min, followed by sequential aqueous washes totaling 3.5h. The amount of drug in the last wash was used to calculate a wash criterion to determine whether samples were positive due to use or contamination. Analyses of cocaine and metabolites were done by LC/MS/MS. These procedures were applied to samples produced by a U.S. government-sponsored cooperative study, in which this laboratory participated, and to samples in a parallel in-house study. All contaminated samples in both studies were correctly identified as contaminated by cutoff, benzoylecgonine (BE) presence, BE ratio, and/or the wash criterion. A method for determining hair porosity was applied to samples in both studies, and porosity characteristics of hair are discussed as they relate to experimental and real-world contamination of hair, preparation of proficiency survey samples, and analysis of unknown hair samples.

Method development for compositional analysis of low molecular weight poly(vinyl acetate) by matrix-assisted/laser desorption-mass spectrometry and its application to analysis of chewing gum.

PubMed

Tisdale, Evgenia; Wilkins, Charles

2014-04-11

The influence of the sample preparation parameters (the choice of the solvent and of the matrix:analyte ratio) was investigated and optimal conditions were established for MALDI mass spectrometry analysis of the pristine low molecular weight polyvinyl acetate (PVAc). It was demonstrated that comparison of polymer's and solvent's Hansen solubility parameters could be used as a guide when choosing the solvent for MALDI sample preparation. The highest intensity PVAc signals were obtained when ethyl acetate was used as a solvent along with the lowest matrix-analyte ratio (2,5-dihydroxybenzoic acid was used as a matrix in all experiments). The structure of the PVAc was established with high accuracy using the matrix-assisted laser desorption/ionization-Fourier transform mass spectrometry (MALDI-FTMS) analysis. It was demonstrated that PVAc undergoes unimolecular decomposition by losing acetic acid molecules from its backbone under the conditions of FTMS measurements. Number and weight average molecular weights as well as polydispersity indices were determined with both MALDI-TOF and MALDI-FTMS methods. The sample preparation protocol developed was applied to the analysis of a chewing gum and the molecular weight and structure of the polyvinyl acetate present in the sample were established. Thus, it was shown that optimized MALDI mass spectrometry could be used successfully for characterization of polyvinyl acetate in commercially available chewing gum. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of polyaniline on MWCNTs supercapacitor properties prepared by electrophoretic deposition

NASA Astrophysics Data System (ADS)

Razak, Rozelia Azila Abd; Eleas, Nor Hamizah; Mohammad, Nurul Nazwa; Yusof, Azmi Mohamed; Zaine, Intan Syaffinazzilla

2017-08-01

Multi-walled carbon nanotubes (MWCNTs) is widely used as supercapacitor electrode material. However, the specific capacitance of MWCNTs cannot achieve optimum value to facilitate required demand. Conducting polymers have been introduced to achieve optimum energy density and power density of supercapacitor electrode material. Previous work had demonstrated the effects of adding conducting polymer into carbon base material to get pseudocapacitance effect. Nevertheless the effects specifically of polyaniline (PANi) to MWCNTs were significantly low. This work describes the effect of PANi adding on MWCNTs film prepared by electrophoretic deposition (EPD) technique in order to increase the specific capacitance of MWCNTs. The commercial MWCNTs is dispersed in deionized water by using crystal violet. The admixtures without PANi (sample A), 5wt.% of PANi (sample B) and 10wt.% of PANi (sample C) have been prepared by ex-situ polymerization. The voltage supplied for film deposition is 8 V for 5 minutes. The morphology, functional group and electrochemical properties of MWCNTs due to the presence of PANi had been studied. From FESEM analysis, the presence of PANi can be clearly observed for sample B and sample C while FTIR analysis, proves PANi structure on MWCNTs with its functional group presence in sample B and sample C through the absorbtion band which obviously shifted to higher value compare to sample A. Cyclic voltammogram (CV) analysis shown redox activity occurred in sample B and sample C with identical anodic and cathodic peaks. Sample B hold the higher specific capacitance and higher energy density compared than sample A and sample B. From galvanostatic charge-discharge (CD) measurement, the charge and discharge process for sample B is longer than sample A and sample C which consequently lower its power density. The presence of PANi at 5wt.% is able to increase specific capacitance as well as energy density to optimum value.

Carbonate and silicate rock standards for cosmogenic 36Cl

NASA Astrophysics Data System (ADS)

Mechernich, Silke; Dunai, Tibor J.; Binnie, Steven A.; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred; Benedetti, Lucilla; Schimmelpfennig, Irene; Phillips, Fred; Marrero, Shasta; Akif Sarıkaya, Mehmet; Gregory, Laura C.; Phillips, Richard J.; Wilcken, Klaus; Simon, Krista; Fink, David

2017-04-01

The number of studies using cosmogenic nuclides has increased multi-fold during the last two decades and several new dedicated target preparation laboratories and Accelerator Mass Spectrometry (AMS) facilities have been established. Each facility uses sample preparation and AMS measurement techniques particular to their needs. It is thus desirable to have community-accepted and well characterized rock standards available for routine processing using identical target preparation procedures and AMS measurement methods as carried out for samples of unknown cosmogenic nuclide concentrations. The usefulness of such natural standards is that they allow more rigorous quality control, for example, the long-term reproducibility of results and hence measurement precision, or the testing of new target preparation techniques or newly established laboratories. This is particularly pertinent for in-situ 36Cl studies due to the multiplicity of 36Cl production pathways that requires a variety of elemental and isotopic determinations in addition to AMS 36Cl assay. We have prepared two natural rock samples (denoted CoCal-N and CoFsp-N) to serve as standard material for in situ-produced cosmogenic 36Cl analysis. The sample CoCal-N is a pure limestone prepared from pebbles in a Namibian lag deposit, while the alkali-feldspar CoFsp-N is derived from a single crystal in a Namibian pegmatite. The sample preparation took place at the University of Cologne, where first any impurities were removed manually from both standards. CoCal-N was leached in 10 % HNO3 to remove the outer rim, and afterwards crushed and sieved to 250-500 μm size fractions. CoFsp-N was crushed, sieved to 250-500 μm size fractions and then leached in 1% HNO3 / 1% HF until 20% of the sample were removed. Both standards were thoroughly mixed using a rotating sample splitter before being distributed to other laboratories. To date, a total of 28 CoCal-N aliquots (between 2 and 16 aliquots per facility) and 31 CoFsp-N aliquots (between 2 and 20 aliquots per facility) have been analyzed by six target preparation laboratories employing five different AMS facilities. Currently, the internal reproducibility of the measurements underlines the homogeneity of both standards. The inter-laboratory comparison suggests low over-dispersion. Further measurements are pending and should allow meaningful statistical analysis. Both standard materials are freely available and can be obtained from Tibor Dunai tdunai@uni-koeln.de).

Field Summary Report for Remedial Investigation of Hanford Site Releases to the Columbia River, Hanford Site, Washington

DOE Office of Scientific and Technical Information (OSTI.GOV)

L.C. Hulstrom

2010-09-28

This report documents field activity associated with the collection, preparation, and shipment of fish samples. The purpose of the report is to describe the sampling locations, identify samples collected, and describe any modifications and additions made to the sampling and analysis plan.

A recommended procedure for the preparation of oriented clay-mineral specimens for X-ray diffraction analysis; modifications to Drever's filter-membrane peel technique

USGS Publications Warehouse

Pollastro, R.M.

1982-01-01

Extremely well-oriented clay mineral mounts for X-ray diffraction analysis can be prepared quickly and without introducing segregation using the filter-membrane peel technique. Mounting problems encountered with smectite-rich samples can be resolved by using minimal sample and partial air-drying of the clay film before transfer to a glass slide. Samples containing small quantities of clay can produce useful oriented specimens if Teflon masks having more restrictive areas are inserted above the membrane filter during clay deposition. War]page and thermal shock of glass slides can be controlled by using a flat, porous, ceramic plate as a holding surface during heat treatments.

Improving ultraviolet photodetection of ZnO nanorods by Cr doped ZnO encapsulation process

NASA Astrophysics Data System (ADS)

Safa, S.; Mokhtari, S.; Khayatian, A.; Azimirad, R.

2018-04-01

Encapsulated ZnO nanorods (NRs) with different Cr concentration (0-4.5 at.%) were prepared in two different steps. First, ZnO NRs were grown by hydrothermal method. Then, they were encapsulated by dip coating method. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy, and ultraviolet (UV)-visible spectrophotometer analyses. XRD analysis proved that Cr incorporated into the ZnO structure successfully. Based on optical analysis, band gap changes in the range of 2.74-3.84 eV. Finally, UV responses of all samples were deeply investigated. It revealed 0.5 at.% Cr doped sample had the most photocurrent (0.75 mA) and photoresponsivity (0.8 A/W) of all which were about three times greater than photocurrent and photoresponsivity of the undoped sample.

Prevalence of bacteria and absence of anisakid parasites in raw and prepared fish and seafood dishes in Spanish restaurants.

PubMed

Sospedra, I; Rubert, J; Soriano, J M; Mañes, J; Fuentes, M V

2015-03-01

This study evaluated the presence of bacteria and anisakid parasites in 45 samples of raw anchovies in vinegar, a dish widely eaten in Spain, and in 227 samples of cooked fish and cephalopods served in Spanish food service establishments. Our analysis showed that, according to European and Spanish regulation, 14 to 30% of the prepared fish and cephalopod dishes exceeded the maximum allowable level for mesophilic aerobic counts, and 10 to 40% of these samples exceeded the allowable levels for Enterobacteriaceae. None of the studied samples showed evidence of anisakid parasites, Escherichia coli, Staphylococcus aureus, Salmonella, or Listeria monocytogenes. These results indicate that application of hazard analysis and critical control points, food safety training courses, and routine inspections in compliance with current European and Spanish legislation help protect consumer health.

Tailoring the optical and hydrophobic property of zinc oxide nanorod by coating with amorphous graphene

NASA Astrophysics Data System (ADS)

Pahari, D.; Das, N. S.; Das, B.; Chattopadhyay, K. K.; Banerjee, D.

2016-09-01

Zinc oxide (ZnO) nanorods were synthesized at room temperature on potassium permanganate activated silicon and glass substrate by simple chemical method using zinc acetate as precursor. To modify the surface energy of the as prepared ZnO thin films the samples were coated with amorphous graphene (a-G) synthesized by un-zipping of chemically synthesized amorphous carbon nanotubes (a-CNTs). All the pure and coated samples were characterized by x-ray diffraction, field emission scanning electron microscope, Raman spectroscopy, and Fourier transformed infrared spectroscopy. The roughness analysis of the as prepared samples was done by atomic force microscopic analysis. The detail optical properties of all the samples were studied with the help of a UV-Visible spectrophotometer. The surface energy of the as prepared pure and coated samples was calculated by measuring the contact angle of two different liquids. It is seen that the water repellence of ZnO nanorods got increased after they are being coated with a-Gs. Also even after UV irradiation the contact angle remain same unlike the case for the uncoated sample where the contact angle gets decreased significantly after UV irradiation. Existing Cassie-Wenzel model has been employed along with the Owen's approach to determine the different components of surface energy.

Sample preparation and detection device for infectious agents

DOEpatents

Miles, Robin R.; Wang, Amy W.; Fuller, Christopher K.; Lemoff, Asuncion V.; Bettencourt, Kerry A.; Yu, June

2003-06-10

A sample preparation and analysis device which incorporates both immunoassays and PCR assays in one compact, field-portable microchip. The device provides new capabilities in fluid and particle control which allows the building of a fluidic chip with no moving parts, thus decreasing fabrication cost and increasing the robustness of the device. The device can operate in a true continuous (not batch) mode. The device incorporates magnetohydrodynamic (MHD) pumps to move the fluid through the system, acoustic mixing and fractionation, dielectropheretic (DEP) sample concentration and purification, and on-chip optical detection capabilities.

Evidence of a miscibility gap in the FeTe1-xSex polycrystalline samples prepared with a melting process

NASA Astrophysics Data System (ADS)

Sala, A.; Palenzona, A.; Bernini, C.; Caglieris, F.; Cimberle, M. R.; Ferdeghini, C.; Lamura, G.; Martinelli, A.; Pani, M.; Hecher, J.; Eisterer, M.; Putti, M.

2014-05-01

The study of overdoped FeTe1-xSex (0.5 < x < 1) polycrystalline superconductor samples is reported. The samples were prepared using a melting technique previously developed by our group. Increasing the Se content a phase separation related to the formation of FeSe inside the Fe(Se,Te) phase happens, as demonstrated by structural analysis and magnetic characterization. The proposed phase separation picture is likely the fingerprint of a miscibility gap in the Fe(Se,Te) system.

Study on preparation of ultrafine amorphous particles by chemical reduction

NASA Astrophysics Data System (ADS)

Song, Xu; Yusheng, Xu; Huali, Jiang; Qing, Xue

1993-04-01

Ultrafine amorphous FeNiB powder was prepared by potassium borohydride reduction by mixing the aqueous solutions in a bath of supersonic oscillator. Different mixing ratios of potassium borohydride to metal salt were applied. Analysis of the composition of the sample and the Fe 2+ and Ni 2+ remaining in the filtrate after preparation shows that a quantity of KBH 4 about 1.5 times the stoichiometrical quantity is enough. Mössbauer measurements were performed at room temperature and it was found that excess KBH 4 makes no distinct difference in the spectra of the samples.

High-resolution X-ray diffraction with no sample preparation

PubMed Central

Turner, S. M. R.; Degryse, P.; Shortland, A. J.

2017-01-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions. PMID:28660862

Quantitative LIBS analysis of vanadium in samples of hexagonal mesoporous silica catalysts.

PubMed

Pouzar, Miloslav; Kratochvíl, Tomás; Capek, Libor; Smoláková, Lucie; Cernohorský, Tomás; Krejcová, Anna; Hromádko, Ludek

2011-02-15

The method for the analysis of vanadium in hexagonal mesoporous silica (V-HMS) catalysts using Laser Induced Breakdown Spectrometry (LIBS) was suggested. Commercially available LIBS spectrometer was calibrated with the aid of authentic V-HMS samples previously analyzed by ICP OES after microwave digestion. Deposition of the sample on the surface of adhesive tape was adopted as a sample preparation method. Strong matrix effect connected with the catalyst preparation technique (1st vanadium added in the process of HMS synthesis, 2nd already synthesised silica matrix was impregnated by vanadium) was observed. The concentration range of V in the set of nine calibration standards was 1.3-4.5% (w/w). Limit of detection was 0.13% (w/w) and it was calculated as a triple standard deviation from five replicated determinations of vanadium in the real sample with a very low vanadium concentration. Comparable results of LIBS and ED XRF were obtained if the same set of standards was used for calibration of both methods and vanadium was measured in the same type of real samples. LIBS calibration constructed using V-HMS-impregnated samples failed for measuring of V-HMS-synthesized samples. LIBS measurements seem to be strongly influenced with different chemical forms of vanadium in impregnated and synthesised samples. The combination of LIBS and ED XRF is able to provide new information about measured samples (in our case for example about procedure of catalyst preparation). Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

Direct Analysis of Triterpenes from High-Salt Fermented Cucumbers Using Infrared Matrix-Assisted Laser Desorption Electrospray Ionization (IR-MALDESI)

NASA Astrophysics Data System (ADS)

Ekelöf, Måns; McMurtrie, Erin K.; Nazari, Milad; Johanningsmeier, Suzanne D.; Muddiman, David C.

2017-02-01

High-salt samples present a challenge to mass spectrometry (MS) analysis, particularly when electrospray ionization (ESI) is used, requiring extensive sample preparation steps such as desalting, extraction, and purification. In this study, infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI) coupled to a Q Exactive Plus mass spectrometer was used to directly analyze 50-μm thick slices of cucumber fermented and stored in 1 M sodium chloride brine. From the several hundred unique substances observed, three triterpenoid lipids produced by cucumbers, β-sitosterol, stigmasterol, and lupeol, were putatively identified based on exact mass and selected for structural analysis. The spatial distribution of the lipids were imaged, and the putative assignments were confirmed by tandem mass spectrometry performed directly on the same cucumber, demonstrating the capacity of the technique to deliver confident identifications from highly complex samples in molar concentrations of salt without the need for sample preparation.

Evaporator Feed Qualification Analysis Of Tank 38H And 43H Samples: January 2010 Through April 2013

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martino, C. J.; Coleman, C. J.

2013-08-21

This report provides the results of analyses that focused on the chemical species that pertain to the sodium aluminosilicate formation potential for archived Tank 38H and 43H subsurface samples from January 2010 through April 2013. Analyses included warm acid strike preparation followed by analysis of silicon, aluminum, and sodium and water dilution preparation followed by analysis for anions. The Tank 43H and 38H supernatant liquid silicon measurements for the January 2010 through April 2013 time period exhibit a slight increasing trend. Over this time period, the silicon concentration in the Tank 43H and Tank 38H samples averaged 179 mg/L andmore » 235 mg/L, respectively. Comparison of Tank 43H sample results from 2005 through April 2013 to the previously developed process control models indicates that the current formation of sodium aluminosilicate in the 2H system is due to the seeded direct precipitation of cancrinite and sodalite.« less

Laser-induced breakdown spectroscopy for quantitative spectrochemical analysis of geological materials: effects of the matrix and simultaneous determination.

PubMed

Anzano, Jesús M; Villoria, Mark A; Ruíz-Medina, Antonio; Lasheras, Roberto J

2006-08-11

A microscopic laser-induced breakdown spectrometer was used to evaluate the analytical matrix effect commonly observed in the analysis of geological materials. Samples were analyzed in either the powder or pressed pellet forms. Calibration curves of a number of iron and aluminum compounds showed a linear relationship between the elemental concentration and peak intensity. A direct determination of elemental content can thus be made from extrapolation on these calibration curves. To investigate matrix effects, synthetic model samples were prepared from various iron and aluminum compounds spiked with SiO2 and CaCO3. The addition of these matrices had a pronounced analytical effect on those compounds prepared as pressed pellets. However, results indicated the absence of matrix effects when the samples were presented to the laser as loose powders on tape and results were compared to certified values, indicating the reliability of this approach for accurate analysis, provided the sample particle diameters are greater than approximately 100 microm. Finally, the simultaneous analysis of two different elements was demonstrated using powders on tape.

Quantification of 31 illicit and medicinal drugs and metabolites in whole blood by fully automated solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Bjørk, Marie Kjærgaard; Simonsen, Kirsten Wiese; Andersen, David Wederkinck; Dalsgaard, Petur Weihe; Sigurðardóttir, Stella Rögn; Linnet, Kristian; Rasmussen, Brian Schou

2013-03-01

An efficient method for analyzing illegal and medicinal drugs in whole blood using fully automated sample preparation and short ultra-high-performance liquid chromatography-tandem mass spectrometry (MS/MS) run time is presented. A selection of 31 drugs, including amphetamines, cocaine, opioids, and benzodiazepines, was used. In order to increase the efficiency of routine analysis, a robotic system based on automated liquid handling and capable of handling all unit operation for sample preparation was built on a Freedom Evo 200 platform with several add-ons from Tecan and third-party vendors. Solid-phase extraction was performed using Strata X-C plates. Extraction time for 96 samples was less than 3 h. Chromatography was performed using an ACQUITY UPLC system (Waters Corporation, Milford, USA). Analytes were separated on a 100 mm × 2.1 mm, 1.7 μm Acquity UPLC CSH C(18) column using a 6.5 min 0.1 % ammonia (25 %) in water/0.1 % ammonia (25 %) in methanol gradient and quantified by MS/MS (Waters Quattro Premier XE) in multiple-reaction monitoring mode. Full validation, including linearity, precision and trueness, matrix effect, ion suppression/enhancement of co-eluting analytes, recovery, and specificity, was performed. The method was employed successfully in the laboratory and used for routine analysis of forensic material. In combination with tetrahydrocannabinol analysis, the method covered 96 % of cases involving driving under the influence of drugs. The manual labor involved in preparing blood samples, solvents, etc., was reduced to a half an hour per batch. The automated sample preparation setup also minimized human exposure to hazardous materials, provided highly improved ergonomics, and eliminated manual pipetting.

Green and Fast Laser Fusion Technique for Bulk Silicate Rock Analysis by Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Zhang, Chenxi; Hu, Zhaochu; Zhang, Wen; Liu, Yongsheng; Zong, Keqing; Li, Ming; Chen, Haihong; Hu, Shenghong

2016-10-18

Sample preparation of whole-rock powders is the major limitation for their accurate and precise elemental analysis by laser ablation inductively-coupled plasma mass spectrometry (ICPMS). In this study, a green, efficient, and simplified fusion technique using a high energy infrared laser was developed for major and trace elemental analysis. Fusion takes only tens of milliseconds for each sample. Compared to the pressed pellet sample preparation, the analytical precision of the developed laser fusion technique is higher by an order of magnitude for most elements in granodiorite GSP-2. Analytical results obtained for five USGS reference materials (ranging from mafic to intermediate to felsic) using the laser fusion technique generally agree with recommended values with discrepancies of less than 10% for most elements. However, high losses (20-70%) of highly volatile elements (Zn and Pb) and the transition metal Cu are observed. The achieved precision is within 5% for major elements and within 15% for most trace elements. Direct laser fusion of rock powders is a green and notably simple method to obtain homogeneous samples, which will significantly accelerate the application of laser ablation ICPMS for whole-rock sample analysis.

ZnO/Ag nanocomposite: an efficient catalyst for degradation studies of textile effluents under visible light.

PubMed

Saravanan, R; Karthikeyan, N; Gupta, V K; Thirumal, E; Thangadurai, P; Narayanan, V; Stephen, A

2013-05-01

Degradation of model organic dye and industry effluent was studied using different weight percentages of Ag into ZnO as a catalyst. In this study, the catalysts were prepared by thermal decomposition method, which was employed for the first time in the preparation of ZnO/Ag nanocomposite catalysts. The physical and chemical properties of the prepared samples were studied using various techniques. The specific surface area, which plays an important role in the photocatalytic degradation, was studied using BET analysis and 10 wt.% Ag into ZnO showed the best degrading efficiency. The optical absorption (UV-vis) and emission (PL) properties of the samples were studied and results suggest better photocatalytic properties for 10 wt.% Ag sample compared to other samples. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

NASA Astrophysics Data System (ADS)

Crevelin, Eduardo J.; Salami, Fernanda H.; Alves, Marcela N. R.; De Martinis, Bruno S.; Crotti, Antônio E. M.; Moraes, Luiz A. B.

2016-05-01

Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis.

PubMed

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-05

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p=0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis

NASA Astrophysics Data System (ADS)

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-01

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4 mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p = 0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes.

Rapid identification of bacteria with miniaturized pyrolysis/GC analysis

NASA Astrophysics Data System (ADS)

Morgan, Catherine H.; Mowry, Curtis; Manginell, Ronald P.; Frye-Mason, Gregory C.; Kottenstette, Richard J.; Lewis, Patrick

2001-02-01

Identification of bacteria and other biological moieties finds a broad range of applications in the environmental, biomedical, agricultural, industrial, and military arenas. Linking these applications are biological markers such as fatty acids, whose mass spectral profiles can be used to characterize biological samples and to distinguish bacteria at the gram-type, genera, and even species level. Common methods of sample analysis require sample preparation that is both lengthy and labor intensive, especially for whole cell bacteria. The background technique relied on here utilizes chemical derivatization of fatty acids to the more volatile fatty acid methyl esters (FAMEs), which can be separated on a gas chromatograph column or input directly into a mass spectrometer. More recent publications demonstrate improved sample preparation time with in situ derivatization of whole bacterial samples using pyrolysis at the inlet; although much faster than traditional techniques, these systems still rely on bench-top analytical equipment and individual sample preparation. Development of a miniaturized pyrolysis/GC instrument by this group is intended to realize the benefits of FAME identification of bacteria and other biological samples while further facilitating sample handling and instrument portability. The technologies being fabricated and tested have the potential of achieving pyrolysis and FAME separation on a very small scale, with rapid detection time (1-10 min from introduction to result), and with a modular sample inlet. Performance results and sensor characterization will be presented for the first phase of instrument development, encompassing the microfabricated pyrolysis and gas chromatograph elements.

Inorganic chemical analysis of environmental materials—A lecture series

USGS Publications Warehouse

Crock, J.G.; Lamothe, P.J.

2011-01-01

At the request of the faculty of the Colorado School of Mines, Golden, Colorado, the authors prepared and presented a lecture series to the students of a graduate level advanced instrumental analysis class. The slides and text presented in this report are a compilation and condensation of this series of lectures. The purpose of this report is to present the slides and notes and to emphasize the thought processes that should be used by a scientist submitting samples for analyses in order to procure analytical data to answer a research question. First and foremost, the analytical data generated can be no better than the samples submitted. The questions to be answered must first be well defined and the appropriate samples collected from the population that will answer the question. The proper methods of analysis, including proper sample preparation and digestion techniques, must then be applied. Care must be taken to achieve the required limits of detection of the critical analytes to yield detectable analyte concentration (above "action" levels) for the majority of the study's samples and to address what portion of those analytes answer the research question-total or partial concentrations. To guarantee a robust analytical result that answers the research question(s), a well-defined quality assurance and quality control (QA/QC) plan must be employed. This QA/QC plan must include the collection and analysis of field and laboratory blanks, sample duplicates, and matrix-matched standard reference materials (SRMs). The proper SRMs may include in-house materials and/or a selection of widely available commercial materials. A discussion of the preparation and applicability of in-house reference materials is also presented. Only when all these analytical issues are sufficiently addressed can the research questions be answered with known certainty.

Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis.

PubMed

Quaresma, Maria Cristina Baptista; de Carvalho, Maria de Fátima Batista; Meirelles, Francis Assis; Santiago, Vânia Maria Junqueira; Santelli, Ricardo Erthal

2007-02-01

A sample preparation procedure for the quantitative determination of free and total cyanides in industrial effluents has been developed that involves hydrocyanic acid vapor generation via focused microwave radiation. Hydrocyanic acid vapor was generated from free cyanides using only 5 min of irradiation time (90 W power) and a purge time of 5 min. The HCN generated was absorbed into an accepting NaOH solution using very simple glassware apparatus that was appropriate for the microwave oven cavity. After that, the cyanide concentration was determined within 90 s using a well-known spectrophotometric flow injection analysis system. Total cyanide analysis required 15 min irradiation time (90 W power), as well as chemical conditions such as the presence of EDTA-acetate buffer solution or ascorbic acid, depending on the effluent to be analyzed (petroleum refinery or electroplating effluents, respectively). The detection limit was 0.018 mg CN l(-1) (quantification limit of 0.05 mg CN l(-1)), and the measured RSD was better than 8% for ten independent analyses of effluent samples (1.4 mg l(-1) cyanide). The accuracy of the procedure was assessed via analyte spiking (with free and complex cyanides) and by performing an independent sample analysis based on the standard methodology recommended by the APHA for comparison. The sample preparation procedure takes only 10 min for free and 20 min for total cyanide, making this procedure much faster than traditional methodologies (conventional heating and distillation), which are time-consuming (they require at least 1 h). Samples from oil (sour and stripping tower bottom waters) and electroplating effluents were analyzed successfully.

The determination of elements in herbal teas and medicinal plant formulations and their tisanes.

PubMed

Pohl, Pawel; Dzimitrowicz, Anna; Jedryczko, Dominika; Szymczycha-Madeja, Anna; Welna, Maja; Jamroz, Piotr

2016-10-25

Elemental analysis of herbal teas and their tisanes is aimed at assessing their quality and safety in reference to specific food safety regulations and evaluating their nutritional value. This survey is dedicated to atomic spectroscopy and mass spectrometry element detection methods and sample preparation procedures used in elemental analysis of herbal teas and medicinal plant formulations. Referring to original works from the last 15 years, particular attention has been paid to tisane preparation, sample matrix decomposition, calibration and quality assurance of results in elemental analysis of herbal teas by different atomic and mass spectrometry methods. In addition, possible sources of elements in herbal teas and medicinal plant formulations have been discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

Utility of eButton images for identifying food preparation behaviors and meal-related tasks in adolescents.

PubMed

Raber, Margaret; Patterson, Monika; Jia, Wenyan; Sun, Mingui; Baranowski, Tom

2018-02-24

Food preparation skills may encourage healthy eating. Traditional assessment of child food preparation employs self- or parent proxy-reporting methods, which are prone to error. The eButton is a wearable all-day camera that has promise as an objective, passive method for measuring child food preparation practices. This paper explores the feasibility of the eButton to reliably capture home food preparation behaviors and practices in a sample of pre- and early adolescents (ages 9 to 13). This is a secondary analysis of two eButton pilot projects evaluating the dietary intake of pre- and early adolescents in or around Houston, Texas. Food preparation behaviors were coded into seven major categories including: browsing, altering food/adding seasoning, food media, meal related tasks, prep work, cooking and observing. Inter-coder reliability was measured using Cohen's kappa and percent agreement. Analysis was completed on data for 31 participants. The most common activity was browsing in the pantry or fridge. Few participants demonstrated any food preparation work beyond unwrapping of food packages and combining two or more ingredients; actual cutting or measuring of foods were rare. Although previous research suggests children who "help" prepare meals may obtain some dietary benefit, accurate assessment tools of food preparation behavior are lacking. The eButton offers a feasible approach to food preparation behavior measurement among pre- and early adolescents. Follow up research exploring the validity of this method in a larger sample, and comparisons between cooking behavior and dietary intake are needed.

Tracking Matrix Effects in the Analysis of DNA Adducts of Polycyclic Aromatic Hydrocarbons

PubMed Central

Klaene, Joshua J.; Flarakos, Caroline; Glick, James; Barret, Jennifer T.; Zarbl, Helmut; Vouros, Paul

2015-01-01

LC-MS using electrospray ionization is currently the method of choice in bio-organic analysis covering a wide range of applications in a broad spectrum of biological media. The technique is noted for its high sensitivity but one major limitation which hinders achievement of its optimal sensitivity is the signal suppression due to matrix inferences introduced by the presence of co-extracted compounds during the sample preparation procedure. The analysis of DNA adducts of common environmental carcinogens is particularly sensitive to such matrix effects as sample preparation is a multistep process which involves “contamination” of the sample due to the addition of enzymes and other reagents for digestion of the DNA in order to isolate the analyte(s). This problem is further exacerbated by the need to reach low levels of quantitation (LOQ in the ppb level) while also working with limited (2-5 μg) quantities of sample. We report here on the systematic investigation of ion signal suppression contributed by each individual step involved in the sample preparation associated with the analysis of DNA adducts of polycyclic aromatic hydrocarbon (PAH) using as model analyte dG-BaP, the deoxyguanosine adduct of benzo[a]pyrene (BaP). The individual matrix contribution of each one of these sources to analyte signal was systematically addressed as were any interactive effects. The information was used to develop a validated analytical protocol for the target biomarker at levels typically encountered in vivo using as little as 2 μg of DNA and applied to a dose response study using a metabolically competent cell line. PMID:26607319

Environmental Asbestos Assessment Manual: Superfund Method for the Determination of Asbestos in Ambient Air, Part 1: Method

EPA Science Inventory

This is a sampling and analysis method for the determination of asbestos in air. Samples are analyzed by transmission electron microscopy (TEM). Although a small subset of samples are to be prepared using a direct procedure, the majority of samples analyzed using this method wil...

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to ∼1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had ∼2.5× higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice ∼25 μm cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

Thermoelectric properties and thermal stability of Bi-doped PbTe single crystal

NASA Astrophysics Data System (ADS)

Chen, Zhong; Li, Decong; Deng, Shuping; Tang, Yu; Sun, Luqi; Liu, Wenting; Shen, Lanxian; Yang, Peizhi; Deng, Shukang

2018-06-01

In this study, n-type Bi-doped single-crystal PbTe thermoelectric materials were prepared by melting and slow cooling method according to the stoichiometric ratio of Pb:Bi:Te = 1-x:x:1 (x = 0, 0.1, 0.15, 0.2, 0.25). The X-ray diffraction patterns of Pb1-xBixTe samples show that all main diffraction peaks are well matched with the PbTe matrix, which has a face-centered cubic structure with the space group Fm 3 bar m . Electron probe microanalysis reveals that Pb content decreases gradually, and Te content remains invariant basically with the increase of Bi content, indicating that Bi atoms are more likely to replace Pb atoms. Thermal analysis shows that the prepared samples possess relatively high thermal stability. Simultaneously, transmission electron microscopy and selected area electron diffraction pattern indicate that the prepared samples have typical single-crystal structures with good mechanical properties. Moreover, the electrical conductivity of the prepared samples improved significantly compared with that of the pure sample, and the maximum ZT value of 0.84 was obtained at 600 K by the sample with x = 0.2.

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken frommore » the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.« less

Analysis of microstructure and mechanical properties of aluminium-copper joints welded by FSW process

NASA Astrophysics Data System (ADS)

Iordache, M.; Sicoe, G.; Iacomi, D.; Niţu, E.; Ducu, C.

2017-08-01

The research conducted in this article aimed to check the quality of joining some dissimilar materials Al-Cu by determining the mechanical properties and microstructure analysis. For the experimental measurements there were used tin alloy Al - EN-AW-1050A with a thickness of 2 mm and Cu99 sheet with a thickness of 2 mm, joined by FSW weld overlay. The main welding parameters were: rotating speed of the rotating element 1400 rev/min, speed of the rotating element 50 mm/min. The experimental results were determined on samples specially prepared for metallographic analysis. In order to prepare samples for their characterization, there was designed and built a device that allowed simultaneous positioning and fixing for grinding. The characteristics analyzed in the joint welded samples were mictrostructure, microhardness and residual stresses. The techniques used to determine these characteristics were optical microscopy, electron microscopy with fluorescence radioactive elemental analysis (EDS), Vickers microhardness line - HV0.3 and X-ray diffractometry.

Analysis of human tissues by total reflection X-ray fluorescence. Application of chemometrics for diagnostic cancer recognition

NASA Astrophysics Data System (ADS)

Benninghoff, L.; von Czarnowski, D.; Denkhaus, E.; Lemke, K.

1997-07-01

For the determination of trace element distributions of more than 20 elements in malignant and normal tissues of the human colon, tissue samples (approx. 400 mg wet weight) were digested with 3 ml of nitric acid (sub-boiled quality) by use of an autoclave system. The accuracy of measurements has been investigated by using certified materials. The analytical results were evaluated by using a spreadsheet program to give an overview of the element distribution in cancerous samples and in normal colon tissues. A further application, cluster analysis of the analytical results, was introduced to demonstrate the possibility of classification for cancer diagnosis. To confirm the results of cluster analysis, multivariate three-way principal component analysis was performed. Additionally, microtome frozen sections (10 μm) were prepared from the same tissue samples to compare the analytical results, i.e. the mass fractions of elements, according to the preparation method and to exclude systematic errors depending on the inhomogeneity of the tissues.

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fang, Yurui; Bionanophotonics, Department of Applied Physics, Chalmers University of Technology, Göteborg, SE 41296; Zhang, Zhenglong

2016-03-15

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10{sup −7} Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 ×more » 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.« less

Comparing paraffined and deparaffinized breast cancer tissue samples and an analysis of Raman spectroscopy and infrared methods

NASA Astrophysics Data System (ADS)

Depciuch, J.; Kaznowska, E.; Szmuc, K.; Zawlik, I.; Cholewa, M.; Heraud, P.; Cebulski, J.

2016-05-01

Breast cancer makes up a quarter of all cancer in women, which is why research into new diagnostic methods and sample preparations need to be developed at an accelerated pace. Researchers are looking for diagnostic tools to detect when an individual has cancer cells and use that information to see what measurements and approaches can be used to take further diagnostic steps. The most common method of sample preparation is the imbibing of tumor tissue in paraffin, which can produce a background for spectroscopic measurements in the range of 500-3500 cm-1. In this study we demonstrated that proper preparation of paraffin-embedded specimens and the measurement methodology can eliminate paraffin vibration, as was done in the work Depciuch et al. 2015. Thanks to this spectroscopic technique there may become a reliable and accurate method of diagnosing breast cancer based on the evidence found from the prepared samples. The study compared the results obtained through Raman spectroscopy and FTIR (Fourier Transform Infrared) measurements of healthy and cancerous breast tissues that were either embedded in paraffin or deparaffinized. The resulting spectrum and accurate analysis led to the conclusion that the appropriate measurement of the background and the elimination of peaks from the paraffin had the greatest impact on the reliability of results. Furthermore, after the accurate, detailed studies FTIR and Raman spectroscopy on samples of breast tissue that were deparaffinized or embedded in paraffin, including a complete analysis of the peak after transformation Kramers-Kröning (KK), it was found that sample preparation did not affect the result obtained by measuring the reflectance in the mid-infrared range, and that this only had a minimal effect relating to the intensity obtained by the measurement of the Raman peak. Only in special cases, when Raman spectroscopic methods are used for research to find the peculiarities of the spectra, are deparaffinization recommended, in order to attain more detailed results that could be crucial in understanding the process of carcinogenesis.

Bridging the gap between sample collection and laboratory analysis: using dried blood spots to identify human exposure to chemical agents

NASA Astrophysics Data System (ADS)

Hamelin, Elizabeth I.; Blake, Thomas A.; Perez, Jonas W.; Crow, Brian S.; Shaner, Rebecca L.; Coleman, Rebecca M.; Johnson, Rudolph C.

2016-05-01

Public health response to large scale chemical emergencies presents logistical challenges for sample collection, transport, and analysis. Diagnostic methods used to identify and determine exposure to chemical warfare agents, toxins, and poisons traditionally involve blood collection by phlebotomists, cold transport of biomedical samples, and costly sample preparation techniques. Use of dried blood spots, which consist of dried blood on an FDA-approved substrate, can increase analyte stability, decrease infection hazard for those handling samples, greatly reduce the cost of shipping/storing samples by removing the need for refrigeration and cold chain transportation, and be self-prepared by potentially exposed individuals using a simple finger prick and blood spot compatible paper. Our laboratory has developed clinical assays to detect human exposures to nerve agents through the analysis of specific protein adducts and metabolites, for which a simple extraction from a dried blood spot is sufficient for removing matrix interferents and attaining sensitivities on par with traditional sampling methods. The use of dried blood spots can bridge the gap between the laboratory and the field allowing for large scale sample collection with minimal impact on hospital resources while maintaining sensitivity, specificity, traceability, and quality requirements for both clinical and forensic applications.

Advantages of infrared transflection micro spectroscopy and paraffin-embedded sample preparation for biological studies

NASA Astrophysics Data System (ADS)

Yao, Jie; Li, Qian; Zhou, Bo; Wang, Dan; Wu, Rie

2018-04-01

Fourier-Transform Infrared micro-spectroscopy is an excellent method for biological analyses. In this paper, series metal coating films on ITO glass were prepared by the electrochemical method and the different thicknesses of paraffin embedding rat's brain tissue on the substrates were studied by IR micro-spetroscopy in attenuated total reflection (ATR) mode and transflection mode respectively. The Co-Ni-Cu alloy coating film with low cost is good reflection substrates for the IR analysis. The infrared microscopic transflection mode needs not to touch the sample at all and can get the IR spectra with higher signal to noise ratios. The Paraffin-embedding method allows tissues to be stored for a long time for re-analysis to ensure the traceability of the sample. Also it isolates the sample from the metal and avoids the interaction of biological tissue with the metals. The best thickness of the tissues is 4 μm.

Cooked Food Waste-An Efficient and Less Expensive Precursor for the Generation of Activated Carbon.

PubMed

Krithiga, Thangavelu; Sabina, Xavier Janet; Rajesh, Baskaran; Ilbeygi, Hamid; Shetty, Adka Nityananda; Reddy, Ramanjaneya; Karthikeyan, Jayabalan

2018-06-01

Activated carbon was synthesized from cooked food waste, especially dehydrated rice kernels, by chemical activation method using NaOH and KOH as activating agents. It was then characterized by ultimate and proximate analysis, BET surface analysis, XRD, FTIR, Raman and SEM. The XRD patterns and Raman spectra confirmed the amorphous nature of the prepared activated carbons. Ultimate analysis showed an increase in the carbon content after activation of the raw carbon samples. Upon activation with NaOH and KOH, the surface area of the carbon sample was found to have increased from 0.3424 to 539.78 and 306.83 m2g-1 respectively. The SEM images revealed the formation of heterogeneous pores on the surface of the activated samples. The samples were then tested for their adsorption activity using acetic acid and methylene blue. Based on the regression coefficients, the adsorption kinetics of methylene blue dye were fitted with pseudo-second order model for both samples. Similarly, the Freundlich isotherm was found to be a better fit than Langmuir isotherm for both samples. The activity of thus prepared activated carbons was found to be comparable with the commercial carbon.

Techniques for the inorganic analysis in a controlled ecological life support system

NASA Technical Reports Server (NTRS)

1983-01-01

Sample preparation, instrumental analysis, a direct injection device for IC/ICP interfacing, a hydraulic jet bend impaction device, monodisperse aerosol generator, and low gravity environments are discussed.

Final Technical Report for subcontract number B612144

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mayali, X.; Marcu, O.

The original statement of work stipulated that the Subcontractor shall perform bacterial and algal cultivation and manipulation, microbe isolation, preparation of samples for sequencing and isotopic analysis, data analysis, and manuscript preparation. The Subcontractor shall work closely with Dr. Mayali and other LLNL scientists, and shall participate in monthly SFA meetings (either in person or by telephone). The Subcontractor shall deliver a final report at the conclusion of the work.

Perchlorate in Fertilizers

DTIC Science & Technology

1999-09-01

Harrington , showed that with respect to mixed water analysis containing TDS at greater 1,000 ppm, the performance of the AS-5 column is not as robust...to note, these raw test materials were heterogeneous. Regardless of mixing time and mesh quality, dividing the raw test materials for laboratory...raw test material was prepared and shipped to seven laboratories for blind analysis. The suspension was prepared by 4 mixing the solid sample with

Autonomous microfluidic sample preparation system for protein profile-based detection of aerosolized bacterial cells and spores.

PubMed

Stachowiak, Jeanne C; Shugard, Erin E; Mosier, Bruce P; Renzi, Ronald F; Caton, Pamela F; Ferko, Scott M; Van de Vreugde, James L; Yee, Daniel D; Haroldsen, Brent L; VanderNoot, Victoria A

2007-08-01

For domestic and military security, an autonomous system capable of continuously monitoring for airborne biothreat agents is necessary. At present, no system meets the requirements for size, speed, sensitivity, and selectivity to warn against and lead to the prevention of infection in field settings. We present a fully automated system for the detection of aerosolized bacterial biothreat agents such as Bacillus subtilis (surrogate for Bacillus anthracis) based on protein profiling by chip gel electrophoresis coupled with a microfluidic sample preparation system. Protein profiling has previously been demonstrated to differentiate between bacterial organisms. With the goal of reducing response time, multiple microfluidic component modules, including aerosol collection via a commercially available collector, concentration, thermochemical lysis, size exclusion chromatography, fluorescent labeling, and chip gel electrophoresis were integrated together to create an autonomous collection/sample preparation/analysis system. The cycle time for sample preparation was approximately 5 min, while total cycle time, including chip gel electrophoresis, was approximately 10 min. Sensitivity of the coupled system for the detection of B. subtilis spores was 16 agent-containing particles per liter of air, based on samples that were prepared to simulate those collected by wetted cyclone aerosol collector of approximately 80% efficiency operating for 7 min.

Closed tubes preparation of graphite for high-precision AMS radiocarbon analysis

NASA Astrophysics Data System (ADS)

Hajdas, I.; Michczynska, D.; Bonani, G.; Maurer, M.; Wacker, L.

2009-04-01

Radiocarbon dating is an established tool applied in Geochronology. Technical developments of Accelerator Mass Spectrometry AMS, which allow measurements of samples containing less than 1 mg of carbon, opened opportunities for new applications. Moreover, high resolution records of the past changes require high-resolution chronologies i.e. sampling for 14C dating. In result, the field of applications is rapidly expanding and number of radiocarbon analysis is growing rapidly. Nowadays dedicated 14C AMS machines have great capacity for analysis but in order to keep up with the demand for analysis and provide the results as fast as possible a very efficient way of sample preparation is required. Sample preparation for 14C AMS analysis consists of two steps: separation of relevant carbon from the sample material (removing contamination) and preparation of graphite for AMS analysis. The last step usually involves reaction of CO2 with H2, in the presence of metal catalyst (Fe or Co) of specific mesh size heated to 550-625°C, as originally suggested by Vogel et al. (1984). Various graphitization systems have been built in order to fulfil the requirement of sample quality needed for high-precision radiocarbon data. In the early 90ties another method has been proposed (Vogel 1992) and applied by few laboratories mainly for environmental or biomedical samples. This method uses TiH2 as a source of H2 and can be easily and flexibly applied to produce graphite. Sample of CO2 is frozen in to the tube containing pre-conditioned Zn/TiH2 and Fe catalyst. Torch sealed tubes are then placed in the stepwise heated oven at 500/550°C and left to react for several hours. The greatest problem is the lack of control of the reaction completeness and considerable fractionation. However, recently reported results (Xu et al. 2007) suggest that high precision dating using graphite produced in closed tubes might be possible. We will present results of radiocarbon dating of the set of standards and secondary IAEA standards to demonstrate to what level this method can be used for high precision radiocarbon dating. References Vogel JS. 1992. Rapid Production of Graphite without Contamination for Biomedical Ams. Radiocarbon 34: 344-350. Vogel JS, Southon JR, Nelson DE, and Brown TA. 1984. Performance of Catalytically Condensed Carbon for Use in Accelerator Mass-Spectrometry. Nuclear Instruments & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 233: 289-293. Xu X, Trumbore SE, Zheng S, Southon JR, McDuffee KE, Luttgen M, and Liu JC. 2007. Modifying a sealed tube zinc reduction method for preparation of AMS graphite targets: Reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms Accelerator Mass Spectrometry - Proceedings of the Tenth International Conference on Accelerator Mass Spectrometry 259: 320-329.

Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity

NASA Astrophysics Data System (ADS)

Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.

2015-12-01

Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to < 10 TU currently) since the cessation of above ground nuclear testing in the 1960's. We are developing sample preparation methods coupled to direct counting of T via ultra-low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks depending on T content.

Combined liquid chromatography-mass spectrometry for trace analysis of pharmaceuticals

NASA Astrophysics Data System (ADS)

Schmidt, Lothar; Danigel, Harald; Jungclas, Hartmut

1982-07-01

A 252Cf-plasma desorption mass spectrometer (PDMS) for the analysis of thin layers from nonvolatile organic samples has been set up to be combined with a liquid chromatograph. A novel interface performs the direct inlet of the liquid sample through a capillary into the vacuum system of the spectrometer. Samples of drugs are periodically collected, transferred to the ion source and analysed using a rotating disk. This on-line sample preparation has been tested for three antiarrhythmic drugs using various solvents and mixtures.

Trace Chemical Analysis Methodology

DTIC Science & Technology

1980-04-01

oxidation of nitrite-containing species. Calibration studies were then made in preparation for the analysis of unknown samples of nitrate in urine and...the procedure for nitrate determination was made on two types of samples : human urine , and drinking water from a city water supply. Five samples of...AND URINE Concentration Standard Sample type of NO3, ppm deviation Drinking water 1.29 ±0 04 1.20 ±0.09 1.29 ±0.14 1.15 ±0.08 0.88 ±0.07 Human urine

Preparation and Certification of Two New Bulk Welding Fume Reference Materials for Use in Laboratories Undertaking Analysis of Occupational Hygiene Samples

PubMed Central

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

Workers can be exposed to fume, arising from welding activities, which contain toxic metals and metalloids. Occupational hygienists need to assess and ultimately minimize such exposure risks. The monitoring of the concentration of particles in workplace air is one assessment approach whereby fume, from representative welding activities, is sampled onto a filter and returned to a laboratory for analysis. Inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry are generally employed as instrumental techniques of choice for the analysis of such filter samples. An inherent difficulty, however, with inductively coupled plasma-based analytical techniques is that they typically require a sample to be presented for analysis in the form of a solution. The efficiency of the required dissolution step relies heavily upon the skill and experience of the analyst involved. A useful tool in assessing the efficacy of this dissolution step would be the availability and subsequent analysis of welding fume reference materials with stated elemental concentrations and matrices that match as closely as possible the matrix composition of welding fume samples submitted to laboratories for analysis. This article describes work undertaken at the Health and Safety Laboratory to prepare and certify two new bulk welding fume reference materials that can be routinely used by analysts to assess the performance of the digestion procedures they employ in their laboratories. PMID:24499055

Preparation and certification of two new bulk welding fume reference materials for use in laboratories undertaking analysis of occupational hygiene samples.

PubMed

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

Workers can be exposed to fume, arising from welding activities, which contain toxic metals and metalloids. Occupational hygienists need to assess and ultimately minimize such exposure risks. The monitoring of the concentration of particles in workplace air is one assessment approach whereby fume, from representative welding activities, is sampled onto a filter and returned to a laboratory for analysis. Inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry are generally employed as instrumental techniques of choice for the analysis of such filter samples. An inherent difficulty, however, with inductively coupled plasma-based analytical techniques is that they typically require a sample to be presented for analysis in the form of a solution. The efficiency of the required dissolution step relies heavily upon the skill and experience of the analyst involved. A useful tool in assessing the efficacy of this dissolution step would be the availability and subsequent analysis of welding fume reference materials with stated elemental concentrations and matrices that match as closely as possible the matrix composition of welding fume samples submitted to laboratories for analysis. This article describes work undertaken at the Health and Safety Laboratory to prepare and certify two new bulk welding fume reference materials that can be routinely used by analysts to assess the performance of the digestion procedures they employ in their laboratories.

Mixed-mode ion exchange-based integrated proteomics technology for fast and deep plasma proteome profiling.

PubMed

Xue, Lu; Lin, Lin; Zhou, Wenbin; Chen, Wendong; Tang, Jun; Sun, Xiujie; Huang, Peiwu; Tian, Ruijun

2018-06-09

Plasma proteome profiling by LC-MS based proteomics has drawn great attention recently for biomarker discovery from blood liquid biopsy. Due to standard multi-step sample preparation could potentially cause plasma protein degradation and analysis variation, integrated proteomics sample preparation technologies became promising solution towards this end. Here, we developed a fully integrated proteomics sample preparation technology for both fast and deep plasma proteome profiling under its native pH. All the sample preparation steps, including protein digestion and two-dimensional fractionation by both mixed-mode ion exchange and high-pH reversed phase mechanism were integrated into one spintip device for the first time. The mixed-mode ion exchange beads design achieved the sample loading at neutral pH and protein digestion within 30 min. Potential sample loss and protein degradation by pH changing could be voided. 1 μL of plasma sample with depletion of high abundant proteins was processed by the developed technology with 12 equally distributed fractions and analyzed with 12 h of LC-MS gradient time, resulting in the identification of 862 proteins. The combination of the Mixed-mode-SISPROT and data-independent MS method achieved fast plasma proteome profiling in 2 h with high identification overlap and quantification precision for a proof-of-concept study of plasma samples from 5 healthy donors. We expect that the Mixed-mode-SISPROT become a generally applicable sample preparation technology for clinical oriented plasma proteome profiling. Copyright © 2018 Elsevier B.V. All rights reserved.

Simple and rapid determination of serotonin and catecholamines in biological tissue using high-performance liquid chromatography with electrochemical detection.

PubMed

Patel, Bhavik Anil; Arundell, Martin; Parker, Kim H; Yeoman, Mark S; O'Hare, Danny

2005-04-25

Using the CNS of Lymnaea stagnalis a method is described for the rapid analysis of neurotransmitters and their metabolites using high performance liquid chromatography coupled with electrochemical detection. Tissue samples were homogenised in ice-cold 0.1 M perchloric acid and centrifuged. Using a C(18) microbore column the mobile phase was maintained at a flow rate of 100 microl/min and consisted of sodium citrate buffer (pH 3.2)-acetonitrile (82.5:17.5, v/v) with 2 mM decane-sulfonic acid sodium salt. The potential was set at +750 mV versus Ag|AgCl reference electrode at a sensitivity of 50 nA full scale deflection. The detection limit for serotonin was 11.86 ng ml(-1) for a 5 microl injection. Preparation of tissue samples in mobile phase reduced the response to dopamine and serotonin compared with perchloric acid. In addition it was found that the storage of tissue samples at -20 degrees C caused losses of dopamine and serotonin. As a result of optimising the sample preparation and mobile phase the total time of analysis was substantially reduced resulting in a sample preparation and assay time of 15-20 min.

Analysis of Carbohydrate and Fatty Acid Marker Abundance in Ricin Toxin Preparations for Forensic Information

DOE Office of Scientific and Technical Information (OSTI.GOV)

Colburn, Heather A.; Wunschel, David S.; Kreuzer-Martin, Helen W.

2010-07-15

One challenge in the forensic analysis of ricin samples is determining the method and extent of sample preparation. Ricin purification from the source castor seeds is essentially a protein purification through removal of the non-protein fractions of the seed. Two major, non-protein constituents in the seed are the castor oil and carbohydrates. Ricinoleic acid is a relatively unique fatty acid in nature and is the most abundant component of castor oil, which comprises roughly half the seed weight. The carbohydrate component comprises roughly half of the remaining “mash” left after oil and hull removal. We used derivatization of carbohydrate andmore » fatty acid markers followed by identification and quantification using gas chromatography/mass spectrometry (GC/MS) to assess compositional changes in ricin samples purified by different methods. The loss of ricinoleic acid indicated steps for oil removal had occurred. Changes to the carbohydrate content of the sample were also observed following protein precipitation. The differential loss of arabinose relative to mannose indicated removal of the major carbohydrate fraction of the seed and enrichment of the protein content. Taken together, these changes in fatty acid and carbohydrate abundance are indicative of the preparation method used for each sample.« less

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

PubMed

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

Spectral Characterization of H2020/PTAL Mineral Samples: Implications for In Situ Martian Exploration and Mars Sample Selection

NASA Astrophysics Data System (ADS)

Lantz, C.; Pilorget, C.; Poulet, F.; Riu, L.; Dypvik, H.; Hellevang, H.; Rull Perez, F.; Veneranda, M.; Cousin, A.; Viennet, J.-C.; Werner, S. C.

2018-04-01

We present combined analysis performed in the framework of the Planetary Terrestrial Analogues Library (H2020 project). XRD, NIR, Raman, and LIBS spectroscopies are used to characterise samples to prepare ExoMars/ESA and Mars2020/NASA observations.

Applications of reversible covalent chemistry in analytical sample preparation.

PubMed

Siegel, David

2012-12-07

Reversible covalent chemistry (RCC) adds another dimension to commonly used sample preparation techniques like solid-phase extraction (SPE), solid-phase microextraction (SPME), molecular imprinted polymers (MIPs) or immuno-affinity cleanup (IAC): chemical selectivity. By selecting analytes according to their covalent reactivity, sample complexity can be reduced significantly, resulting in enhanced analytical performance for low-abundance target analytes. This review gives a comprehensive overview of the applications of RCC in analytical sample preparation. The major reactions covered include reversible boronic ester formation, thiol-disulfide exchange and reversible hydrazone formation, targeting analyte groups like diols (sugars, glycoproteins and glycopeptides, catechols), thiols (cysteinyl-proteins and cysteinyl-peptides) and carbonyls (carbonylated proteins, mycotoxins). Their applications range from low abundance proteomics to reversible protein/peptide labelling to antibody chromatography to quantitative and qualitative food analysis. In discussing the potential of RCC, a special focus is on the conditions and restrictions of the utilized reaction chemistry.

Multiple-step preparation and physicochemical characterization of crystalline α-germanium hydrogenphosphate

NASA Astrophysics Data System (ADS)

Romano, Ricardo; Ruiz, Ana I.; Alves, Oswaldo L.

2004-04-01

The reaction between germanium oxide and phosphoric acid has previously been described and led to impure germanium hydrogenphosphate samples with low crystallinity. A new multiple-step route involving the same reaction under refluxing and soft hydrothermal conditions is described for the preparation of pure and crystalline α-GeP. The physicochemical characterization of the samples allows accompaniment of the reaction evolution as well as determining short- and long-range structural organization. The phase purity of the α-GeP sample was confirmed by applying Rietveld's profile analysis, which also determined the cell parameters of its crystals.

Optical Properties of Natural Minerals in the Far-Infrared

NASA Astrophysics Data System (ADS)

Long, Larry Lavern

The reflectivity of natural mineral powders were measured in the far infrared. The complex indices of refraction were then determined by Kramers-Kronig analysis or dispersive analysis. The samples were constructed by pressing the powdered sample into a 13 mm diameter pellet. A few of the samples that were measured were kaolin, illite, and montmorillonite, clay samples that could not be obtained in large single crystals. For calcite and gypsum crystals a comparison between the single crystal measurements and powder measurements was done to determine the effect of sample preparation on the measured spectra.

High temperature flow-through device for rapid solubilization and analysis

DOEpatents

West, Jason A. A. [Castro Valley, CA; Hukari, Kyle W [San Ramon, CA; Patel, Kamlesh D [Dublin, CA; Peterson, Kenneth A [Albuquerque, NM; Renzi, Ronald F [Tracy, CA

2009-09-22

Devices and methods for thermally lysing of biological material, for example vegetative bacterial cells and bacterial spores, are provided. Hot solution methods for solubilizing bacterial spores are described. Systems for direct analysis are disclosed including thermal lysers coupled to sample preparation stations. Integrated systems capable of performing sample lysis, labeling and protein fingerprint analysis of biological material, for example, vegetative bacterial cells, bacterial spores and viruses are provided.

High temperature flow-through device for rapid solubilization and analysis

DOEpatents

West, Jason A. A.; Hukari, Kyle W.; Patel, Kamlesh D.; Peterson, Kenneth A.; Renzi, Ronald F.

2013-04-23

Devices and methods for thermally lysing of biological material, for example vegetative bacterial cells and bacterial spores, are provided. Hot solution methods for solubilizing bacterial spores are described. Systems for direct analysis are disclosed including thermal lysers coupled to sample preparation stations. Integrated systems capable of performing sample lysis, labeling and protein fingerprint analysis of biological material, for example, vegetative bacterial cells, bacterial spores and viruses are provided.

Analytical platform for metabolome analysis of microbial cells using methyl chloroformate derivatization followed by gas chromatography-mass spectrometry.

PubMed

Smart, Kathleen F; Aggio, Raphael B M; Van Houtte, Jeremy R; Villas-Bôas, Silas G

2010-09-01

This protocol describes an analytical platform for the analysis of intra- and extracellular metabolites of microbial cells (yeast, filamentous fungi and bacteria) using gas chromatography-mass spectrometry (GC-MS). The protocol is subdivided into sampling, sample preparation, chemical derivatization of metabolites, GC-MS analysis and data processing and analysis. This protocol uses two robust quenching methods for microbial cultures, the first of which, cold glycerol-saline quenching, causes reduced leakage of intracellular metabolites, thus allowing a more reliable separation of intra- and extracellular metabolites with simultaneous stopping of cell metabolism. The second, fast filtration, is specifically designed for quenching filamentous micro-organisms. These sampling techniques are combined with an easy sample-preparation procedure and a fast chemical derivatization reaction using methyl chloroformate. This reaction takes place at room temperature, in aqueous medium, and is less prone to matrix effect compared with other derivatizations. This protocol takes an average of 10 d to complete and enables the simultaneous analysis of hundreds of metabolites from the central carbon metabolism (amino and nonamino organic acids, phosphorylated organic acids and fatty acid intermediates) using an in-house MS library and a data analysis pipeline consisting of two free software programs (Automated Mass Deconvolution and Identification System (AMDIS) and R).

Community-Level Physiological Profiling of Microbial Communities in Constructed Wetlands: Effects of Sample Preparation.

PubMed

Button, Mark; Weber, Kela; Nivala, Jaime; Aubron, Thomas; Müller, Roland Arno

2016-03-01

Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized.

EPA Method 3135.2I: Cyanide, Total and Amenable in Aqueous and Solid Samples Automated Colorimetric With Manual Digestion

EPA Pesticide Factsheets

This method describes procedures for preparation and analysis of solid, water and wipe samples for detection and measurement of cyanide amendable to chlorination using acid digestion and spectrophotometry.

Preparation and Thermoelectric Properties of Semiconcucting Zn(sub 4) Sb(sub 3)

NASA Technical Reports Server (NTRS)

Caillat, T.; Fleurial, J. P.; Barshchevsky, A.

1996-01-01

Hot-pressed samples fothe semiconducting compound Beta - Zn(sub 4) Sb(sub 3) were prepared and characterized by x-ray and microprobe analysis. Some physical properties of Beta - Zn(sub 4) Sb(sub 3) were determined and its thermoelectric properties measured between room temperature and 650K.

The Preparation and Simple Analysis of a Clay Nanoparticle Composite Hydrogel

ERIC Educational Resources Information Center

Warren, David S.; Sutherland, Sam P. H.; Kao, Jacqueline Y.; Weal, Geoffrey R.; Mackay, Sean M.

2017-01-01

Samples of a composite hydrogel incorporating clay (Laponite XLG and S-482) nanoparticles were prepared using N-isopropylacrylamide. The hydrogels were formed via a radical-initiated addition polymerization using potassium persulfate and N,N,N',N'-tetramethylethylenediamine. Students then measured the force required to stretch the gels and…

Simultaneous quantification of fluoxetine and norfluoxetine in colostrum and mature human milk using a 2-dimensional liquid chromatography-tandem mass spectrometry system.

PubMed

Lopes, Bianca Rebelo; Cassiano, Neila Maria; Carvalho, Daniela Miarelli; Moisés, Elaine Christine Dantas; Cass, Quezia Bezerra

2018-02-20

A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the determination of fluoxetine (FLU) and norfluoxetine (N-FLU) in colostrum and mature milk by direct sample injection. With a run time of 12 min representing a gain in throughput analysis, the validated methods furnished selectivity, extraction efficiency, accuracy, and precision in accordance with the criteria preconized by the European Medicines Agency guidelines. With a linear range of 3.00-150 ng/mL for FLU and 4.00-200 ng/mL for N-FLU they were applied to the analysis of colostrum and mature milk samples from nursing mothers. The paper discusses the differences and similarity of sample preparation for this two sample matrices. The herein reported methods are an advance in sample preparation procedures providing waste reduction and a sustainable approach. Copyright © 2017 Elsevier B.V. All rights reserved.

Computer graphics for quality control in the INAA of geological samples

USGS Publications Warehouse

Grossman, J.N.; Baedecker, P.A.

1987-01-01

A data reduction system for the routine instrumental activation analysis of samples is described, with particular emphasis on interactive graphics capabilities for evaluating analytical quality. Graphics procedures have been developed to interactively control the analysis of selected photopeaks during spectral analysis, and to evaluate detector performance during a given counting cycle. Graphics algorithms are also used to compare the data on reference samples with accepted values, to prepare quality control charts to evaluate long term precision and to search for systematic variations in data on reference samples as a function of time. ?? 1987 Akade??miai Kiado??.

Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

PubMed

Baghdady, Yehia Z; Schug, Kevin A

2016-01-01

Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Acid digestion of geological and environmental samples using open-vessel focused microwave digestion.

PubMed

Taylor, Vivien F; Toms, Andrew; Longerich, Henry P

2002-01-01

The application of open vessel focused microwave acid digestion is described for the preparation of geological and environmental samples for analysis using inductively coupled plasma-mass spectrometry (ICP-MS). The method is compared to conventional closed-vessel high pressure methods which are limited in the use of HF to break down silicates. Open-vessel acid digestion more conveniently enables the use of HF to remove Si from geological and plant samples as volatile SiF4, as well as evaporation-to-dryness and sequential acid addition during the procedure. Rock reference materials (G-2 granite, MRG-1 gabbros, SY-2 syenite, JA-1 andesite, and JB-2 and SRM-688 basalts) and plant reference materials (BCR and IAEA lichens, peach leaves, apple leaves, Durham wheat flour, and pine needles) were digested with results comparable to conventional hotplate digestion. The microwave digestion method gave poor results for granitic samples containing refractory minerals, however fusion was the preferred method of preparation for these samples. Sample preparation time was reduced from several days, using conventional hotplate digestion method, to one hour per sample using our microwave method.

Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandrakumar, K.

2016-04-01

The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol-gel, microwave assisted sol-gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6-12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M-H curve of all the samples. But the sol-gel derived sample shows the higher values of saturation magnetization (Ms) and remanence (Mr) than other two samples. This study reveals that the sol-gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.

Multivariable Analysis of Gluten-Free Pasta Elaborated with Non-Conventional Flours Based on the Phenolic Profile, Antioxidant Capacity and Color.

PubMed

Camelo-Méndez, Gustavo A; Flores-Silva, Pamela C; Agama-Acevedo, Edith; Bello-Pérez, Luis A

2017-12-01

The phenolic compounds, color and antioxidant capacity of gluten-free pasta prepared with non-conventional flours such as chickpea (CHF), unripe plantain (UPF), white maize (WMF) and blue maize (BMF) were analyzed. Fifteen phenolic compounds (five anthocyanins, five hydroxybenzoic acids, three hydroxycinnamic acids, one hydroxyphenylacetic acid and one flavonol) were identified in pasta prepared with blue maize, and 10 compounds were identified for samples prepared with white maize. The principal component analysis (PCA) led to results describing 98% of the total variance establishing a clear separation for each pasta. Both the proportion (25, 50 and 75%) and type of maize flour (white and blue) affected the color parameters (L*, C ab *, h ab and ΔE* ab ) and antioxidant properties (DPPH, ABTS and FRAP methods) of samples, thus producing gluten-free products with potential health benefits intended for general consumers (including the population with celiac disease).

The effect of preliminary hydrolysis on the properties of ZrO2-7% Y2O3 powders prepared by hydroxide precipitation

NASA Astrophysics Data System (ADS)

Zhirenkina, Nina V.; Mashkovtsev, Maxim A.; Bereskina, Polina A.; Zakirov, Ilsur F.; Baksheev, Evgenie O.; Bujnachev, Sergey V.; Vereshchagin, Artem O.

2017-09-01

In this study, the effect of preliminary hydrolysis of zirconyl oxysulfate on the properties of ZrO2-7 % Y2O3 powders prepared by hydroxides precipitation at a constant pH of 5 was studied. X-ray diffraction analysis showed the monophasic nature of the samples and the insignificant difference between CSR (coherent scattering regions). Samples differed in particle size distribution, porosity and morphology.

Apparatus for preparing a sample for mass spectrometry

DOEpatents

Villa-Aleman, Eliel

1994-01-01

An apparatus for preparing a sample for analysis by a mass spectrometer system. The apparatus has an entry chamber and an ionization chamber separated by a skimmer. A capacitor having two space-apart electrodes followed by one or more ion-imaging lenses is disposed in the ionization chamber. The chamber is evacuated and the capacitor is charged. A valve injects a sample gas in the form of sample pulses into the entry chamber. The pulse is collimated by the skimmer and enters the ionization chamber. When the sample pulse passes through the gap between the electrodes, it discharges the capacitor and is thereby ionized. The ions are focused by the imaging lenses and enter the mass analyzer, where their mass and charge are analyzed.

Associations among School Characteristics and Foodservice Practices in a Nationally Representative Sample of U.S. Schools

PubMed Central

Thomson, Jessica L.; Tussing-Humphreys, Lisa M.; Martin, Corby K.; LeBlanc, Monique M.; Onufrak, Stephen J.

2012-01-01

Objective Determine school characteristics associated with healthy/unhealthy foodservice offerings or healthy food preparation practices. Design Retrospective analysis of cross-sectional data. Setting Nationally representative sample of public and private elementary, middle and high schools. Participants 526 and 520 schools with valid data from the 2006 School Health Policies and Practices Study (SHPPS) Food Service School Questionnaire. Main Outcome Measure(s) Scores for healthy/unhealthy foodservice offerings and healthy food preparation practices. Analysis Multivariable regression to determine significant associations among school characteristics and offerings/preparation practices. Results Public schools and schools participating in USDA Team Nutrition reported more healthy offerings and preparation than private or non-participating schools, respectively. Elementary schools reported less unhealthy offerings than middle or high schools; middle schools reported less unhealthy offerings than high schools. Schools requiring foodservice managers to have a college education reported more healthy preparation while those requiring completion of a foodservice training program reported less unhealthy offerings and more healthy preparation than schools without these requirements. Conclusions and Implications Results suggest the school nutrition environment may be improved by requiring foodservice managers to hold a nutrition-related college degree and/or successfully pass a foodservice training program, and by participating in a school-based nutrition program, such as USDA Team Nutrition. PMID:22963956

Storage of cell samples for ToF-SIMS experiments-How to maintain sample integrity.

PubMed

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Henss, Anja; Wenisch, Sabine; Janek, Jürgen

2016-06-25

In order to obtain comparable and reproducible results from time-of-flight secondary ion mass spectrometry (ToF-SIMS) analysis of biological cells, the influence of sample preparation and storage has to be carefully considered. It has been previously shown that the impact of the chosen preparation routine is crucial. In continuation of this work, the impact of storage needs to be addressed, as besides the fact that degradation will unavoidably take place, the effects of different storage procedures in combination with specific sample preparations remain largely unknown. Therefore, this work examines different wet (buffer, water, and alcohol) and dry (air-dried, freeze-dried, and critical-point-dried) storage procedures on human mesenchymal stem cell cultures. All cell samples were analyzed by ToF-SIMS immediately after preparation and after a storage period of 4 weeks. The obtained spectra were compared by principal component analysis with lipid- and amino acid-related signals known from the literature. In all dry storage procedures, notable degradation effects were observed, especially for lipid-, but also for amino acid-signal intensities. This leads to the conclusion that dried samples are to some extent easier to handle, yet the procedure is not the optimal storage solution. Degradation proceeds faster, which is possibly caused by oxidation reactions and cleaving enzymes that might still be active. Just as well, wet stored samples in alcohol struggle with decreased signal intensities from lipids and amino acids after storage. Compared to that, the wet stored samples in a buffered or pure aqueous environment revealed no degradation effects after 4 weeks. However, this storage bears a higher risk of fungi/bacterial contamination, as sterile conditions are typically not maintained. Thus, regular solution change is recommended for optimized storage conditions. Not directly exposing the samples to air, wet storage seems to minimize oxidation effects, and hence, buffer or water storage with regular renewal of the solution is recommended for short storage periods.

Storage of cell samples for ToF-SIMS experiments—How to maintain sample integrity

PubMed Central

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Henss, Anja; Wenisch, Sabine; Janek, Jürgen

2016-01-01

In order to obtain comparable and reproducible results from time-of-flight secondary ion mass spectrometry (ToF-SIMS) analysis of biological cells, the influence of sample preparation and storage has to be carefully considered. It has been previously shown that the impact of the chosen preparation routine is crucial. In continuation of this work, the impact of storage needs to be addressed, as besides the fact that degradation will unavoidably take place, the effects of different storage procedures in combination with specific sample preparations remain largely unknown. Therefore, this work examines different wet (buffer, water, and alcohol) and dry (air-dried, freeze-dried, and critical-point-dried) storage procedures on human mesenchymal stem cell cultures. All cell samples were analyzed by ToF-SIMS immediately after preparation and after a storage period of 4 weeks. The obtained spectra were compared by principal component analysis with lipid- and amino acid-related signals known from the literature. In all dry storage procedures, notable degradation effects were observed, especially for lipid-, but also for amino acid-signal intensities. This leads to the conclusion that dried samples are to some extent easier to handle, yet the procedure is not the optimal storage solution. Degradation proceeds faster, which is possibly caused by oxidation reactions and cleaving enzymes that might still be active. Just as well, wet stored samples in alcohol struggle with decreased signal intensities from lipids and amino acids after storage. Compared to that, the wet stored samples in a buffered or pure aqueous environment revealed no degradation effects after 4 weeks. However, this storage bears a higher risk of fungi/bacterial contamination, as sterile conditions are typically not maintained. Thus, regular solution change is recommended for optimized storage conditions. Not directly exposing the samples to air, wet storage seems to minimize oxidation effects, and hence, buffer or water storage with regular renewal of the solution is recommended for short storage periods. PMID:26810048

Classification of bacteria by simultaneous methylation-solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters.

PubMed

Lu, Yao; Harrington, Peter B

2010-08-01

Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid-liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 +/- 3% correct classification efficiency.

Preparation of activated carbon monolith by application of phenolic resins as carbon precursors

NASA Astrophysics Data System (ADS)

Sajad, Mehran; Kazemzad, Mahmood; Hosseinnia, Azarmidokht

2014-04-01

In the current work, activated carbon monoliths have been prepared by application of different phenolic hydrocarbons namely catechol and resorcinol as carbon precursors. For synthesis of carbon monolith, the precursors have been mixed with Genapol PF-10 as template and then polymerized in the presence of lysine as catalyst. Then the polymerized monolith carbonized in inert atmosphere at 700°C and activated by water steam at 550°C. It was found that resorcinol polymerization is easier than catechol and occurred at 90°C while for polymerization of catechol elevated temperature of 120°C at hydrothermal condition is necessary. The prepared activated carbon samples have been characterized by various analysis methods including scanning electron microscopy (SEM), surface area measurement, and transmission electron microscopy (TEM). The adsorptions of three different aromatic hydrocarbons by the prepared activated carbon samples have also been investigated by high performance liquid chromatography (HPLC) and UV-Vis spectroscopy. It was found that carbon monolith prepared by catechol as carbon precursor has higher adsorpability and strength in comparison with the other sample. The higher performance of carbon monolith prepared by catechol can be associated with its higher active sites in comparison with resorcinol.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR COLLECTION OF SURFACE WIPE SAMPLES FOR PESTICIDES OR METALS ANALYSIS (UA-F-8.1)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for collecting surface wipe samples inside a home for analysis of either metals or pesticides. This procedure covers the preparation of the surface wipe material and field activities. This protocol was followed to ensure con...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF SOIL AND HOUSE DUST SAMPLES FOR GC/MS ANALYSIS OF PESTICIDE AND PAH (BCO-L-28.0)

EPA Science Inventory

The purpose of this SOP is to describe procedures for extracting and preparing a dust or soil sample for gas chromatography mass spectrometry (GC/MS) analysis of pesticides and polyaromatic hydrocarbons (PAHs). This procedure was followed to ensure consistent data retrieval durin...

Determination of 14C/ 12C of acetaldehyde in indoor air by compound specific radiocarbon analysis

NASA Astrophysics Data System (ADS)

Kato, Yoshimi; Shinohara, Naohide; Yoshinaga, Jun; Uchida, Masao; Matsuda, Ayuri; Yoneda, Minoru; Shibata, Yasuyuki

A method of compound-specific radiocarbon analysis (CSRA) for acetaldehyde in indoor air was established for the source apportionment purpose and the methodology was applied to indoor air samples. Acetaldehyde in indoor air samples was collected using the conventional 2,4-dinitrophenylhydrazine (DNPH) derivatization method. Typically 24-h air sampling at 5-10 L min -1 allowed collection of adequate amount of acetaldehyde for radiocarbon analysis by accelerator mass spectrometry (AMS). The 14C abundance of acetaldehyde in indoor air was measured by AMS after solvent extraction of derivatized acetaldehyde and sequential purification by a preparative liquid chromatography system and a preparative capillary gas chromatography system. The recovery and purity of the derivatized acetaldehyde was satisfactory for 14C analysis by AMS. 14C abundance of acetaldehyde was calculated by considering that of derivatizing agent DNPH. Our preliminary survey showed that percent modern carbon (pMC) values of acetaldehyde isolated from indoor air sampled in newly built, unoccupied housings ( n=5) in the suburb of Tokyo ranged from 49.4 to 67.0. This result indicated that contribution of anthropogenic source was greater than previously expected.

Electrical and thermal properties of Ca and Ni doped barium ferrite

NASA Astrophysics Data System (ADS)

Agrawal, Shraddha; Parveen, Azra; Azam, Ameer

2018-05-01

Ca and Ni doped M type Barium ferrite of the composition ((Ba0.9Ca0.1) (Fe0.8 Ni0.2)12O19) were prepared by the traditional sol gel auto combustion method using citric acid as a fuel. Microstructural analyses were carried out with the help of XRD and SEM. XRD analysis is the evidence of nanometer regime along with crystalline planes of hexagonal structure. It also confirms the hexagonal structure of barium ferrite even with the doping of Ca and Ni. SEM analysis is the signature of the spherical shape and surface morphology of agglomerated form of nano-powders of doped samples. The thermal properties of samples were carried out with the help of TGA. That shows the variation of weight loss of the prepared sample with the temperature.

Detection of halogenated flame retardants in polyurethane foam by particle induced X-ray emission

NASA Astrophysics Data System (ADS)

Maley, Adam M.; Falk, Kyle A.; Hoover, Luke; Earlywine, Elly B.; Seymour, Michael D.; DeYoung, Paul A.; Blum, Arlene; Stapleton, Heather M.; Peaslee, Graham F.

2015-09-01

A novel application of particle-induced X-ray emission (PIXE) has been developed to detect the presence of chlorinated and brominated flame retardant chemicals in polyurethane foams. Traditional Gas Chromatography-Mass Spectrometry (GC-MS) methods for the detection and identification of halogenated flame retardants in foams require extensive sample preparation and data acquisition time. The elemental analysis of the halogens in polyurethane foam performed by PIXE offers the opportunity to identify the presence of halogenated flame retardants in a fraction of the time and sample preparation cost. Through comparative GC-MS and PIXE analysis of 215 foam samples, excellent agreement between the two methods was obtained. These results suggest that PIXE could be an ideal rapid screening method for the presence of chlorinated and brominated flame retardants in polyurethane foams.

Preparing Monodisperse Macromolecular Samples for Successful Biological Small-Angle X-ray and Neutron Scattering Experiments

PubMed Central

Jeffries, Cy M.; Graewert, Melissa A.; Blanchet, Clément E.; Langley, David B.; Whitten, Andrew E.; Svergun, Dmitri I

2017-01-01

Small-angle X-ray and neutron scattering (SAXS and SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume including the solvent and buffer components as well as the macromolecules of interest. In order to obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis so it is essential that the samples are pure and monodisperse for the duration of the experiment. This Protocol outlines the basic physics of SAXS and SANS and reveals how the underlying conceptual principles of the techniques ultimately ‘translate’ into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size exclusion chromatography and light scattering. Also included are procedures specific to X-rays (in-line size exclusion chromatography SAXS) and neutrons, specifically preparing samples for contrast matching/variation experiments and deuterium labeling of proteins. PMID:27711050

Cytology Preparations of Formalin Fixative Aid Detection of Giardia in Duodenal Biopsy Samples.

PubMed

Panarelli, Nicole C; Gobara, Nariman; Hoda, Rana S; Chaump, Michael; Jessurun, Jose; Yantiss, Rhonda K

2017-04-01

Giardiasis is the most common intestinal parasitic infection in the United States. The organism elicits no, or minimal, inflammatory changes in duodenal biopsy samples, so it can be easily overlooked. We performed this study to determine whether Giardia could be isolated from the formalin fixative of biopsy samples, and to evaluate the value of fluid analysis in the assessment for potential infection. We prospectively evaluated duodenal biopsy samples from 92 patients with a clinical suspicion of giardiasis or symptoms compatible with that diagnosis (ie, diarrhea, bloating, or abdominal pain) Biopsy samples were routinely processed and stained with hematoxylin and eosin. Histologic diagnoses included giardiasis (5 cases, 4%), normal findings (64 cases, 70%), peptic injury/active duodenitis (12 cases, 13%), and intraepithelial lymphocytosis with villous blunting (10 cases, 12%). Fifteen cases (13%) showed detached degenerated epithelial cells or mucus droplets in the intervillous space that resembled Giardia. Cytology slides were prepared from formalin in the biopsy container using the standard Cytospin protocol and reviewed by a cytopathologist blinded to the biopsy findings. Cytologic evaluation revealed Giardia spp. in all 5 biopsy-proven cases, and identified an additional case that was not detected by biopsy analysis. Organisms were significantly more numerous (mean: 400 trophozoites; range, 120 to 810) and showed better morphologic features in cytology preparations compared with tissue sections (mean: 129 trophozoites; range, 37 to 253 organisms; P=0.05). Our findings suggest that cytology preparations from formalin fixative can resolve diagnostically challenging cases and even enhance Giardia detection in some cases.

Spectrochemical analysis of powdered biological samples using transversely excited atmospheric carbon dioxide laser plasma excitation

NASA Astrophysics Data System (ADS)

Zivkovic, Sanja; Momcilovic, Milos; Staicu, Angela; Mutic, Jelena; Trtica, Milan; Savovic, Jelena

2017-02-01

The aim of this study was to develop a simple laser induced breakdown spectroscopy (LIBS) method for quantitative elemental analysis of powdered biological materials based on laboratory prepared calibration samples. The analysis was done using ungated single pulse LIBS in ambient air at atmospheric pressure. Transversely-Excited Atmospheric pressure (TEA) CO2 laser was used as an energy source for plasma generation on samples. The material used for the analysis was a blue-green alga Spirulina, widely used in food and pharmaceutical industries and also in a few biotechnological applications. To demonstrate the analytical potential of this particular LIBS system the obtained spectra were compared to the spectra obtained using a commercial LIBS system based on pulsed Nd:YAG laser. A single sample of known concentration was used to estimate detection limits for Ba, Ca, Fe, Mg, Mn, Si and Sr and compare detection power of these two LIBS systems. TEA CO2 laser based LIBS was also applied for quantitative analysis of the elements in powder Spirulina samples. Analytical curves for Ba, Fe, Mg, Mn and Sr were constructed using laboratory produced matrix-matched calibration samples. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used as the reference technique for elemental quantification, and reasonably well agreement between ICP and LIBS data was obtained. Results confirm that, in respect to its sensitivity and precision, TEA CO2 laser based LIBS can be successfully applied for quantitative analysis of macro and micro-elements in algal samples. The fact that nearly all classes of materials can be prepared as powders implies that the proposed method could be easily extended to a quantitative analysis of different kinds of materials, organic, biological or inorganic.

Metrological approach to quantitative analysis of clinical samples by LA-ICP-MS: A critical review of recent studies.

PubMed

Sajnóg, Adam; Hanć, Anetta; Barałkiewicz, Danuta

2018-05-15

Analysis of clinical specimens by imaging techniques allows to determine the content and distribution of trace elements on the surface of the examined sample. In order to obtain reliable results, the developed procedure should be based not only on the properly prepared sample and performed calibration. It is also necessary to carry out all phases of the procedure in accordance with the principles of chemical metrology whose main pillars are the use of validated analytical methods, establishing the traceability of the measurement results and the estimation of the uncertainty. This review paper discusses aspects related to sampling, preparation and analysis of clinical samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with emphasis on metrological aspects, i.e. selected validation parameters of the analytical method, the traceability of the measurement result and the uncertainty of the result. This work promotes the introduction of metrology principles for chemical measurement with emphasis to the LA-ICP-MS which is the comparative method that requires studious approach to the development of the analytical procedure in order to acquire reliable quantitative results. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid detection of bacteria with miniaturized pyrolysis-gas chromatographic analysis

NASA Astrophysics Data System (ADS)

Mowry, Curtis; Morgan, Catherine H.; Baca, Quentin; Manginell, Ronald P.; Kottenstette, Richard J.; Lewis, Patrick; Frye-Mason, Gregory C.

2002-02-01

Rapid detection and identification of bacteria and other pathogens is important for many civilian and military applications. The profiles of biological markers such as fatty acids can be used to characterize biological samples or to distinguish bacteria at the gram-type, genera, and even species level. Common methods for whole cell bacterial analysis are neither portable nor rapid, requiring lengthy, labor intensive sample preparation and bench-scale instrumentation. These methods chemically derivatize fatty acids to produce more volatile fatty acid methyl esters (FAMEs) that can be separated and analyzed by a gas chromatograph (GC)/mass spectrometer. More recent publications demonstrate decreased sample preparation time with in situ derivatization of whole bacterial samples using pyrolysis/derivatization. Ongoing development of miniaturized pyrolysis/GC instrumentation by this department capitalizes on Sandia advances in the field of microfabricated chemical analysis systems ((mu) ChemLab). Microdevices include rapidly heated stages capable of pyrolysis or sample concentration, gas chromatography columns, and surface acoustic wave (SAW) sensor arrays. We will present results demonstrating the capabilities of these devices toward fulfilling the goal of portable, rapid detection and early warning of the presence of pathogens in air or water.

Influence of Capping Ligand and Synthesis Method on Structure and Morphology of Aqueous Phase Synthesized CuInSe2 Nanoparticles

NASA Astrophysics Data System (ADS)

Ram Kumar, J.; Ananthakumar, S.; Moorthy Babu, S.

2017-01-01

A facile route to synthesize copper indium diselenide (CuInSe2) nanoparticles in aqueous medium was developed using mercaptoacetic acid (MAA) as capping agent. Two different mole ratios (5 and 10) of MAA were used to synthesize CuInSe2 nanoparticles at room temperature, as well as hydrothermal (high temperature) method. Powder x-ray diffraction analysis reveals that the nanoparticles exhibit chalcopyrite phase and the crystallinity increases with increasing the capping ratio. Raman analysis shows a strong band at 233 cm-1 due to the combination of B2 (E) modes. Broad absorption spectra were observed for the synthesized CuInSe2 nanoparticles. The effective surface capping by MAA on the nanoparticles surface was confirmed through attenuated total reflection-Fourier transform infrared spectral analysis. The thermal stability of the synthesized samples was analyzed through thermogravimetric analysis-differential scanning calorimetry. The change in morphology of the synthesized samples was analyzed through scanning electron microscope and it shows that the samples prepared at room temperature are spherical in shape, whereas hydrothermally synthesized samples were found to have nanorod- and nanoflake-like structures. Transmission electron microscope analysis further indicates larger grains for the hydrothermally prepared samples with 10 mol ratio of MAA. Comparative analyses were made for synthesizing CuInSe2 nanoparticles by two different methods to explore the role of ligand and influence of temperature.

Optical Methods for Identifying Hard Clay Core Samples During Petrophysical Studies

NASA Astrophysics Data System (ADS)

Morev, A. V.; Solovyeva, A. V.; Morev, V. A.

2018-01-01

X-ray phase analysis of the general mineralogical composition of core samples from one of the West Siberian fields was performed. Electronic absorption spectra of the clay core samples with an added indicator were studied. The speed and availability of applying the two methods in petrophysical laboratories during sample preparation for standard and special studies were estimated.

Quantifying inter-laboratory variability in stable isotope analysis of ancient skeletal remains.

PubMed

Pestle, William J; Crowley, Brooke E; Weirauch, Matthew T

2014-01-01

Over the past forty years, stable isotope analysis of bone (and tooth) collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond), the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a) sample preparation, and b) analysis (instrumentation, working standards, and data calibration). Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration). These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite isotope values. To address the issues arising from inter-laboratory comparisons, we devise a novel measure we term the Minimum Meaningful Difference (MMD), and demonstrate its application.

Quantifying Inter-Laboratory Variability in Stable Isotope Analysis of Ancient Skeletal Remains

PubMed Central

Pestle, William J.; Crowley, Brooke E.; Weirauch, Matthew T.

2014-01-01

Over the past forty years, stable isotope analysis of bone (and tooth) collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond), the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a) sample preparation, and b) analysis (instrumentation, working standards, and data calibration). Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration). These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite isotope values. To address the issues arising from inter-laboratory comparisons, we devise a novel measure we term the Minimum Meaningful Difference (MMD), and demonstrate its application. PMID:25061843

Marine sediment sample preparation for analysis for low concentrations of fine detrital gold

USGS Publications Warehouse

Clifton, H. Edward; Hubert, Arthur; Phillips, R. Lawrence

1967-01-01

Analyses by atomic absorption for detrital gold in more than 2,000 beach, offshore, marine-terrace, and alluvial sands from southern Oregon have shown that the values determined from raw or unconcentrated sediment containing small amounts of gold are neither reproducible nor representative of the initial sample. This difficulty results from a 'particle sparsity effect', whereby the analysis for gold in a given sample depends more upon the occurrence of random flakes of gold in the analyzed portion than upon the actual gold content of the sample. The particle sparsity effect can largely be eliminated by preparing a gold concentrate prior to analysis. A combination of sieve, gravimetric, and magnetic separation produces a satisfactory concentrate that yields accurate and reproducible analyses. In concentrates of nearly every marine and beach sand studied, the gold occurs in the nonmagnetic fraction smaller than 0.124 mm and with a specific gravity greater than 3.3. The grain size of gold in stream sediments is somewhat more variable. Analysis of concentrates provides a means of greatly increasing the sensitivity of the analytical technique in relation to the initial sample. Gold rarely exceeds 1 part per million in even the richest black sand analyzed; to establish the distribution of gold (and platinum) in marine sediments and its relationship to source and environmental factors, one commonly needs to know their content to the part per billion range. Analysis of a concentrate and recalculation to the value in the initial sample permits this degree of sensitivity.

Preparation and Analysis of Solid Solutions in the Potassium Perchlorate-Permanganate System.

ERIC Educational Resources Information Center

Johnson, Garrett K.

1979-01-01

Describes an experiment, designed for and tested in an advanced inorganic laboratory methods course for college seniors and graduate students, that prepares and analyzes several samples in the nearly ideal potassium perchlorate-permanganate solid solution series. The results are accounted for by a theoretical treatment based upon aqueous…

Optimization and validation of a fully automated silica-coated magnetic beads purification technology in forensics.

PubMed

Nagy, M; Otremba, P; Krüger, C; Bergner-Greiner, S; Anders, P; Henske, B; Prinz, M; Roewer, L

2005-08-11

Automated procedures for forensic DNA analyses are essential not only for large-throughput sample preparation, but are also needed to avoid errors during routine sample preparation. The most critical stage in PCR-based forensic analysis is DNA isolation, which should yield as much highly purified DNA as possible. The extraction method used consists of pre-treatment of stains and samples, cell lysis using chaotropic reagents, binding of the DNA to silica-coated magnetic particles, followed by elution of the DNA. Our work focuses mainly on sample preparation, obtaining the maximum possible amount of biological material from forensic samples, and the following cell lysis, to create a simple standardized lysis protocol suitable for nearly all forensic material. After optimization and validation, the M-48 BioRobot((R)) workstation has been used for more than 20,000 routine lab samples. There has been no evidence of cross contamination. Resulting DNA from as small as three nuclear cells yield reliable complete STR amplification profiles. The DNA remains stable after 2 years of storage.

Solid-Phase Extraction (SPE): Principles and Applications in Food Samples.

PubMed

Ötles, Semih; Kartal, Canan

2016-01-01

Solid-Phase Extraction (SPE) is a sample preparation method that is practised on numerous application fields due to its many advantages compared to other traditional methods. SPE was invented as an alternative to liquid/liquid extraction and eliminated multiple disadvantages, such as usage of large amount of solvent, extended operation time/procedure steps, potential sources of error, and high cost. Moreover, SPE can be plied to the samples combined with other analytical methods and sample preparation techniques optionally. SPE technique is a useful tool for many purposes through its versatility. Isolation, concentration, purification and clean-up are the main approaches in the practices of this method. Food structures represent a complicated matrix and can be formed into different physical stages, such as solid, viscous or liquid. Therefore, sample preparation step particularly has an important role for the determination of specific compounds in foods. SPE offers many opportunities not only for analysis of a large diversity of food samples but also for optimization and advances. This review aims to provide a comprehensive overview on basic principles of SPE and its applications for many analytes in food matrix.

Electrical, structural and thermal studies of carbon nanotubes from natural legume seeds: kala chana

NASA Astrophysics Data System (ADS)

Ranu, Rachana; Chauhan, Yatishwar; Singh, Pramod K.; Bhattacharya, B.; Tomar, S. K.

2016-12-01

Carbon nanotubes (CNTs) are the carbon materials measured at nanoscale level and they are defined in two types according to the number of concentric layers, i.e. single-layer tube is single-walled nanotubes, while multi-layer tube structure is called multi-walled nanotubes. The green method synthesis for the preparation of CNTs begins with the smashing of legume seeds kala chana, and then they form complex with cobalt salt. Desiccation of the complex compound forms cobalt salt and seed protein. The complex is then decomposed at 625 °C in muffle furnace for 20 min. Purification of the decomposed sample is done through acid wash treatment and dried in vacuum oven. The confirmations of CNTs are done by nuclear magnetic resonance and Fourier transform infrared, which analyzes the denatured protein, reacted to the metal salt. X-Ray diffraction determines the MWNTs with transmission electron microscope (TEM) reports the network structure of CNTs. thermal gravimetric analysis (TGA)-differential thermal analysis (DTA)-thermogravimetric analysis (DTG) tests the amount of sample under thermal treatment. Vibrating sample magnetometer determines the paramagnetic nature of CNTs. CNTs thus prepared can be used in mechanical fields, in solar cells, in electronics fields, etc. because of their multidisciplinary properties. The synthesized CNTs are eco-friendly in nature, prepared by the legume seed natural precursor.

Advances in ultrasensitive mass spectrometry of organic molecules.

PubMed

Kandiah, Mathivathani; Urban, Pawel L

2013-06-21

Ultrasensitive mass spectrometric analysis of organic molecules is important for various branches of chemistry, and other fields including physics, earth and environmental sciences, archaeology, biomedicine, and materials science. It finds applications--as an enabling tool--in systems biology, biological imaging, clinical analysis, and forensics. Although there are a number of technical obstacles associated with the analysis of samples by mass spectrometry at ultratrace level (for example analyte losses during sample preparation, insufficient sensitivity, ion suppression), several noteworthy developments have been made over the years. They include: sensitive ion sources, loss-free interfaces, ion optics components, efficient mass analyzers and detectors, as well as "smart" sample preparation strategies. Some of the mass spectrometric methods published to date can achieve sensitivity which is by several orders of magnitude higher than that of alternative approaches. Femto- and attomole level limits of detection are nowadays common, while zepto- and yoctomole level limits of detection have also been reported. We envision that the ultrasensitive mass spectrometric assays will soon contribute to new discoveries in bioscience and other areas.

Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

PubMed

Bibi, Aisha; Ju, Huangxian

2016-04-01

A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd.

Evaluation of SDS depletion using an affinity spin column and IMS-MS detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hengel, Shawna M.; Floyd, Erica A.; Baker, Erin Shammel

2012-11-01

While the use of detergents is necessary for a variety of protein isolation preparation protocols, often prior to mass spectral (MS) analysis, they are not compatible with MS analysis due to ion suppression and adduct formation. This manuscript describes optimization of detergent removal, using commercially available SDS depletion spin columns containing an affinity resin, providing for both increased protein recovery and thorough SDS removal. Ion mobility spectrometry coupled with mass spectrometry (IMS-MS) allowed for a concurrent analysis of both analyte and detergent. In the case of both proteins and peptides, higher detergent concentrations than previously reported provided an increase ofmore » sample recovery; however there was a limit as SDS was detected by IMS-MS at higher levels of SDS indicating incomplete detergent depletion. The results also suggest optimal conditions for SDS removal are dependent on the sample concentration. Overall, this study provides a useful guide for proteomic studies where SDS is required for efficient sample preparation.« less

An overview on forensic analysis devoted to analytical chemists.

PubMed

Castillo-Peinado, L S; Luque de Castro, M D

2017-05-15

The present article has as main aim to show analytical chemists interested in forensic analysis the world they will face if decision in favor of being a forensic analytical chemist is adopted. With this purpose, the most outstanding aspects of forensic analysis in dealing with sampling (involving both bodily and no bodily samples), sample preparation, and analytical equipment used in detection, identification and quantitation of key sample components are critically discussed. The role of the great omics in forensic analysis, and the growing role of the youngest of the great omics -metabolomics- are also discussed. The foreseeable role of integrative omics is also outlined. Copyright © 2017 Elsevier B.V. All rights reserved.

The chemical stability and sterility of sodium thiopental after preparation.

PubMed

Haws, J L; Herman, N; Clark, Y; Bjoraker, R; Jones, D

1998-01-01

Manufacturer's instructions recommend discarding unused portions of sodium thiopental 24 h after reconstitution. Heeding this recommendation may result in the disposal of a large proportion of prepared thiopental. Although thiopental is relatively inexpensive, the volume prepared by many anesthesia departments could make this waste significant. To address this possibility, we investigated the chemical stability and sterility of thiopental in pharmacy-prepared, prefilled syringes. Stock solutions of thiopental were mixed and drawn into syringes under sterile conditions by pharmacists or pharmacy assistants. Fifty-six samples were stored under refrigeration (3 degrees C); the remaining 56 samples were stored at room temperature (22 degrees C). Each day for 7 days, eight samples from each group were analyzed by using high-performance liquid chromatography for chemical stability and cultured for microbiological colonization. Differences in thiopental concentration between the room temperature and the refrigerated samples were measured over time by using repeated-measures analysis of variance (P < or = 0.05). Three positive culture samples (S. epidermidis and S. hemolyticus) most likely represent laboratory contamination and not colonization. At 22 degrees C, thiopental remains stable and sterile for 6 days and well beyond 7 days at 3 degrees C. This study examines the shelf life of the anesthetic drug thiopental in pharmacy-filled syringes stored at either room temperature or under refrigeration. The results justify the use of prepared solutions beyond the package insert recommendation of 24 h.

AEROBIC SOIL MICROCOSMS FOR LONG-TERM BIODEGRADATION OF HYDROCARBON VAPORS

EPA Science Inventory

The aims of this research project included the development of laboratory protocols for the preparation of aerobic soil microcosms using aseptic field soil samples, and for the gas chromatographic analysis of hydrocarbon vapor biodegradation based on vapor samples obtained from th...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP-5.20)

EPA Science Inventory

This SOP describes the procedures for homogenizing, extracting and concentrating solid food samples for persistent organic pollutants such as organochlorine compounds, organophosphate compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, substituted phenols, and...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING LIQUID FOOD SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP-5.19)

EPA Science Inventory

This SOP describes the procedures for homogenizing, extracting, and concentrating liquid food samples for neutral persistent organic pollutants such as organochlorine compounds, organophosphate compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and phenols.

Crystal engineering: co-crystals of cinnamic acid derivatives with a pyridyl derivative co-crystallizer.

PubMed

Lorenzo, Daniel A; Forrest, Sebastian J K; Sparkes, Hazel A

2016-02-01

A number of hydrogen-bonded co-crystals, consisting of a cinnamic acid derivative and a pyridyl co-crystallizer, have been synthesized and their properties investigated by X-ray diffraction. Samples were prepared by recrystallization or solvent drop grinding of trans-cinnamic acid (1), 4-methylcinnamic acid (2), 4-methoxy cinnamic acid (3) or 3,4-methoxy cinnamic acid (4), with 4,4-dipyridyl (A), iso-nicotinamide (B) or nicotinamide (C). The X-ray single-crystal structures of seven novel co-crystals, obtained through recrystallization, are examined and the hydrogen-bonding interactions discussed. Consistent hydrogen-bonding motifs were observed for samples prepared when using 4,4-dipyridyl (A) or iso-nicotinamide (B) as the co-crystallizing agent. Powder X-ray diffraction analysis of the samples prepared by solvent drop grinding suggests the formation of ten co-crystals.

3D chemical mapping: application of scanning transmission (soft) X-ray microscopy (STXM) in combination with angle-scan tomography in bio-, geo-, and environmental sciences.

PubMed

Obst, Martin; Schmid, Gregor

2014-01-01

The identification of environmental processes and mechanisms often requires information on the organochemical and inorganic composition of specimens at high spatial resolution. X-ray spectroscopy (XAS) performed in the soft X-ray range (100-2,200 eV) provides chemical speciation information for elements that are of high biogeochemical relevance such as carbon, nitrogen, and oxygen but also includes transition metals such as iron, manganese, or nickel. Synchrotron-based scanning transmission X-ray microscopy (STXM) combines XAS with high resolution mapping on the 20-nm scale. This provides two-dimensional (2D) quantitative information about the distribution of chemical species such as organic macromolecules, metals, or mineral phases within environmental samples. Furthermore, the combination of STXM with angle-scan tomography allows for three-dimensional (3D) spectromicroscopic analysis of bio-, geo-, or environmental samples. For the acquisition of STXM tomography data, the sample is rotated around an axis perpendicular to the X-ray beam. Various sample preparation approaches such as stripes cut from TEM grids or the preparation of wet cells allow for preparing environmentally relevant specimens in a dry or in a fully hydrated state for 2D and 3D STXM measurements. In this chapter we give a short overview about the principles of STXM, its application to environmental sciences, different preparation techniques, and the analysis and 3D reconstruction of STXM tomography data.

Preparation and investigation of dc conductivity and relative permeability of epoxy/Li-Ni-Zn ferrite composites

NASA Astrophysics Data System (ADS)

Darwish, M. A.; Saafan, S. A.; El-Kony, D.; Salahuddin, N. A.

2015-07-01

Ferrite nanoparticles - having the compositions Li(x/2)(Ni0.5Zn0.5)(1-x)Fe(2+x/2)O4 (x=0, 0.2, 0.3) - have been prepared by the co-precipitation method. The prepared powders have been divided into groups and sintered at different temperatures (373 K, 1074 K and 1473 K). X-Ray diffraction analysis (XRD) for all samples has confirmed the formation of the desired ferrites with crystallite sizes within the nanoscale (<100 nm). The dc conductivity, the relative permeability and the magnetization of the ferrite samples have been investigated and according to the results, the sample Li0.15(Ni0.5Zn0.5)0.7 Fe2.15O4 sintered at 1473 K has been chosen to prepare the composites. The particle size of this sample has been recalculated by using JEOL JEM-100SX transmission electron microscope and it has been found about 64.7 nm. Then, a pure epoxy sample and four pristine epoxy resin /Li0.15(Ni0.5Zn0.5)0.7 Fe2.15O4 composites have been prepared using different ferrite contents (20%, 30%, 40%, and 50%) wt.%. These samples have been characterized by Fourier transform infrared (FTIR) spectroscopy and their dc conductivity, relative permeability and magnetization have also been investigated. The obtained results indicate that the investigated composites may be promising candidates for practical applications such as EMI suppressor and high frequency applications.

Chemical composition and physicochemical properties of green banana (Musa acuminata x balbisiana Colla cv. Awak) flour.

PubMed

Haslinda, W H; Cheng, L H; Chong, L C; Noor Aziah, A A

2009-01-01

Flour was prepared from peeled and unpeeled banana Awak ABB. Samples prepared were subjected to analysis for determination of chemical composition, mineral, dietary fibre, starch and total phenolics content, antioxidant activity and pasting properties. In general, flour prepared from unpeeled banana was found to show enhanced nutrition values with higher contents of mineral, dietary fibre and total phenolics. Hence, flour fortified with peel showed relatively higher antioxidant activity. On the other hand, better pasting properties were shown when banana flour was blended with peel. It was found that a relatively lower pasting temperature, peak viscosity, breakdown, final viscosity and setback were evident in a sample blended with peel.

Method development and subsequent survey analysis of biological tissues for platinum, lead, and manganese content.

PubMed Central

Yoakum, A M; Stewart, P L; Sterrett, J E

1975-01-01

An emission spectrochemical method is described for the determination of trace quantities of platinum, lead, and manganese in biological tissues. Total energy burns in an argon-oxygen atmosphere are employed. Sample preparation, conditions of analysis, and preparation of standards are discussed. The precision of the method is consistently better than +/- 15%, and comparative analyses indicate comparable accuracies. Data obtained for experimental rat tissues and for selected autopsy tissues are presented. PMID:1157798

Micro-computed tomography analysis of post space preparation in root canals filled with carrier-based thermoplasticized gutta-percha.

PubMed

Schroeder, A A; Ford, N L; Coil, J M

2017-03-01

To determine whether post space preparation deviated from the root canal preparation in canals filled with Thermafil, GuttaCore or warm vertically compacted gutta-percha. Forty-two extracted human permanent maxillary lateral incisors were decoronated, and their root canals instrumented using a standardized protocol. Samples were divided into three groups and filled with Thermafil (Dentsply Tulsa Dental Specialties, Johnson City, TN, USA), GuttaCore (Dentsply Tulsa Dental Specialties) or warm vertically compacted gutta-percha, before post space preparation was performed with a GT Post drill (Dentsply Tulsa Dental Specialties). Teeth were scanned using micro-computed tomography after root filling and again after post space preparation. Scans were examined for number of samples with post space deviation, linear deviation of post space preparation and minimum root thickness before and after post space preparation. Parametric data were analysed with one-way analysis of variance (anova) or one-tailed paired Student's t-tests, whilst nonparametric data were analysed with Fisher's exact test. Deviation occurred in eight of forty-two teeth (19%), seven of fourteen from the Thermafil group (50%), one of fourteen from the GuttaCore group (7%), and none from the gutta-percha group. Deviation occurred significantly more often in the Thermafil group than in each of the other two groups (P < 0.05). Linear deviation of post space preparation was greater in the Thermafil group than in both of the other groups and was significantly greater than that of the gutta-percha group (P < 0.05). Minimum root thickness before post space preparation was significantly greater than it was after post space preparation for all groups (P < 0.01). The differences between the Thermafil, GuttaCore and gutta-percha groups in the number of samples with post space deviation and in linear deviation of post space preparation were associated with the presence or absence of a carrier as well as the different carrier materials. © 2016 International Endodontic Journal. Published by John Wiley & Sons Ltd.

Development of a Novel Self-Enclosed Sample Preparation Device for DNA/RNA Isolation in Space

NASA Technical Reports Server (NTRS)

Zhang, Ye; Mehta, Satish K.; Pensinger, Stuart J.; Pickering, Karen D.

2011-01-01

Modern biology techniques present potentials for a wide range of molecular, cellular, and biochemistry applications in space, including detection of infectious pathogens and environmental contaminations, monitoring of drug-resistant microbial and dangerous mutations, identification of new phenotypes of microbial and new life species. However, one of the major technological blockades in enabling these technologies in space is a lack of devices for sample preparation in the space environment. To overcome such an obstacle, we constructed a prototype of a DNA/RNA isolation device based on our novel designs documented in the NASA New Technology Reporting System (MSC-24811-1/3-1). This device is self-enclosed and pipette free, purposely designed for use in the absence of gravity. Our design can also be modified easily for preparing samples in space for other applications, such as flowcytometry, immunostaining, cell separation, sample purification and separation according to its size and charges, sample chemical labeling, and sample purification. The prototype of our DNA/RNA isolation device was tested for efficiencies of DNA and RNA isolation from various cell types for PCR analysis. The purity and integrity of purified DNA and RNA were determined as well. Results showed that our developed DNA/RNA isolation device offers similar efficiency and quality in comparison to the samples prepared using the standard protocol in the laboratory.

Gene expression profiling of whole blood: Comparison of target preparation methods for accurate and reproducible microarray analysis

PubMed Central

Vartanian, Kristina; Slottke, Rachel; Johnstone, Timothy; Casale, Amanda; Planck, Stephen R; Choi, Dongseok; Smith, Justine R; Rosenbaum, James T; Harrington, Christina A

2009-01-01

Background Peripheral blood is an accessible and informative source of transcriptomal information for many human disease and pharmacogenomic studies. While there can be significant advantages to analyzing RNA isolated from whole blood, particularly in clinical studies, the preparation of samples for microarray analysis is complicated by the need to minimize artifacts associated with highly abundant globin RNA transcripts. The impact of globin RNA transcripts on expression profiling data can potentially be reduced by using RNA preparation and labeling methods that remove or block globin RNA during the microarray assay. We compared four different methods for preparing microarray hybridization targets from human whole blood collected in PAXGene tubes. Three of the methods utilized the Affymetrix one-cycle cDNA synthesis/in vitro transcription protocol but varied treatment of input RNA as follows: i. no treatment; ii. treatment with GLOBINclear; or iii. treatment with globin PNA oligos. In the fourth method cDNA targets were prepared with the Ovation amplification and labeling system. Results We find that microarray targets generated with labeling methods that reduce globin mRNA levels or minimize the impact of globin transcripts during hybridization detect more transcripts in the microarray assay compared with the standard Affymetrix method. Comparison of microarray results with quantitative PCR analysis of a panel of genes from the NF-kappa B pathway shows good correlation of transcript measurements produced with all four target preparation methods, although method-specific differences in overall correlation were observed. The impact of freezing blood collected in PAXGene tubes on data reproducibility was also examined. Expression profiles show little or no difference when RNA is extracted from either fresh or frozen blood samples. Conclusion RNA preparation and labeling methods designed to reduce the impact of globin mRNA transcripts can significantly improve the sensitivity of the DNA microarray expression profiling assay for whole blood samples. While blockage of globin transcripts during first strand cDNA synthesis with globin PNAs resulted in the best overall performance in this study, we conclude that selection of a protocol for expression profiling studies in blood should depend on several factors, including implementation requirements of the method and study design. RNA isolated from either freshly collected or frozen blood samples stored in PAXGene tubes can be used without altering gene expression profiles. PMID:19123946

Avoiding artefacts during electron microscopy of silver nanomaterials exposed to biological environments

PubMed Central

Goode, Angela E.; Skepper, Jeremy N.; Thorley, Andrew J.; Seiffert, Joanna M.; Chung, K. Fan; Tetley, Teresa D.; Shaffer, Milo S. P.; Ryan, Mary P.

2015-01-01

Electron microscopy has been applied widely to study the interaction of nanomaterials with proteins, cells and tissues at nanometre scale. Biological material is most commonly embedded in thermoset resins to make it compatible with the high vacuum in the electron microscope. Room temperature sample preparation protocols developed over decades provide contrast by staining cell organelles, and aim to preserve the native cell structure. However, the effect of these complex protocols on the nanomaterials in the system is seldom considered. Any artefacts generated during sample preparation may ultimately interfere with the accurate prediction of the stability and reactivity of the nanomaterials. As a case study, we review steps in the room temperature preparation of cells exposed to silver nanomaterials (AgNMs) for transmission electron microscopy imaging and analysis. In particular, embedding and staining protocols, which can alter the physicochemical properties of AgNMs and introduce artefacts thereby leading to a misinterpretation of silver bioreactivity, are scrutinised. Recommendations are given for the application of cryogenic sample preparation protocols, which simultaneously fix both particles and diffusible ions. By being aware of the advantages and limitations of different sample preparation methods, compromises or selection of different correlative techniques can be made to draw more accurate conclusions about the data. PMID:25606708

Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

PubMed

Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

2017-05-12

A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

HPLC-MS/MS analysis of anthocyanins in human plasma and urine using protein precipitation and dilute-and-shoot sample preparation methods, respectively.

PubMed

Liu, Junguo; Song, Jiuxue; Huang, Karen; Michel, Deborah; Fang, Jim

2018-05-01

A high-performance liquid chromatography tandem-mass spectrometry (HPLC-MS/MS) method has been developed to analyze anthocyanins in urine and plasma to further understand their absorption, distribution, metabolism and excretion. The method employed a Synergi RP-Max column (250 × 4.6 mm, 4 μm) and an API 4000 mass spectrometer. A gradient elution system consisted of mobile phase A (water-1% formic acid) and mobile phase B (acetonitrile) with a flow rate of 0.60 mL/min. The gradient was initiated at 5% B, increased to 21% B at 20 min, and then increased to 40% B at 35 min. The analysis of anthocyanins presents a challenge because of the poor stability of anthocyanins during sample preparation, especially during solvent evaporation. In this method, the degradation of anthocyanins was minimized using protein precipitation and dilute-and-shoot and sample preparation methods for plasma and urine, respectively. No interferences were observed from endogenous compounds. The method has been used to analyze anthocyanin concentrations in urine and plasma samples from volunteers administered saskatoon berries. Cyanidin-3-galactoside, cyanidin-3-glucoside, cyanidin-3-arabinoside, cyanidin-3-xyloside and quercetin-3-galactoside, the five major flavonoid components in saskatoon berries, were identified in plasma and urine samples. Copyright © 2017 John Wiley & Sons, Ltd.

Apparatus for preparing a sample for mass spectrometry

DOEpatents

Villa-Aleman, E.

1994-05-10

An apparatus is described for preparing a sample for analysis by a mass spectrometer system. The apparatus has an entry chamber and an ionization chamber separated by a skimmer. A capacitor having two space-apart electrodes followed by one or more ion-imaging lenses is disposed in the ionization chamber. The chamber is evacuated and the capacitor is charged. A valve injects a sample gas in the form of sample pulses into the entry chamber. The pulse is collimated by the skimmer and enters the ionization chamber. When the sample pulse passes through the gap between the electrodes, it discharges the capacitor and is thereby ionized. The ions are focused by the imaging lenses and enter the mass analyzer, where their mass and charge are analyzed. 1 figures.

Laboratory and quality assurance protocols for the analysis of herbicides in ground water from the Management Systems Evaluation Area, Princeton, Minnesota

USGS Publications Warehouse

Larson, S.J.; Capel, P.D.; VanderLoop, A.G.

1996-01-01

Laboratory and quality assurance procedures for the analysis of ground-water samples for herbicides at the Management Systems Evaluation Area near Princeton, Minnesota are described. The target herbicides include atrazine, de-ethylatrazine, de-isopropylatrazine, metribuzin, alachlor, 2,6-diethylaniline, and metolachlor. The analytical techniques used are solid-phase extraction, and analysis by gas chromatography with mass-selective detection. Descriptions of cleaning procedures, preparation of standard solutions, isolation of analytes from water, sample transfer methods, instrumental analysis, and data analysis are included.

Plasma synthesis, Mössbauer spectroscopy and X-ray diffraction studies of nanosized iron oxides

NASA Astrophysics Data System (ADS)

Paneva, Daniela; Zaharieva, Katerina; Grabis, Janis; Mitov, Ivan; Vissokov, Gheorghi

2010-06-01

In this article synthesis and study of iron oxide nanopowders are described. The synthesis of sample 1 and sample 2—iron oxides—was carried out by electric arc plasma cutting of ordinary steel. The sample 3 was prepared by evaporation of Fe2O3/FeO mixture in radio-frequency nitrogen plasma. The characterization of the as prepared iron oxide nanoproducts was achieved by means of Mössbauer spectroscopy and X-ray diffraction analysis. The presence of different phases of iron oxide with a basic phase Fe3 - xO4 (magnetite), additional Fe1 - xO (wüstite) and α or γ-Fe2O3 (hematite or maghemite) with superparamagnetic particles for sample 1 and sample 2 and Fe3 - xO4 (magnetite) for sample 3 is observed.

Rapid Assessment of Contaminants and Interferences in Mass Spectrometry Data Using Skyline

NASA Astrophysics Data System (ADS)

Rardin, Matthew J.

2018-04-01

Proper sample preparation in proteomic workflows is essential to the success of modern mass spectrometry experiments. Complex workflows often require reagents which are incompatible with MS analysis (e.g., detergents) necessitating a variety of sample cleanup procedures. Efforts to understand and mitigate sample contamination are a continual source of disruption with respect to both time and resources. To improve the ability to rapidly assess sample contamination from a diverse array of sources, I developed a molecular library in Skyline for rapid extraction of contaminant precursor signals using MS1 filtering. This contaminant template library is easily managed and can be modified for a diverse array of mass spectrometry sample preparation workflows. Utilization of this template allows rapid assessment of sample integrity and indicates potential sources of contamination. [Figure not available: see fulltext.

Stability of extemporaneously prepared rifaximin oral suspensions.

PubMed

Cober, Mary Petrea; Johnson, Cary E; Lee, Jordan; Currie, Kenne

2010-02-15

The stability of extemporaneously prepared rifaximin oral suspensions was studied. An oral suspension of rifaximin 20 mg/mL was prepared by thoroughly grinding six 200-mg tablets of rifaximin in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of each formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and were stored at room temperature (23-25 degrees C). A 1-mL sample was withdrawn from each of the six bottles with a micropipette immediately after preparation and at 7, 15, 30, and 60 days. After further dilution to an expected concentration of 20 microg/mL with mobile phase, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and pH was tested on each day of analysis. Stability was determined by evaluating the percentage of the initial concentration remaining at each time point and defined as retention of at least 90% of the initial concentration of rifaximin. At least 99% of the initial rifaximin remained throughout the 60-day study period in both preparations. There were no detectable changes in color, odor, taste, or pH and no visible microbial growth in any sample. Extemporaneously prepared suspensions of rifaximin 20 mg/mL in 1:1 mixtures of Ora-Plus with either Ora-Sweet or Ora-Sweet SF were stable for at least 60 days when stored in 2-oz amber plastic bottles at room temperature.

Needle Trap Device as a New Sampling and Preconcentration Approach for Volatile Organic Compounds of Herbal Medicines and its Application to the Analysis of Volatile Components in Viola tianschanica.

PubMed

Qin, Yan; Pang, Yingming; Cheng, Zhihong

2016-11-01

The needle trap device (NTD) technique is a new microextraction method for sampling and preconcentration of volatile organic compounds (VOCs). Previous NTD studies predominantly focused on analysis of environmental volatile compounds in the gaseous and liquid phases. Little work has been done on its potential application in biological samples and no work has been reported on analysis of bioactive compounds in essential oils from herbal medicines. The main purpose of the present study is to develop a NTD sampling method for profiling VOCs in biological samples using herbal medicines as a case study. A combined method of NTD sample preparation and gas chromatography-mass spectrometry was developed for qualitative analysis of VOCs in Viola tianschanica. A 22-gauge stainless steel, triple-bed needle packed with Tenax, Carbopack X and Carboxen 1000 sorbents was used for analysis of VOCs in the herb. Furthermore, different parameters affecting the extraction efficiency and capacity were studied. The peak capacity obtained by NTDs was 104, more efficient than those of the static headspace (46) and hydrodistillation (93). This NTD method shows potential to trap a wide range of VOCs including the lower and higher volatile components, while the static headspace and hydrodistillation only detects lower volatile components, and semi-volatile and higher volatile components, respectively. The developed NTD sample preparation method is a more rapid, simpler, convenient, and sensitive extraction/desorption technique for analysis of VOCs in herbal medicines than the conventional methods such as static headspace and hydrodistillation. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Comparison of analytical methods for profiling N- and O-linked glycans from cultured cell lines

PubMed Central

Togayachi, Akira; Azadi, Parastoo; Ishihara, Mayumi; Geyer, Rudolf; Galuska, Christina; Geyer, Hildegard; Kakehi, Kazuaki; Kinoshita, Mitsuhiro; Karlsson, Niclas G.; Jin, Chunsheng; Kato, Koichi; Yagi, Hirokazu; Kondo, Sachiko; Kawasaki, Nana; Hashii, Noritaka; Kolarich, Daniel; Stavenhagen, Kathrin; Packer, Nicolle H.; Thaysen-Andersen, Morten; Nakano, Miyako; Taniguchi, Naoyuki; Kurimoto, Ayako; Wada, Yoshinao; Tajiri, Michiko; Yang, Pengyuan; Cao, Weiqian; Li, Hong; Rudd, Pauline M.; Narimatsu, Hisashi

2016-01-01

The Human Disease Glycomics/Proteome Initiative (HGPI) is an activity in the Human Proteome Organization (HUPO) supported by leading researchers from international institutes and aims at development of disease-related glycomics/glycoproteomics analysis techniques. Since 2004, the initiative has conducted three pilot studies. The first two were N- and O-glycan analyses of purified transferrin and immunoglobulin-G and assessed the most appropriate analytical approach employed at the time. This paper describes the third study, which was conducted to compare different approaches for quantitation of N- and O-linked glycans attached to proteins in crude biological samples. The preliminary analysis on cell pellets resulted in wildly varied glycan profiles, which was probably the consequence of variations in the pre-processing sample preparation methodologies. However, the reproducibility of the data was not improved dramatically in the subsequent analysis on cell lysate fractions prepared in a specified method by one lab. The study demonstrated the difficulty of carrying out a complete analysis of the glycome in crude samples by any single technology and the importance of rigorous optimization of the course of analysis from preprocessing to data interpretation. It suggests that another collaborative study employing the latest technologies in this rapidly evolving field will help to realize the requirements of carrying out the large-scale analysis of glycoproteins in complex cell samples. PMID:26511985

Determination of drugs and drug-like compounds in different samples with direct analysis in real time mass spectrometry.

PubMed

Chernetsova, Elena S; Morlock, Gertrud E

2011-01-01

Direct analysis in real time (DART), a relatively new ionization source for mass spectrometry, ionizes small-molecule components from different kinds of samples without any sample preparation and chromatographic separation. The current paper reviews the published data available on the determination of drugs and drug-like compounds in different matrices with DART-MS, including identification and quantitation issues. Parameters that affect ionization efficiency and mass spectra composition are also discussed. Copyright © 2011 Wiley Periodicals, Inc.

Characterization Results For The 2013 HTF 3H Evaporator Overhead Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Washington, A. L. II

2013-12-04

This report tabulates the radiochemical analysis of the 3H evaporator overhead sample for {sup 137}Cs, {sup 90}Sr, and {sup 129}I to meet the requirements in the Effluent Treatment Project (ETP) Waste Acceptance Criteria (WAC) (rev. 6). This report identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. All data was found to be within the ETP WAC (rev. 6) specification for the Waste Water Collection Tanks (WWCT).

Characterization Results for the 2014 HTF 3H & 2H Evaporator Overhead Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Washington, A.

2015-05-11

This report tabulates the radiochemical analysis of the 3H and 2H evaporator overhead samples for 137Cs, 90Sr, and 129I to meet the requirements in the Effluent Treatment Project (ETP) Waste Acceptance Criteria (WAC) (rev. 6). This report identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. All data was found to be within the ETP WAC (rev. 6) specification for the Waste Water Collection Tanks (WWCT).

A combined method for correlative 3D imaging of biological samples from macro to nano scale

NASA Astrophysics Data System (ADS)

Kellner, Manuela; Heidrich, Marko; Lorbeer, Raoul-Amadeus; Antonopoulos, Georgios C.; Knudsen, Lars; Wrede, Christoph; Izykowski, Nicole; Grothausmann, Roman; Jonigk, Danny; Ochs, Matthias; Ripken, Tammo; Kühnel, Mark P.; Meyer, Heiko

2016-10-01

Correlative analysis requires examination of a specimen from macro to nano scale as well as applicability of analytical methods ranging from morphological to molecular. Accomplishing this with one and the same sample is laborious at best, due to deformation and biodegradation during measurements or intermediary preparation steps. Furthermore, data alignment using differing imaging techniques turns out to be a complex task, which considerably complicates the interconnection of results. We present correlative imaging of the accessory rat lung lobe by combining a modified Scanning Laser Optical Tomography (SLOT) setup with a specially developed sample preparation method (CRISTAL). CRISTAL is a resin-based embedding method that optically clears the specimen while allowing sectioning and preventing degradation. We applied and correlated SLOT with Multi Photon Microscopy, histological and immunofluorescence analysis as well as Transmission Electron Microscopy, all in the same sample. Thus, combining CRISTAL with SLOT enables the correlative utilization of a vast variety of imaging techniques.

Preparation, Structural Characterization and Magnetic Properties of La-SUBSTITUTED co Ferrites via a Modified Citrate Precursor Route

NASA Astrophysics Data System (ADS)

Ai, Lunhong; Jiang, Jing

CoLaxFe2-xO4 (x = 0.00, 0.05 and 0.1) nanoparticles were prepared simply by a modified citrate precursor route. Effects of La-substituting level on the their magnetic properties were investigated on the basis of the structural analysis. The thermal evolution of the precursor, as well as the microstructure of as-prepared products were studied by means of a thermogravimetric analyzer (TGA), X-ray diffractometer (XRD) and Fourier transform infrared (FTIR) spectrometer. The magnetic properties of the as-prepared samples were measured using a vibrating sample magnetometer (VSM). It was found that the magnetic properties were dependent on many factors such as La-substituting level, particle size and microstructure. The observed saturation magnetization decreased with increasing La content, whereas coercivity exhibited reverse behavior.

Effect of Zn doping on the microwave absorption of BFO multiferroic materials

NASA Astrophysics Data System (ADS)

Bi, S.; Li, J.; Mei, B.; Su, X. J.; Ying, C. Z.; Li, P. H.

2018-01-01

The microwave absorbing materials were firstly used in the Second World War. And the BiFeO3 (BFO) based microwave absorbers have been widely applied into the microwave absorbing area due to its possession of excellent electromagnetic properties. Various methods have been conducted to improve the microwave absorption performance of the BFO based materials. In the work, the sol-gel method were used to prepare the BFO, and the Zn were doped into the BFO to prepare the Bi1-xZnxFeO3 nanoparticles. The X-ray diffraction, scanning electron microscope, and vector network analysis (VNA) were conducted to characterize the microstructure and electromagnetic properties of the as-prepared samples. The results indicate that the Bi1-xZnxFeO3 nanoparticles were successfully gained and the as-prepared samples possess excellent microwave absorption properties.

Stability of extemporaneously prepared glycopyrrolate oral suspensions.

PubMed

Cober, Mary Petrea; Johnson, Cary E; Sudekum, David; Penprase, Kimberly

2011-05-01

The stability of extemporaneously prepared glycopyrrolate 0.5-mg/mL suspensions was evaluated. An oral suspension of glycopyrrolate 0.5 mg/mL was prepared by thoroughly grinding 30 1-mg tablets of glycopyrrolate in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and 7, 15, 30, 60, and 90 days afterward. After further dilution to an expected concentration of 50 μg/mL with sample diluent, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH on each day of analysis. Taste evaluations were performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 95% of the initial glycopyrrolate remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. Extemporaneously compounded suspensions of glycopyrrolate 0.5 mg/mL in a 1:1 mixture of Ora-Plus/Ora-Sweet or Ora-Plus/Ora-Sweet SF were stable for at least 90 days when stored in amber plastic bottles at room temperature.

Specimen preparation for NanoSIMS analysis of biological materials

NASA Astrophysics Data System (ADS)

Grovenor, C. R. M.; Smart, K. E.; Kilburn, M. R.; Shore, B.; Dilworth, J. R.; Martin, B.; Hawes, C.; Rickaby, R. E. M.

2006-07-01

In order to achieve reliable and reproducible analysis of biological materials by SIMS, it is critical both that the chosen specimen preparation method does not modify substantially the in vivo chemistry that is the focus of the study and that any chemical information obtained can be calibrated accurately by selection of appropriate standards. In Oxford, we have been working with our new Cameca NanoSIMS50 on two very distinct classes of biological materials; the first where the sample preparation problems are relatively undemanding - human hair - but calibration for trace metal analysis is a critical issue and, the second, marine coccoliths and hyperaccumulator plants where reliable specimen preparation by rapid freezing and controlled drying to preserve the distribution of diffusible species is the first and most demanding requirement, but worthwhile experiments on tracking key elements can still be undertaken even when it is clear that some redistribution of the most diffusible ions has occurred.

Overcoming Matrix Effects in a Complex Sample: Analysis of Multiple Elements in Multivitamins by Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Arnold, Randy J.; Arndt, Brett; Blaser, Emilia; Blosser, Chris; Caulton, Dana; Chung, Won Sog; Fiorenza, Garrett; Heath, Wyatt; Jacobs, Alex; Kahng, Eunice; Koh, Eun; Le, Thao; Mandla, Kyle; McCory, Chelsey; Newman, Laura; Pithadia, Amit; Reckelhoff, Anna; Rheinhardt, Joseph; Skljarevski, Sonja; Stuart, Jordyn; Taylor, Cassie; Thomas, Scott; Tse, Kyle; Wall, Rachel; Warkentien, Chad

2011-01-01

A multivitamin tablet and liquid are analyzed for the elements calcium, magnesium, iron, zinc, copper, and manganese using atomic absorption spectrometry. Linear calibration and standard addition are used for all elements except calcium, allowing for an estimate of the matrix effects encountered for this complex sample. Sample preparation using…

A Simple and Reproducible Method to Prepare Membrane Samples from Freshly Isolated Rat Brain Microvessels.

PubMed

Brzica, Hrvoje; Abdullahi, Wazir; Reilly, Bianca G; Ronaldson, Patrick T

2018-05-07

The blood-brain barrier (BBB) is a dynamic barrier tissue that responds to various pathophysiological and pharmacological stimuli. Such changes resulting from these stimuli can greatly modulate drug delivery to the brain and, by extension, cause considerable challenges in the treatment of central nervous system (CNS) diseases. Many BBB changes that affect pharmacotherapy, involve proteins that are localized and expressed at the level of endothelial cells. Indeed, such knowledge on BBB physiology in health and disease has sparked considerable interest in the study of these membrane proteins. From a basic science research standpoint, this implies a requirement for a simple but robust and reproducible method for isolation of microvessels from brain tissue harvested from experimental animals. In order to prepare membrane samples from freshly isolated microvessels, it is essential that sample preparations be enriched in endothelial cells but limited in the presence of other cell types of the neurovascular unit (i.e., astrocytes, microglia, neurons, pericytes). An added benefit is the ability to prepare samples from individual animals in order to capture the true variability of protein expression in an experimental population. In this manuscript, details regarding a method that is utilized for isolation of rat brain microvessels and preparation of membrane samples are provided. Microvessel enrichment, from samples derived, is achieved by using four centrifugation steps where dextran is included in the sample buffer. This protocol can easily be adapted by other laboratories for their own specific applications. Samples generated from this protocol have been shown to yield robust experimental data from protein analysis experiments that can greatly aid the understanding of BBB responses to physiological, pathophysiological, and pharmacological stimuli.

Effect of annealing temperature on titania nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manikandan, K., E-mail: sanjaymani367@gmail.com; Arumugam, S., E-mail: sanjaymani367@gmail.com; Chandrasekaran, G.

2014-04-24

Titania polycrystalline samples are prepared by using sol-gel route hydrolyzing a alkoxide titanium precursor under acidic conditions. The as prepared samples are treated with different calcination temperatures. The anatase phase of titania forms when treated below 600°C, above that temperature the anatase phase tends to transform into the rutile phase of titania. The experimental determination of average grain size, phase formation, lattice parameters and the crystal structures of titania samples at different calcinations is done using X-ray diffraction (XRD). Fourier Transform Infra-red Spectroscopy (FTIR), UV-vis-NIR spectroscopy and Scanning Electron Microscopy (SEM) and Energy Dispersive Analysis X-ray are used to characterizemore » the samples to bring impact on the respective properties.« less

Capacitive deionization on-chip as a method for microfluidic sample preparation.

PubMed

Roelofs, Susan H; Kim, Bumjoo; Eijkel, Jan C T; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu

2015-03-21

Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before analysis to improve the signal-to-noise ratio. Capacitive deionization is an electrostatic desalination (CDI) technique which uses two porous electrodes facing each other to remove ions from a solution. Upon the application of a potential of 0.5 V ions migrate to the electrodes and are stored in the electrical double layer. In this article we demonstrate CDI on a chip, and desalinate a solution by the removal of 23% of Na(+) and Cl(-) ions, while the concentration of a larger molecule (FITC-dextran) remains unchanged. For the first time impedance spectroscopy is introduced to monitor the salt concentration in situ in real-time in between the two desalination electrodes.

X-ray fluorescence analysis of K, Al and trace elements in chloroaluminate melts

NASA Astrophysics Data System (ADS)

Shibitko, A. O.; Abramov, A. V.; Denisov, E. I.; Lisienko, D. G.; Rebrin, O. I.; Bunkov, G. M.; Rychkov, V. N.

2017-09-01

Energy dispersive x-ray fluorescence spectrometry was applied to quantitative determination of K, Al, Cr, Fe and Ni in chloroaluminate melts. To implement the external standard calibration method, an unconventional way of samples preparation was suggested. A mixture of metal chlorides was melted in a quartz cell at 350-450 °C under a slightly excessive pressure of purified argon (99.999 %). The composition of the calibration samples (CSs) prepared was controlled by means of the inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimal conditions for analytical lines excitation were determined, the analytes calibration curves were obtained. There was some influence of matrix effects in synthesized samples on the analytical signal of some elements. The CSs are to be stored in inert gas atmosphere. The precision, accuracy, and reproducibility factors of the quantitative chemical analysis were computed.

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992-2006

USGS Publications Warehouse

Martin, Jeffrey D.

2009-01-01

This report provides a water-quality data set of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through August 2006 at stream-water sites of the U.S. Geological Survey National Water-Quality Assessment Program and the National Stream Quality Accounting Network Program were compiled, reviewed, selected, and prepared for trend analysis as described in this report. Samples analyzed at the U.S. Geological Survey National Water Quality Laboratory by a gas chromatography/mass spectrometry analytical method were the most extensive in time and space and were selected for national trend analysis. The selection criteria described in the report produced a trend data set of 16,869 pesticide samples at 201 stream and river sites.

Immune Blood Sample Draw

NASA Image and Video Library

2012-04-26

ISS030-E-257690 (26 April 2012) --- European Space Agency astronaut Andre Kuipers, Expedition 30 flight engineer, prepares for IMMUNE venous blood sample draws in the Columbus laboratory of the International Space Station. Following the blood draws, the samples were temporarily stowed in the Minus Eighty Laboratory Freezer for ISS 1 (MELFI-1) and later packed together with saliva samples on the Soyuz TMA-22 for return to Earth for analysis.

Analysis of the aflatoxin AFB1 from corn by direct analysis in real time - mass spectrometry (DART-MS)

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to a high resolution mass spectrometer (MS) was used for screening of aflatoxins from a variety of surfaces and the rapid quantitative analysis of aflatoxins extracted from corn. Sample preparation procedure and instrument parameter settings wer...

Comet composition and density analyzer

NASA Technical Reports Server (NTRS)

Clark, B. C.

1982-01-01

Distinctions between cometary material and other extraterrestrial materials (meteorite suites and stratospherically-captured cosmic dust) are addressed. The technique of X-ray fluorescence (XRF) for analysis of elemental composition is involved. Concomitant with these investigations, the problem of collecting representative samples of comet dust (for rendezvous missions) was solved, and several related techniques such as mineralogic analysis (X-ray diffraction), direct analysis of the nucleus without docking (electron macroprobe), dust flux rate measurement, and test sample preparation were evaluated. An explicit experiment concept based upon X-ray fluorescence analysis of biased and unbiased sample collections was scoped and proposed for a future rendezvous mission with a short-period comet.

Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

DIFFERENCES IN CULTURAL YIELD OF MYCOBACTERIUM TUBERCULOSIS ON MEDIA PREPARED USING COMMERCIAL AND HOUSEHOLD EGGS.

PubMed

Noori, Muhammad Yahya; AJi, Zaheer; Khan, Ghazala; Sharafat, Shaheen; Masroor, Muhammad

2015-01-01

Mycobacterial culture is considered as the gold standard for TB diagnosis. It is performed on egg-based media using commercially available eggs to grow Mycobacteria from clinical samples. These eggs are known to contain high concentration of antibiotics, including fluoroquinolones, given to chicken to prevent early mortality. This study was performed to compare Mycobacterial growth on media prepared from commercial and antibiotic free household eggs. Sputum samples from negative (No bacilli in 100 oil immersion field), scanty (1-9 AFB in 100 fields), 1+ (10-99 bacilli per field), 2+ (1-10 bacilli per field) and 3+ (>10 bacilli per field) were inoculated dually on Ogawa medium prepared from commercial and household eggs. Tubes were inspected every fourth day for the appearance of colonies till 60 days. Data tabulations and statistical analysis (F test for variation and unpaired Student's t test) were performed on Microsoft Excel. One microscopically negative sample showed growth on media prepared from household eggs, while all were negative on that prepared from commercial eggs. There were significant differences in time to culture positivity for samples graded 1+ (p = 0.02), 2+ (p = 0.002) and 3+ (p = 0.0003). Commercial eggs containing antibiotics can be a source of false negativity in cultures especially in microscopically negative samples. This can be of special concern in HIV patients who have high smear negativity. It is therefore important to either develop provision of antibiotic free eggs for media preparation or to develop and validate other laboratory investigations for smear negative TB patients.

Segmental hair analysis for differentiation of tilidine intake from external contamination using LC-ESI-MS/MS and MALDI-MS/MS imaging.

PubMed

Poetzsch, Michael; Baumgartner, Markus R; Steuer, Andrea E; Kraemer, Thomas

2015-02-01

Segmental hair analysis has been used for monitoring changes of consumption habit of drugs. Contamination from the environment or sweat might cause interpretative problems. For this reason, hair analysis results were compared in hair samples taken 24 h and 30 days after a single tilidine dose. The 24-h hair samples already showed high concentrations of tilidine and nortilidine. Analysis of wash water from sample preparation confirmed external contamination by sweat as reason. The 30-day hair samples were still positive for tilidine in all segments. Negative wash-water analysis proved incorporation from sweat into the hair matrix. Interpretation of a forensic case was requested where two children had been administered tilidine by their nanny and tilidine/nortilidine had been detected in all hair segments, possibly indicating multiple applications. Taking into consideration the results of the present study and of MALDI-MS imaging, a single application as cause for analytical results could no longer be excluded. Interpretation of consumption behaviour of tilidine based on segmental hair analysis has to be done with caution, even after typical wash procedures during sample preparation. External sweat contamination followed by incorporation into the hair matrix can mimic chronic intake. For assessment of external contamination, hair samples should not only be collected several weeks but also one to a few days after intake. MALDI-MS imaging of single hair can be a complementary tool for interpretation. Limitations for interpretation of segmental hair analysis shown here might also be applicable to drugs with comparable physicochemical and pharmacokinetic properties. Copyright © 2014 John Wiley & Sons, Ltd.

Aerosol preparation of intact lipoproteins

DOEpatents

Benner, W Henry [Danville, CA; Krauss, Ronald M [Berkeley, CA; Blanche, Patricia J [Berkeley, CA

2012-01-17

A medical diagnostic method and instrumentation system for analyzing noncovalently bonded agglomerated biological particles is described. The method and system comprises: a method of preparation for the biological particles; an electrospray generator; an alpha particle radiation source; a differential mobility analyzer; a particle counter; and data acquisition and analysis means. The medical device is useful for the assessment of human diseases, such as cardiac disease risk and hyperlipidemia, by rapid quantitative analysis of lipoprotein fraction densities. Initially, purification procedures are described to reduce an initial blood sample to an analytical input to the instrument. The measured sizes from the analytical sample are correlated with densities, resulting in a spectrum of lipoprotein densities. The lipoprotein density distribution can then be used to characterize cardiac and other lipid-related health risks.

Detection of caffeine in tea, instant coffee, green tea beverage, and soft drink by direct analysis in real time (DART) source coupled to single-quadrupole mass spectrometry.

PubMed

Wang, Lei; Zhao, Pengyue; Zhang, Fengzu; Bai, Aijuan; Pan, Canping

2013-01-01

Ambient ionization direct analysis in real time (DART) coupled to single-quadrupole MS (DART-MS) was evaluated for rapid detection of caffeine in commercial samples without chromatographic separation or sample preparation. Four commercial samples were examined: tea, instant coffee, green tea beverage, and soft drink. The response-related parameters were optimized for the DART temperature and MS fragmentor. Under optimal conditions, the molecular ion (M+H)+ was the major ion for identification of caffeine. The results showed that DART-MS is a promising tool for the quick analysis of important marker molecules in commercial samples. Furthermore, this system has demonstrated significant potential for high sample throughput and real-time analysis.

Imaging of polysaccharides in the tomato cell wall with Raman microspectroscopy

PubMed Central

2014-01-01

Background The primary cell wall of fruits and vegetables is a structure mainly composed of polysaccharides (pectins, hemicelluloses, cellulose). Polysaccharides are assembled into a network and linked together. It is thought that the percentage of components and of plant cell wall has an important influence on mechanical properties of fruits and vegetables. Results In this study the Raman microspectroscopy technique was introduced to the visualization of the distribution of polysaccharides in cell wall of fruit. The methodology of the sample preparation, the measurement using Raman microscope and multivariate image analysis are discussed. Single band imaging (for preliminary analysis) and multivariate image analysis methods (principal component analysis and multivariate curve resolution) were used for the identification and localization of the components in the primary cell wall. Conclusions Raman microspectroscopy supported by multivariate image analysis methods is useful in distinguishing cellulose and pectins in the cell wall in tomatoes. It presents how the localization of biopolymers was possible with minimally prepared samples. PMID:24917885

"Soft"or "hard" ionisation? Investigation of metastable gas temperature effect on direct analysis in real-time analysis of Voriconazole.

PubMed

Lapthorn, Cris; Pullen, Frank

2009-01-01

The performance of the direct analysis in real-time (DART) technique was evaluated across a range of metastable gas temperatures for a pharmaceutical compound, Voriconazole, in order to investigate the effect of metastable gas temperature on molecular ion intensity and fragmentation. The DART source has been used to analyse a range of analytes and from a range of matrices including drugs in solid tablet form and preparations, active ingredients in ointment, naturally occurring plant alkaloids, flavours and fragrances, from thin layer chromatography (TLC) plates, melting point tubes and biological matrices including hair, urine and blood. The advantages of this technique include rapid analysis time (as little as 5 s), a reduction in sample preparation requirements, elimination of mobile phase requirement and analysis of samples not typically amenable to atmospheric pressure ionisation (API) techniques. This technology has therefore been proposed as an everyday tool for identification of components in crude organic reaction mixtures.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS.

PubMed

Lou, Xianwen; de Waal, Bas F M; Milroy, Lech-Gustav; van Dongen, Joost L J

2015-05-01

In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte suppression effect (ASE). In our method, analytes are deposited on top of the surface of matrix preloaded on the MALDI plate. To prevent embedding of analyte into the matrix crystals, the sample solution were prepared without matrix and efforts were taken not to re-dissolve the preloaded matrix. The results with model mixtures of peptides, synthetic polymers and lipids show that detection of analyte ions, which were completely suppressed using the conventional dried-droplet method, could be effectively recovered by using our method. Our findings suggest that the incorporation of analytes in the matrix crystals has an important contributory effect on ASE. By reducing ASE, our method should be useful for the direct MALDI MS analysis of multicomponent mixtures. Copyright © 2015 John Wiley & Sons, Ltd.

Soil an-d nutrient loss following site preparation burning

Treesearch

E.A. Carter; J.P. Field; K.W. Farrish

2000-01-01

Sediment loss and nutrient cpncentrations in runoff were evaluated to determine the effects of site preparation burning on a recently harvested loblolly pine (Pinur taeda L.) site in east Texas. Sediment and nutrient losses prior to treatment were approximately the same from control plots and pretreatment burn plots. Nutrient analysis of runoff samples indicated that...

How natural are 'natural herbal remedies'? A Saudi perspective.

PubMed

Bogusz, Maciej J; al Tufail, Mohammed; Hassan, Huda

2002-01-01

There is a rapidly growing trend in the consumption of herbal remedies in industrialised and developing countries. Users of herbal remedies are at risk of toxicity and adverse interactions of herbal preparations due to their frequent contamination with metals and adulteration with synthetic drugs. The purpose of this study was to assess the quality of herbal remedies present on the market in Saudi Arabia in recent years. 247 herbal remedies and related preparations were examined from 2000-2001 at the Toxicology Laboratory, King Faisal Specialist Hospital and Research Centre, Riyadh, Saudi Arabia. Herbal powder samples were the most common sample type examined (n = 80), followed by complete, packed preparations (n = 59), single undescribed capsules or pills (n = 46), loose plant leaves or seeds (n = 28), creams (n = 18) and liquid or jelly samples (n = 16). All samples were subjected to toxicological screening for organic substances using gas chromatographic-mass spectrometric analysis, screening for heavy metals (arsenic, mercury, and lead) using inductive coupled plasma-mass spectrometry and microbiological examination. The preparations analysed were used to treat the following indications: leukaemia and other forms of cancer (n = 22); obesity (n = 18); diabetes mellitus (n = 14); rheumatic disorders (n = 14); skin pigmentation problems (n = 11); or to enhance male sexual activity (n = 9). In 123 cases, the indication of use was not known. 39 samples contained high concentrations of heavy metals. This was particularly striking in remedies used to treat leukaemia (arsenic content of 522-161,600 ppm) and in creams for whitening skin (mercury content of 5,700-126,000 ppm). Eight preparations contained synthetic drugs (e.g. benzodiazepines and tricyclic antidepressants in sedative preparations, cyproheptadine in a remedy to gain bodyweight, ibuprofen and dipyrone in herbal capsules used to treat rheumatism). 18 samples were contaminated with micro-organisms. 14 samples contained toxic substances of natural origin. Of the 247 examined preparations, 77 (i.e. over 30%) were disqualified due to high heavy metals content, bacterial contamination or presence of toxic organic substances. The study shows an urgent need to control the production, importing and selling of herbal preparations.

Synthesis, characterization and antibacterial activity of hybrid chitosan-cerium oxide nanoparticles: As a bionanomaterials.

PubMed

Senthilkumar, R P; Bhuvaneshwari, V; Ranjithkumar, R; Sathiyavimal, S; Malayaman, V; Chandarshekar, B

2017-11-01

The hybrid chitosan cerium oxide nanoparticles were prepared for the first time by green chemistry approach using plant leaf extract. The intense peak observed around 292nm in the UV-vis spectrum indicate the formation of cerium oxide nanoparticles. The XRD pattern revealed that the hybrid chitosan-cerium oxide nanoparticles have a polycrystalline structure with cubic fluorite phase. The FTIR spectrum of prepared samples showed the formation of Ce-O bonds and chitosan main chains COC and CO. The FESEM image of hybrid chitosan cerium oxide nanoparticles revealed that the particles are spherical in shape with grains size varying from 23.12nm to 89.91nm. EDAX analysis confirmed the presence of Ce, O, C and N elements in the prepared sample. TEM images showed that the prepared hybrid chitosan-cerium oxide nanoparticles are predominantly uniform in size and most of the particles are spherical in shape with less agglomeration and the particles size varies from 3.61nm to 24.40nm. The prepared chitosan cerium oxide nanoparticles of 50μL concentration showed good antibacterial properties against test pathogens, which was confirmed by the FESEM analysis. The prepared small particle size facilitate that these hybrid ChiCO 2 NPs could effectively be used in biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

A liquid chromatography/tandem mass spectrometry assay for the analysis of atomoxetine in human plasma and in vitro cellular samples

PubMed Central

Appel, David I.; Brinda, Bryan; Markowitz, John S.; Newcorn, Jeffrey H.; Zhu, Hao-Jie

2012-01-01

A simple, rapid and sensitive method for quantification of atomoxetine by liquid chromatography- tandem mass spectrometry (LC-MS/MS) was developed. This assay represents the first LC-MS/MS quantification method for atomoxetine utilizing electrospray ionization. Deuterated atomoxetine (d3-atomoxetine) was adopted as the internal standard. Direct protein precipitation was utilized for sample preparation. This method was validated for both human plasma and in vitro cellular samples. The lower limit of quantification was 3 ng/ml and 10 nM for human plasma and cellular samples, respectively. The calibration curves were linear within the ranges of 3 ng/ml to 900 ng/ml and 10 nM to 10 μM for human plasma and cellular samples, respectively (r2 > 0.999). The intra- and inter-day assay accuracy and precision were evaluated using quality control samples at 3 different concentrations in both human plasma and cellular lysate. Sample run stability, assay selectivity, matrix effect, and recovery were also successfully demonstrated. The present assay is superior to previously published LC-MS and LC-MS/MS methods in terms of sensitivity or the simplicity of sample preparation. This assay is applicable to the analysis of atomoxetine in both human plasma and in vitro cellular samples. PMID:22275222

Environmental contamination, product contamination and workers exposure using a robotic system for antineoplastic drug preparation.

PubMed

Sessink, Paul J M; Leclercq, Gisèle M; Wouters, Dominique-Marie; Halbardier, Loïc; Hammad, Chaïma; Kassoul, Nassima

2015-04-01

Environmental contamination, product contamination and technicians exposure were measured following preparation of iv bags with cyclophosphamide using the robotic system CytoCare. Wipe samples were taken inside CytoCare, in the clean room environment, from vials, and prepared iv bags including ports and analysed for contamination with cyclophosphamide. Contamination with cyclophosphamide was also measured in environmental air and on the technicians hands and gloves used for handling the drugs. Exposure of the technicians to cyclophosphamide was measured by analysis of cyclophosphamide in urine. Contamination with cyclophosphamide was mainly observed inside CytoCare, before preparation, after preparation and after daily routine cleaning. Contamination outside CytoCare was incidentally found. All vials with reconstituted cyclophosphamide entering CytoCare were contaminated on the outside but vials with powdered cyclophosphamide were not contaminated on the outside. Contaminated bags entering CytoCare were also contaminated after preparation but non-contaminated bags were not contaminated after preparation. Cyclophosphamide was detected on the ports of all prepared bags. Almost all outer pairs of gloves used for preparation and daily routine cleaning were contaminated with cyclophosphamide. Cyclophosphamide was not found on the inner pairs of gloves and on the hands of the technicians. Cyclophosphamide was not detected in the stationary and personal air samples and in the urine samples of the technicians. CytoCare enables the preparation of cyclophosphamide with low levels of environmental contamination and product contamination and no measurable exposure of the technicians. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

Application of PLE for the determination of essential oil components from Thymus vulgaris L.

PubMed

Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

2008-08-15

Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for In-Situ Mars Surface Sample Analysis

NASA Technical Reports Server (NTRS)

Edmunson, J.; Gaskin, J. A.; Jerman, G. A.; Harvey, R. P.; Doloboff, I. J.; Neidholdt, E. L.

2016-01-01

The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Sciences (ROSES), will build upon previous miniaturized SEM designs and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. This project is a collaboration between NASA Marshall Space Flight Center (MSFC), the Jet Propulsion Laboratory (JPL), electron gun and optics manufacturer Applied Physics Technologies, and small vacuum system manufacturer Creare. Dr. Ralph Harvery and environmental SEM (ESEM) inventor Dr. Gerry Danilatos serve as advisors to the team. Variable pressure SEMs allow for fine (nm-scale) resolution imaging and micron-scale chemical study of materials without sample preparation (e.g., carbon or gold coating). Charging of a sample is reduced or eliminated by the gas surrounding the sample. It is this property of ESEMs that make them ideal for locations where sample preparation is not yet feasible, such as the surface of Mars. In addition, the lack of sample preparation needed here will simplify the sample acquisition process and allow caching of the samples for future complementary payload use.

3D imaging of cells and tissues by focused ion beam/scanning electron microscopy (FIB/SEM).

PubMed

Drobne, Damjana

2013-01-01

Integration of a scanning electron microscope (SEM) and focused ion beam (FIB) technology into a single FIB/SEM system permits use of the FIB as a nano-scalpel to reveal site-specific subsurface microstructures which can be examined in great detail by SEM. The FIB/SEM technology is widely used in the semiconductor industry and material sciences, and recently its use in the life sciences has been initiated. Samples for FIB/SEM investigation can be either embedded in a plastic matrix, the traditional means of preparation of transmission electron microscopy (TEM) specimens, or simply dried as in samples prepared for SEM imaging. Currently, FIB/SEM is used in the life sciences for (a) preparation by the lift-out technique of lamella for TEM analysis, (b) tomography of samples embedded in a matrix, and (c) in situ site-specific FIB milling and SEM imaging using a wide range of magnifications. Site-specific milling and imaging has attracted wide interest as a technique in structural research of single eukaryotic and prokaryotic cells, small animals, and different animal tissue, but it still remains to be explored more thoroughly. In the past, preparation of samples for site-specific milling and imaging by FIB/SEM has typically adopted the embedding techniques used for TEM samples, and which have been very well described in the literature. Sample preparation protocols for the use of dried samples in FIB/SEM have been less well investigated. The aim of this chapter is to encourage application of FIB/SEM on dried biological samples. A detailed description of conventional dried sample preparation and FIB/SEM investigation of dried biological samples is presented. The important steps are described and illustrated, and direct comparison between embedded and dried samples of same tissues is provided. The ability to discover links between gross morphology of the tissue or organ, surface characteristics of any selected region, and intracellular structural details on the nanometer scale is an appealing application of electron microscopy in the life sciences and merits further exploration.

Structural elucidation and magnetic behavior evaluation of Cu-Cr doped BaCo-X hexagonal ferrites

NASA Astrophysics Data System (ADS)

Azhar Khan, Muhammad; Hussain, Farhat; Rashid, Muhammad; Mahmood, Asif; Ramay, Shahid M.; Majeed, Abdul

2018-04-01

Ba2-xCuxCo2CryFe28-yO46 (x = 0.0, 0.1, 0.2, 0.3, 0.4, y = 0.0, 0.2, 0.4, 0.6, 0.8) X-type hexagonal ferrites were synthesized via micro-emulsion route. The techniques which were applied to characterize the prepared samples are as follows: X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Dielectric measurements and vibrating sample magnetometer (VSM). The structural parameters i.e. lattice constant (a, c), cell volume (V), X-ray density, bulk density and crystallite size of all the prepared samples were obtained using XRD analysis. The lattice parameters 'a' and 'c' increase from 5.875 Å to 5.934 Å and 83.367 Å to 83.990 Å respectively. The crystallite size of investigated samples lies in the range of 28-32 nm. The magnetic properties of all samples have been calculated by vibrating sample magnetometer (VSM) analysis. The increase in coercivity (Hc) was observed with the increase of doping contents. It was observed that the coercivity (Hc) of all prepared samples is inversely related to the crystalline size which reflects that all materials are super-paramagnetic. The dielectric parameters i.e. dielectric constant, dielectric loss, tangent loss etc were obtained in the frequency range of 1 MHz-3 GHz and followed the Maxwell-Wagner's model. The significant variation the dielectric parameters are observed with increasing frequency. The maximum Q value is obtained at ∼2 GHz due to which these materials are used for high frequency multilayer chip inductors.

Bio-template-assisted synthesis of hierarchically hollow SiO2 microtubes and their enhanced formaldehyde adsorption performance

NASA Astrophysics Data System (ADS)

Le, Yao; Guo, Daipeng; Cheng, Bei; Yu, Jiaguo

2013-06-01

The indoor air quality is crucial for human health, taking into account that people often spend more than 80% of their time in houses, offices and cars. Formaldehyde (HCHO) is a major pollutant and long-term exposure to HCHO may cause health problems such as nasal tumors and skin irritation. In this work, for the first time, hierarchically hollow silica microtubes (HHSM) were synthesized by a simple sol-gel and calcination method using cetyltrimethyl ammonium bromide (CTAB) and bio-template poplar catkin (PC) as co-templates and the PC/SiO2 weight ratio R was varied from 0, 0.1, 0.3 and 1. The prepared samples were further modified with tetraethylenepentamine (TEPA) and characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), differential thermal analysis (DTA), thermal gravimetric analysis (TGA), and N2 physisorption techniques. This was followed by formaldehyde adsorption tests at ambient temperature. The results showed that all the prepared HHSM samples contained small mesopores with peak pore size at ca. 2.5 nm and large several tens of nanometer-sized pores on the tube wall. The R exhibited an obvious influence on specific surface areas and the sample prepared at R = 0.3 exhibited highest specific surface area (896 m2/g). All the TEPA-modified samples exhibited enhanced formaldehyde adsorption performance. The maximum HCHO adsorption capacity (20.65 mg/g adsorbent) was achieved on the sample prepared at R = 0.3 and modified by 50 wt.% TEPA. The present study will provide new insight for the utilization of bio-template used for the fabrication of inorganic hollow tubes with high HCHO adsorption performance for indoor air purification.

SOURCES OF VARIABILITY IN COLLECTION AND PREPARATION OF PAINT AND LEAD-COATING SAMPLES

EPA Science Inventory

Chronic exposure of children to lead can result in permanent physiologic impairment. Since surfaces coated with lead-containing paints and varnishes are potential sources of exposure, it is extremely important that reliable methods for sampling and analysis be available. The so...

Time- and cost-saving apparatus for analytical sample filtration

Treesearch

William R. Kenealy; Joseph C. Destree

2005-01-01

Simple and cost-effective protocols were developed for removing particulates from samples prior to analysis by high performance liquid chromatography and gas chromatography. A filter and vial holder were developed for use with a 96-well filtration plate. The device saves preparation time and costs.

On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tolchard, Julian Richard, E-mail: tolchard@material.ntnu.no; Sømme, Astri; Solberg, Jan Ketil

2015-01-15

Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction inmore » the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.« less

The quality of sperm preparation medium affects the motility, viability, and DNA integrity of human spermatozoa.

PubMed

Anbari, Fatemeh; Halvaei, Iman; Nabi, Ali; Ghazali, Shahin; Khalili, Mohammad Ali; Johansson, Lars

2016-01-01

The goal was to compare the effects of three different sperm preparation media on sperm motility, viability, and DNA integrity of semen samples from normozoospermic men. A total of 15 normozoospermic males were included in the study. The semen analysis (SA) was performed in accordance with the WHO guidelines (2010). After SA, each sample was divided into three aliquots, and swim-up was performed with three different sperm preparation media (Sperm Preparation Media, Origio, Denmark; Ham's F10, Biochrome, Berlin, Germany; and VitaSperm™, Innovative Biotech, Iran). Sperm motility, viability, and DNA fragmentation were evaluated at 0, 1, 2, and 24 h after swim-up. There were no significant differences, at any time intervals, in the total sperm motility between the different sperm preparation media. However, the rate of progressive motility was significantly higher in spermatozoa prepared using the media from Origio in comparison with VitaSperm™ ( P = 0.03), whereas no significant difference was found against Ham's F10 medium. No significant differences in sperm viability were seen between the media products. However, 1 h after swim-up, the extent of sperm DNA fragmentation was lower in the medium from Origio versus VitaSperm™ ( P = 0.02). The data showed that the quality of medium for preparation of semen samples from normozoospermic men significantly affects the performance of spermatozoa in assisted conception programs.

Demonstration of the ExoMars sample preparation and distribution system jointly with an optical instrument head

NASA Astrophysics Data System (ADS)

Schulte, Wolfgang; Thiele, Hans; Hofmann, Peter; Baglioni, Pietro

The ExoMars program will search for past and present life on Mars. ExoMars will address important scientific goals and demonstrate key in-situ enabling technologies. Among such technologies are the acquisition, preparation, distribution and analysis of samples from Mars surface rocks and from the subsurface. The 2018 mission will land an ESA rover on Mars which carries a sample preparation and distribution system (SPDS) and a suite of analytical instruments, the Pasteur Payload with its Analytical Laboratory Drawer (ALD). Kayser-Threde GmbH (Germany) will be responsible for the SPDS as a subcontractor under the mission prime Thales Alenia Space. The SPDS comprises a number of complex mechanisms and mechanical devices designed to transport drill core samples within the rover analytical laboratory, to crush them to powder with a fine grain size, to portion discrete amounts of powdered sample material, to distribute and fill the material into sample containers and to prepare flat sample surfaces for scientific analysis. Breadboards of the crushing mechanism, the dosing mechanism and a distribution carousel with sample containers and a powder sample surface flattening mechanism were built and tested. Kayser-Threde, as a member of the Spanish led ExoMars Raman Instrument team, is also responsible for development of the Raman optical head, which will be mounted inside ALD and will inspect the crushed samples, when they are presented to the instrument by the distribution carousel. Within this activity, which is performed under contract with the Institute of Physical Chemistry of the University of Jena (Germany) and funded by the German DLR, Kayser-Threde can demonstrate Raman measurements with the optical head and a COTS laser and spectrometer and thus simulate the full Raman instrument optical path. An autofocus system with actuator and feedback optics is also part of this activity, which allows focusing the 50 m Raman spot on the surface of the powdered sample. Availability of both, the SPDS mechanisms and the Raman Spectrometer optical head at Kayser-Threde facilities allowed to demonstrate for the first time a sample preparation chain with a joint operation of the optical head. Mineral samples were crushed, dosed into sample containers on the carousel, flattened and then inspected by the Raman optical head. The samples were provided by the University of Jena, a member of the ExoMars Raman science team. This paper will give an overview of the breadboards developed so far for the ExoMars SPDS and the Raman optical head and illustrate the joint demonstration test setup of the SPDS with the instrument. The different behavior of different sample materials will be highlighted and first conclusions will be drawn on what could be learned from test setups combining the ExoMars SPDS and analytical instruments.

Computationally Aided Absolute Stereochemical Determination of Enantioenriched Amines.

PubMed

Zhang, Jun; Gholami, Hadi; Ding, Xinliang; Chun, Minji; Vasileiou, Chrysoula; Nehira, Tatsuo; Borhan, Babak

2017-03-17

A simple and efficient protocol for sensing the absolute stereochemistry and enantiomeric excess of chiral monoamines is reported. Preparation of the sample requires a single-step reaction of the 1,1'-(bromomethylene)dinaphthalene (BDN) with the chiral amine. Analysis of the exciton coupled circular dichroism generated from the BDN-derivatized chiral amine sample, along with comparison to conformational analysis performed computationally, yields the absolute stereochemistry of the parent chiral monoamine.

Rapid and accurate detection of urinary pathogens by mobile IMS-based electronic nose: a proof-of-principle study.

PubMed

Roine, Antti; Saviauk, Taavi; Kumpulainen, Pekka; Karjalainen, Markus; Tuokko, Antti; Aittoniemi, Janne; Vuento, Risto; Lekkala, Jukka; Lehtimäki, Terho; Tammela, Teuvo L; Oksala, Niku K J

2014-01-01

Urinary tract infection (UTI) is a common disease with significant morbidity and economic burden, accounting for a significant part of the workload in clinical microbiology laboratories. Current clinical chemisty point-of-care diagnostics rely on imperfect dipstick analysis which only provides indirect and insensitive evidence of urinary bacterial pathogens. An electronic nose (eNose) is a handheld device mimicking mammalian olfaction that potentially offers affordable and rapid analysis of samples without preparation at athmospheric pressure. In this study we demonstrate the applicability of ion mobility spectrometry (IMS) -based eNose to discriminate the most common UTI pathogens from gaseous headspace of culture plates rapidly and without sample preparation. We gathered a total of 101 culture samples containing four most common UTI bacteries: E. coli, S. saprophyticus, E. faecalis, Klebsiella spp and sterile culture plates. The samples were analyzed using ChemPro 100i device, consisting of IMS cell and six semiconductor sensors. Data analysis was conducted by linear discriminant analysis (LDA) and logistic regression (LR). The results were validated by leave-one-out and 5-fold cross validation analysis. In discrimination of sterile and bacterial samples sensitivity of 95% and specificity of 97% were achieved. The bacterial species were identified with sensitivity of 95% and specificity of 96% using eNose as compared to urine bacterial cultures. These findings strongly demonstrate the ability of our eNose to discriminate bacterial cultures and provides a proof of principle to use this method in urinanalysis of UTI.

Study of sample preparation for determination of endocannabinoids and analogous compounds in human serum by LC-MS/MS in MRM mode.

PubMed

Luque-Córdoba, D; Calderón-Santiago, M; Luque de Castro, M D; Priego-Capote, F

2018-08-01

Endocannabinoids are lipids with a key role in physiological processes such as the immune response or the metabolism. This involvement explains their association to pathologies such as cancer, obesity or multiple sclerosis. The determination of endocannabinoids constitutes a challenge for clinical laboratories due to the variety of biological matrices and the wide range of concentrations at which they can be found. This research deals with the comparison of three sample preparation strategies (viz., on-line SPE, off-line SPE for interferents removal, and protein precipitation) for subsequent LC-MS/MS analysis of 14 endocannabinoids and analogous compounds in serum. As a result, the on-line coupling between SPE and LC-MS/MS is proposed as the best approach for this determination. The proposed method allows full automation of the overall process, shortening of the analysis time, and avoidance of errors associated with sample preparation steps. The improvement in sensitivity and selectivity thus achieved allows obtaining quantification limits at the pg mL -1 level, which makes possible the application of the method for clinical studies. Copyright © 2018 Elsevier B.V. All rights reserved.

Structural and electrical properties of CZTS thin films by electrodeposition

NASA Astrophysics Data System (ADS)

Rao, M. C.; Basha, Sk. Shahenoor

2018-06-01

CZTS (Cu2ZnSnS4) thin films were coated on ITO glass substrates by single bath electrodeposition technique. The prepared films were subsequently characterized by XRD, SEM, FTIR, UV-visible spectroscopy and Raman studies. The thickness of the thin films was measured by wedge method. X-ray diffraction studies revealed the formation of polycrystalline phase. The morphological surface of the prepared thin films was examined by SEM and AFM and showed the presence of microcrystals on the surface of the samples. The elemental analysis and their compositional ratios present in the samples were confirmed by the energy dispersive X-ray analysis. Functional groups and the position of band structure involved in the materials were confirmed by FTIR. Optical absorption studies were performed on the prepared thin films in the wavelength ranging from 300 to 1000 nm and the energy bandgap values were found to be in the range from 1.39 to 1.60 eV. Raman spectral peak which was observed at 360 cm-1 correspond to kesterite phase, was formed due to the vibration of the molecules. Electrical measurements confirmed the nature of the thin film depending on the charge concentration present in the samples.

Preparation of sulfonated graphene/polypyrrole solid-phase microextraction coating by in situ electrochemical polymerization for analysis of trace terpenes.

PubMed

Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

2014-06-13

In this study, a novel sulfonated graphene/polypyrrole (SG/PPy) solid-phase microextraction (SPME) coating was prepared and fabricated on a stainless-steel wire by a one-step in situ electrochemical polymerization method. Crucial preparation conditions were optimized as polymerization time of 15min and SG doping amount of 1.5mg/mL. SG/PPy coating showed excellent thermal stability and mechanical durability with a long lifespan of more than 200 stable replicate extractions. SG/PPy coating demonstrated higher extraction selectivity and capacity to volatile terpenes than commonly-used commercial coatings. Finally, SG/PPy coating was practically applied for the analysis of volatile components from star anise and fennel samples. The majority of volatile components identified were terpenes, which suggested the ultra-high extraction selectivity of SG/PPy coating to terpenes during real analytical projects. Four typical volatile terpenes were further quantified to be 0.2-27.4μg/g from star anise samples with good recoveries of 76.4-97.8% and 0.1-1.6μg/g from fennel samples with good recoveries of 80.0-93.1%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

New mass-spectrometric facility for the analysis of highly radioactive samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Warmack, R.J.; Landau, L.; Christie, W.H.

A new facility has been completed for the analysis of highly radioactive, gamma-emitting solid samples. A commercial spark-source mass spectrometer was adapted for remote handling and loading. Electrodes are prepared in a hot cell and transported to the adjacent lead-shielded source for analysis. The source was redesigned for ease of shielding, loading, and maintenance. Both solutions and residues from irradiated nuclear fuel dissolutions have been analyzed for elemental concentrations to < 1 ppM; isotopic data have also been obtained.

Trace element analysis of extraterrestrial metal samples by inductively coupled plasma mass spectrometry: the standard solutions and digesting acids.

PubMed

Wang, Guiqin; Wu, Yangsiqian; Lin, Yangting

2016-02-28

Nearly 99% of the total content of extraterrestrial metals is composed of Fe and Ni, but with greatly variable trace element contents. The accuracy obtained in the inductively coupled plasma mass spectrometry (ICP-MS) analysis of solutions of these samples can be significantly influenced by matrix contents, polyatomic ion interference, and the concentrations of external standard solutions. An ICP-MS instrument (X Series 2) was used to determine 30 standard solutions with different concentrations of trace elements, and different matrix contents. Based on these measurements, the matrix effects were determined. Three iron meteorites were dissolved separately in aqua regia and HNO3. Deviations due to variation of matrix contents in the external standard solutions were evaluated and the analysis results of the two digestion methods for iron meteorites were assessed. Our results show obvious deviations due to unmatched matrix contents in the external standard solutions. Furthermore, discrepancy in the measurement of some elements was found between the sample solutions prepared with aqua regia and HNO3, due to loss of chloride during sample preparation and/or incomplete digestion of highly siderophile elements in iron meteorites. An accurate ICP-MS analysis method for extraterrestrial metal samples has been established using external standard solutions with matched matrix contents and digesting the samples with HNO3 and aqua regia. Using the data from this work, the Mundrabilla iron meteorite previously classified as IAB-ung is reclassified as IAB-MG. Copyright © 2016 John Wiley & Sons, Ltd.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of antimony by automated-hydride atomic absorption spectrophotometry

USGS Publications Warehouse

Brown, G.E.; McLain, B.J.

1994-01-01

The analysis of natural-water samples for antimony by automated-hydride atomic absorption spectrophotometry is described. Samples are prepared for analysis by addition of potassium and hydrochloric acid followed by an autoclave digestion. After the digestion, potassium iodide and sodium borohydride are added automatically. Antimony hydride (stibine) gas is generated, then swept into a heated quartz cell for determination of antimony by atomic absorption spectrophotometry. Precision and accuracy data are presented. Results obtained on standard reference water samples agree with means established by interlaboratory studies. Spike recoveries for actual samples range from 90 to 114 percent. Replicate analyses of water samples of varying matrices give relative standard deviations from 3 to 10 percent.

Hydrocarbon group type determination in jet fuels by high performance liquid chromatography

NASA Technical Reports Server (NTRS)

Antoine, A. C.

1977-01-01

Results are given for the analysis of some jet and diesel fuel samples which were prepared from oil shale and coal syncrudes. Thirty-two samples of varying chemical composition and physical properties were obtained. Hydrocarbon types in these samples were determined by fluorescent indicator adsorption (FIA) analysis, and the results from three laboratories are presented and compared. Recently, rapid high performance liquid chromatography (HPLC) methods have been proposed for hydrocarbon group type analysis, with some suggestion for their use as a replacement of the FIA technique. Two of these methods were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.

The structural properties of barium cobalt hexaferrite powder prepared by a simple heat treatment method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chauhan, Chetna, E-mail: chetna.chauhan@nirmauni.ac.in; Jotania, Rajshree, E-mail: rbjotania@gmail.com

2016-05-06

The W-type barium hexaferrite was prepared using a simple heat treatment method. The precursor was calcinated at 650°C for 3 hours and then slowly cooled to room temperature in order to obtain barium cobalt hexaferrite powder. The prepared powder was characterised by different experimental techniques like XRD, FTIR and SEM. The X-ray diffractogram of the sample shows W-and M phases. The particle size calculated by Debye Scherrer formula. The FTIR spectra of the sample was taken at room temperature by using KBr pallet method which confirms the formation of hexaferrite phase. The morphological study on the hexaferrite powder was carriedmore » out by SEM analysis.« less

Clinical nurses' perceptions and expectations of the role of doctorally-prepared nurses: a qualitative study in Iran.

PubMed

Cheraghi, Mohammad-Ali; Jasper, Melanie; Vaismoradi, Mojtaba

2014-01-01

Nurses with doctorates are increasing in number throughout the world, yet the multitude of roles they play following graduation is unclear. The purpose of this study was to explore and describe clinical nurses' perceptions and expectations of the role of doctorally-prepared nurses in Iran. A qualitative study, using a content analysis approach was conducted with 43 clinical nurses chosen using a purposive sampling strategy. Oral, semi-structured and written interviews were used to generate data. During data analysis, three main themes emerged; "advantages of the doctoral degree", "clarification of doctorally-prepared nurses' role in clinical practice", and "unmet expectations of doctorally-prepared nurses". An understanding of the expectations of nurses on the role of doctorally-prepared nurses is needed to improve the collaboration between clinical nurses and doctorally-prepared nurses; remove misunderstandings on the abilities and skills of doctorally-prepared nurses; incorporate the expectations into doctoral education in order to facilitate their collaboration; and also remove the theory and practice gap through the utilisation of doctorally-prepared nurses' knowledge and skills in practice. Copyright © 2013 Elsevier Ltd. All rights reserved.

Optimization of sample preparation variables for wedelolactone from Eclipta alba using Box-Behnken experimental design followed by HPLC identification.

PubMed

Patil, A A; Sachin, B S; Shinde, D B; Wakte, P S

2013-07-01

Coumestan wedelolactone is an important phytocomponent from Eclipta alba (L.) Hassk. It possesses diverse pharmacological activities, which have prompted the development of various extraction techniques and strategies for its better utilization. The aim of the present study is to develop and optimize supercritical carbon dioxide assisted sample preparation and HPLC identification of wedelolactone from E. alba (L.) Hassk. The response surface methodology was employed to study the optimization of sample preparation using supercritical carbon dioxide for wedelolactone from E. alba (L.) Hassk. The optimized sample preparation involves the investigation of quantitative effects of sample preparation parameters viz. operating pressure, temperature, modifier concentration and time on yield of wedelolactone using Box-Behnken design. The wedelolactone content was determined using validated HPLC methodology. The experimental data were fitted to second-order polynomial equation using multiple regression analysis and analyzed using the appropriate statistical method. By solving the regression equation and analyzing 3D plots, the optimum extraction conditions were found to be: extraction pressure, 25 MPa; temperature, 56 °C; modifier concentration, 9.44% and extraction time, 60 min. Optimum extraction conditions demonstrated wedelolactone yield of 15.37 ± 0.63 mg/100 g E. alba (L.) Hassk, which was in good agreement with the predicted values. Temperature and modifier concentration showed significant effect on the wedelolactone yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Microextraction techniques combined with capillary electrophoresis in bioanalysis.

PubMed

Kohler, Isabelle; Schappler, Julie; Rudaz, Serge

2013-01-01

Over the past two decades, many environmentally sustainable sample-preparation techniques have been proposed, with the objective of reducing the use of toxic organic solvents or substituting these with environmentally friendly alternatives. Microextraction techniques (MEs), in which only a small amount of organic solvent is used, have several advantages, including reduced sample volume, analysis time, and operating costs. Thus, MEs are well adapted in bioanalysis, in which sample preparation is mandatory because of the complexity of a sample that is available in small quantities (mL or even μL only). Capillary electrophoresis (CE) is a powerful and efficient separation technique in which no organic solvents are required for analysis. Combination of CE with MEs is regarded as a very attractive environmentally sustainable analytical tool, and numerous applications have been reported over the last few decades for bioanalysis of low-molecular-weight compounds or for peptide analysis. In this paper we review the use of MEs combined with CE in bioanalysis. The review is divided into two sections: liquid and solid-based MEs. A brief practical and theoretical description of each ME is given, and the techniques are illustrated by relevant applications.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Electron Microscopy and Image Analysis for Selected Materials

NASA Technical Reports Server (NTRS)

Williams, George

1999-01-01

This particular project was completed in collaboration with the metallurgical diagnostics facility. The objective of this research had four major components. First, we required training in the operation of the environmental scanning electron microscope (ESEM) for imaging of selected materials including biological specimens. The types of materials range from cyanobacteria and diatoms to cloth, metals, sand, composites and other materials. Second, to obtain training in surface elemental analysis technology using energy dispersive x-ray (EDX) analysis, and in the preparation of x-ray maps of these same materials. Third, to provide training for the staff of the metallurgical diagnostics and failure analysis team in the area of image processing and image analysis technology using NIH Image software. Finally, we were to assist in the sample preparation, observing, imaging, and elemental analysis for Mr. Richard Hoover, one of NASA MSFC's solar physicists and Marshall's principal scientist for the agency-wide virtual Astrobiology Institute. These materials have been collected from various places around the world including the Fox Tunnel in Alaska, Siberia, Antarctica, ice core samples from near Lake Vostoc, thermal vents in the ocean floor, hot springs and many others. We were successful in our efforts to obtain high quality, high resolution images of various materials including selected biological ones. Surface analyses (EDX) and x-ray maps were easily prepared with this technology. We also discovered and used some applications for NIH Image software in the metallurgical diagnostics facility.

Multiplexing N-glycan analysis by DNA analyzer.

PubMed

Feng, Hua-Tao; Li, Pingjing; Rui, Guo; Stray, James; Khan, Shaheer; Chen, Shiaw-Min; Li, Sam F Y

2017-07-01

Analysis of N-glycan structures has been gaining attentions over the years due to their critical importance to biopharma-based applications and growing roles in biological research. Glycan profiling is also critical to the development of biosimilar drugs. The detailed characterization of N-glycosylation is mandatory because it is a nontemplate driven process and that significantly influences critical properties such as bio-safety and bio-activity. The ability to comprehensively characterize highly complex mixtures of N-glycans has been analytically challenging and stimulating because of the difficulties in both the structure complexity and time-consuming sample pretreatment procedures. CE-LIF is one of the typical techniques for N-glycan analysis due to its high separation efficiency. In this paper, a 16-capillary DNA analyzer was coupled with a magnetic bead glycan purification method to accelerate the sample preparation procedure and therefore increase N-glycan assay throughput. Routinely, the labeling dye used for CE-LIF is 8-aminopyrene-1,3,6-trisulfonic acid, while the typical identification method involves matching migration times with database entries. Two new fluorescent dyes were used to either cross-validate and increase the glycan identification precision or simplify sample preparation steps. Exoglycosidase studies were carried out using neuramididase, galactosidase, and fucosidase to confirm the results of three dye cross-validation. The optimized method combines the parallel separation capacity of multiple-capillary separation with three labeling dyes, magnetic bead assisted preparation, and exoglycosidase treatment to allow rapid and accurate analysis of N-glycans. These new methods provided enough useful structural information to permit N-glycan structure elucidation with only one sample injection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct Analysis of Textile Fabrics and Dyes Using IR Matrix-Assisted Laser Desorption Electrospray Ionization (MALDESI) Mass Spectrometry

PubMed Central

Cochran, Kristin H.; Barry, Jeremy A.; Muddiman, David C.; Hinks, David

2012-01-01

The forensic analysis of textile fibers uses a variety of techniques from microscopy to spectroscopy. One such technique that is often used to identify the dye(s) within the fiber is mass spectrometry (MS). In the traditional MS method, the dye must be extracted from the fabric and the dye components are separated by chromatography prior to mass spectrometric analysis. Direct analysis of the dye from the fabric allows the omission of the lengthy sample preparation involved in extraction, thereby significantly reducing the overall analysis time. Herein, a direct analysis of dyed textile fabric was performed using the infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI) source for MS. In MALDESI, an IR laser with wavelength tuned to 2.94 μm is used to desorb the dye from the fabric sample with the aid of water as the matrix. The desorbed dye molecules are then post-ionized by electrospray ionization (ESI). A variety of dye classes were analyzed from various fabrics with little to no sample preparation allowing for the identification of the dye mass and in some cases the fiber polymer. Those dyes that were not detected using MALDESI were also not observed by direct infusion ESI of the dye standard. PMID:23237031

Sample Preparation Report of the Fourth OPCW Confidence Building Exercise on Biomedical Sample Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Udey, R. N.; Corzett, T. H.; Alcaraz, A.

Following the successful completion of the 3rd biomedical confidence building exercise (February 2013 – March 2013), which included the analysis of plasma and urine samples spiked at low ppb levels as part of the exercise scenario, another confidence building exercise was targeted to be conducted in 2014. In this 4th exercise, it was desired to focus specifically on the analysis of plasma samples. The scenario was designed as an investigation of an alleged use of chemical weapons where plasma samples were collected, as plasma has been reported to contain CWA adducts which remain present in the human body for severalmore » weeks (Solano et al. 2008). In the 3rd exercise most participants used the fluoride regeneration method to analyze for the presence of nerve agents in plasma samples. For the 4th biomedical exercise it was decided to evaluate the analysis of human plasma samples for the presence/absence of the VX adducts and aged adducts to blood proteins (e.g., VX-butyrylcholinesterase (BuChE) and aged BuChE adducts using a pepsin digest technique to yield nonapeptides; or equivalent). As the aging of VX-BuChE adducts is relatively slow (t1/2 = 77 hr at 37 °C [Aurbek et al. 2009]), soman (GD), which ages much more quickly (t1/2 = 9 min at 37 °C [Masson et al. 2010]), was used to simulate an aged VX sample. Additional objectives of this exercise included having laboratories assess novel OP-adducted plasma sample preparation techniques and analytical instrumentation methodologies, as well as refining/designating the reporting formats for these new techniques.« less

Micropore-free surface-activated carbon for the analysis of polychlorinated dibenzo-p-dioxins-dibenzofurans and non-ortho-substituted polychlorinated biphenyls in environmental samples.

PubMed

Kemmochi, Yukio; Tsutsumi, Kaori; Arikawa, Akihiro; Nakazawa, Hiroyuki

2002-11-22

2,3,7,8-Substituted polychlorinated dibenzo-p-dioxins/polychlorinated dibenzofurans (PCDD/Fs) and non-ortho-substituted polychlorinated biphenyls (PCBs) account for almost all of the total toxic equivalents (TEQ) in environmental samples. Activated carbon columns are used to fractionate the samples for GC-MS analysis or bioassay. Micropore-free surface-activated carbon is highly selective for PCDD/Fs and non-ortho-PCBs and can improve the conventional activated carbon column clean-up. Along with sulfuric acid-coated diatomaceous earth columns, micropore-free surface-activated carbon provides a rapid, robust, and high-throughput sample preparation method for PCDD/Fs and non-ortho-PCBs analysis.

Integrated Multi-process Microfluidic Systems for Automating Analysis

PubMed Central

Yang, Weichun; Woolley, Adam T.

2010-01-01

Microfluidic technologies have been applied extensively in rapid sample analysis. Some current challenges for standard microfluidic systems are relatively high detection limits, and reduced resolving power and peak capacity compared to conventional approaches. The integration of multiple functions and components onto a single platform can overcome these separation and detection limitations of microfluidics. Multiplexed systems can greatly increase peak capacity in multidimensional separations and can increase sample throughput by analyzing many samples simultaneously. On-chip sample preparation, including labeling, preconcentration, cleanup and amplification, can all serve to speed up and automate processes in integrated microfluidic systems. This paper summarizes advances in integrated multi-process microfluidic systems for automated analysis, their benefits and areas for needed improvement. PMID:20514343

Ion beam promoted lithium absorption in glassy polymeric carbon

NASA Astrophysics Data System (ADS)

Ila, D.; Zimmerman, R. L.; Jenkins, G. M.; Maleki, H.; Poker, D. B.

1995-12-01

Glassy Polymeric Carbon (GPC) samples prepared from a precursor possess accessible pore volume that depends on the heat treatment temperature. We have shown that lithium percolates without diffusion into the accessible pores of GPC samples immersed in a molten lithium salt bath at 700°C. Ion bombardment with 10 MeV Au atoms increases the total pore volume available for lithium occupation even for samples normally impermeable to lithium. The lithium concentration depth profile is measured using Li7(p,2α) nuclear reaction analysis. We will report on lithium percolation into GPC prepared at temperatures between 500°C and 1000°C and activated by a 10 MeV gold ion bombardment.

Czochralski growth of LaPd2Al2 single crystals

NASA Astrophysics Data System (ADS)

Doležal, P.; Rudajevová, A.; Vlášková, K.; Kriegner, D.; Václavová, K.; Prchal, J.; Javorský, P.

2017-10-01

The present study is focused on the preparation of single crystalline LaPd2Al2 by the Czochralski method. Differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX) analyses reveal that LaPd2Al2 is an incongruently melting phase which causes difficulties for the preparation of single crystalline LaPd2Al2 by the Czochralski method. Therefore several non-stoichiometric polycrystalline samples were studied for its preparation. Finally the successful growth of LaPd2Al2 without foreign phases has been achieved by using a non-stoichiometric precursor with atomic composition 22:39:39 (La:Pd:Al). X-ray powder diffraction, EDX analysis and DSC were used for the characterisation. A single crystalline sample was separated from the ingot prepared by the Czochralski method using the non-stoichiometric precursor. The presented procedure for the preparation of pure single phase LaPd2Al2 could be modified for other incongruently melting phases.

Testing sample stability using four storage methods and the macroalgae Ulva and Gracilaria

EPA Science Inventory

Concern over the relative importance of different sample preparation and storage techniques frequently used in stable isotope analysis of particulate nitrogen (δ15N) and carbon (δ13C) prompted an experiment to determine how important such factors were to measured values in marine...

Outcomes of using wet pooling to detect STEC and Salmonella

USDA-ARS?s Scientific Manuscript database

Objective: The objective of this work was to examine the reliability of wet pooling sample broths. Experimental Design & Analysis: Fresh sample enrichment broths (n=737) were used to prepare 148 wet pools of 5 broths each. The initial broths and the pools were screened for STEC and Salmonella. ...

Thermal Diffusivity of High-Density Polyethylene Samples of Different Crystallinity Evaluated by Indirect Transmission Photoacoustics

NASA Astrophysics Data System (ADS)

Nesic, M.; Popovic, M.; Rabasovic, M.; Milicevic, D.; Suljovrujic, E.; Markushev, D.; Stojanovic, Z.

2018-02-01

In this work, thermal diffusivity of crystalline high-density polyethylene samples of various thickness, and prepared using different procedures, was evaluated by transmission gas-microphone frequency photoacoustics. The samples' composition analysis and their degree of crystallinity were determined from the wide-angle X-ray diffraction, which confirmed that high-density polyethylene samples, obtained by slow and fast cooling, were equivalent in composition but with different degrees of crystallinity. Structural analysis, performed by differential scanning calorimetry, demonstrated that all of the used samples had different levels of crystallinity, depending not only on the preparing procedure, but also on sample thickness. Therefore, in order to evaluate the samples' thermal diffusivity, it was necessary to modify standard photoacoustic fitting procedures (based on the normalization of photoacoustic amplitude and phase characteristics on two thickness levels) for the interpretation of photoacoustic measurements. The calculated values of thermal diffusivity were in the range of the expected literature values. Besides that, the obtained results indicate the unexpected correlation between the values of thermal diffusivity and thermal conductivity with the degree of crystallinity of the investigated geometrically thin samples. The results indicate the necessity of additional investigation of energy transport in macromolecular systems, as well as the possible employment of the photoacoustic techniques in order to clarify its mechanism.

Atmospheric vs. anaerobic processing of metabolome samples for the metabolite profiling of a strict anaerobic bacterium, Clostridium acetobutylicum.

PubMed

Lee, Sang-Hyun; Kim, Sooah; Kwon, Min-A; Jung, Young Hoon; Shin, Yong-An; Kim, Kyoung Heon

2014-12-01

Well-established metabolome sample preparation is a prerequisite for reliable metabolomic data. For metabolome sampling of a Gram-positive strict anaerobe, Clostridium acetobutylicum, fast filtration and metabolite extraction with acetonitrile/methanol/water (2:2:1, v/v) at -20°C under anaerobic conditions has been commonly used. This anaerobic metabolite processing method is laborious and time-consuming since it is conducted in an anaerobic chamber. Also, there have not been any systematic method evaluation and development of metabolome sample preparation for strict anaerobes and Gram-positive bacteria. In this study, metabolome sampling and extraction methods were rigorously evaluated and optimized for C. acetobutylicum by using gas chromatography/time-of-flight mass spectrometry-based metabolomics, in which a total of 116 metabolites were identified. When comparing the atmospheric (i.e., in air) and anaerobic (i.e., in an anaerobic chamber) processing of metabolome sample preparation, there was no significant difference in the quality and quantity of the metabolomic data. For metabolite extraction, pure methanol at -20°C was a better solvent than acetonitrile/methanol/water (2:2:1, v/v/v) at -20°C that is frequently used for C. acetobutylicum, and metabolite profiles were significantly different depending on extraction solvents. This is the first evaluation of metabolite sample preparation under aerobic processing conditions for an anaerobe. This method could be applied conveniently, efficiently, and reliably to metabolome analysis for strict anaerobes in air. © 2014 Wiley Periodicals, Inc.

Small-scale enzymatic digestion of glycoproteins and proteoglycans for analysis of oligosaccharides by LC-MS and FACE gel electrophoresis.

PubMed

Estrella, Ruby P; Whitelock, John M; Roubin, Rebecca H; Packer, Nicolle H; Karlsson, Niclas G

2009-01-01

Structural characterization of oligosaccharides from proteoglycans and other glycoproteins is greatly enhanced through the use of mass spectrometry and gel electrophoresis. Sample preparation for these sensitive techniques often requires enzymatic treatments to produce oligosaccharide sequences for subsequent analysis. This chapter describes several small-scale methods for in-gel, on-blot, and in-solution enzymatic digestions in preparation for graphitized carbon liquid chromatography-mass spectrometry (LC-MS) analysis, with specific applications indicated for glycosaminoglycans (GAGs) and N-linked oligosaccharides. In addition, accompanying procedures for oligosaccharide reduction by sodium borohydride, sample desalting via carbon microcolumn, desialylation by sialidase enzyme treatment, and small-scale oligosaccharide species fractionation are included. Fluorophore-assisted carbohydrate electrophoresis (FACE) is another useful method to isolate derivatized oligosaccharides. Overall, the modularity of these techniques provides ease and flexibility for use in conjunction with mass spectrometric and electrophoretic tools for glycomic research studies.

Honey with Psilocybe mushrooms: a revival of a very old preparation on the drug market?

PubMed

Bogusz, M J; Maier, R D; Schäfer, A T; Erkens, M

1998-01-01

In 1996 samples of suspicious honey preparations were confiscated at the Dutch-German border. The labels on the 50 ml jars indicated that the honey contained Stropharia cubensis (better known as Psilocybe cubensis). The jars were filled with honey with a ca. 1 cm layer of fine particles on the top. The particles were collected and subjected to microscopic and chemical analysis. By microscopy mushroom tissue (plectenchym) and spores typical for the genus Psilocybe were identified in all samples. The HPLC analysis with atmospheric pressure mass spectrometry and diode array detection revealed psilocine but psilocybine was not found. The quantitative analysis was very difficult due to the matrix problems. A search showed that the honey with Psilocybe can be purchased in Dutch coffee shops without any limitations although psilocine and psilocybine belong to listed substances according to Dutch law.

Preparation and characteristics of epoxy/clay/B4C nanocomposite at high concentration of boron carbide for neutron shielding application

NASA Astrophysics Data System (ADS)

Kiani, Mohammad Amin; Ahmadi, Seyed Javad; Outokesh, Mohammad; Adeli, Ruhollah; Mohammadi, Aghil

2017-12-01

In this research, the characteristics of the prepared samples in epoxy matrix by means of X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), as well as scanning electron microscope (SEM) are evaluated. Meanwhile, the obtained mechanical properties of the specimen are investigated. Thermogravimetric analysis (TGA) is also employed to evaluate the thermal degradation of manufactured nanocomposites. The thermal neutron absorption properties of nanocomposites containing 3 wt% of montmorillonite nanoclay (closite30B) have been studied experimentally, using an Am-Be point source. Mechanical tests reveal that the higher B4C concentrations, the more tensile strengths, but lower Young's modulus in all samples under consideration. TGA analysis also shows that thermal stability of the nanocomposite, increases in presence of B4C. Finally, neutron absorption analysis shows that increasing the B4C concentration leads to a nonlinearly build-up of neutron absorption cross section.

Rapid analysis of the skin irritant p-phenylenediamine (PPD) in henna products using atmospheric solids analysis probe mass spectrometry.

PubMed

Chen, Weiyang; Nkosi, Thobile A N; Combrinck, Sandra; Viljoen, Alvaro M; Cartwright-Jones, Catherine

2016-09-05

Henna (Lawsonia inermis) is applied to stain keratin, present in hair, skin and fingernails, a red-orange or rust colour. Producers of temporary tattoos mix the aromatic amine compound, para-phenylenediamine (PPD) into natural henna to create 'black henna' that rapidly stains the skin black. However, PPD may cause severe delayed hypersensitivity reactions following skin contact. This study proposes a rapid direct-analysis method to detect and identify PPD using an atmospheric solids analysis probe (ASAP) coupled to a Q-ToF mass spectrometer (MS). Since laborious, multistep methods of analysis to determine PPD are undesirable, due to the instability of the compound in solution, a screening method involving no sample preparation steps was developed. Experiments were carried out to optimise the corona current, sample cone voltage, source temperature, and desolvation gas temperature to determine ideal ASAP-Q-ToF-MS analysing conditions. Eleven of the 109 henna samples, originating from various countries, tested positive for PPD when henna products were screened using ASAP-MS, without any form of sample preparation other than grinding. Ultra-performance liquid chromatography electrospray ionisation-mass spectrometry (UPLC-Q-ToF-MS) was subsequently used to confirm the results from ASAP and to determine the concentrations of PPD in henna products. The allergen was detected in the same eleven samples, with concentrations ranging from 0.05-4.21% (w/w). It can be concluded that the sensitivity of the ASAP-MS technique is sufficient (limit of detection=0.025% w/w) to allow screening of henna samples for the presence of PPD. This relatively new technique can be applied to commercial products without extraction, sample treatment or chromatographic separation. Copyright © 2016 Elsevier B.V. All rights reserved.

Improved Identification of Membrane Proteins by MALDI-TOF MS/MS Using Vacuum Sublimated Matrix Spots on an Ultraphobic Chip Surface

PubMed Central

Poetsch, Ansgar; Schlüsener, Daniela; Florizone, Christine; Eltis, Lindsay; Menzel, Christoph; Rögner, Matthias; Steinert, Kerstin; Roth, Udo

2008-01-01

Integral membrane proteins are notoriously difficult to identify and analyze by mass spectrometry because of their low abundance and limited number of trypsin cleavage sites. Our strategy to address this problem is based on a novel technology for MALDI-MS peptide sample preparation that increases the success rate of membrane protein identification by increasing the sensitivity of the MALDI-TOF system. For this, we used sample plates with predeposited matrix spots of CHCA crystals prepared by vacuum sublimation onto an extremely low wettable (ultraphobic) surface. In experiments using standard peptides, an up to 10-fold gain of sensitivity was found for on-chip preparations compared with classical dried-droplet preparations on a steel target. In order to assess the performance of the chips with membrane proteins, three model proteins (bacteriorhodopsin, subunit IV(a) of ATP synthase, and the cp47 subunit from photosystem II) were analyzed. To mimic realistic analysis conditions, purified proteins were separated by SDS-PAGE and digested with trypsin. The digest MALDI samples were prepared either by dried-droplet technique on steel plates using CHCA as matrix, or applied directly onto the matrix spots of the chip surface. Significantly higher signal-to-noise ratios were observed for all of the spectra resulting from on-chip preparations of different peptides. In a second series of experiments, the membrane proteome of Rhodococcus jostii RHA1 was investigated by AIEC/SDS-PAGE in combination with MALDI-TOF MS/MS. As in the first experiments, Coomassie-stained SDS-PAGE bands were digested and the two different preparation methods were compared. For preparations on the Mass·Spec·Turbo Chip, 43 of 60 proteins were identified, whereas only 30 proteins were reliably identified after classical sample preparation. Comparison of the obtained Mascot scores, which reflect the confidence level of the protein identifications, revealed that for 70% of the identified proteins, higher scores were obtained by on-chip sample preparation. Typically, this gain was a consequence of higher sequence coverage due to increased sensitivity. PMID:19137096

Fusion Bead Procedure for Nuclear Forensics Employing Synthetic Enstatite to Dissolve Uraniferous and Other Challenging Materials Prior to Laser Ablation Inductively Coupled Plasma Mass Spectrometry.

PubMed

Reading, David G; Croudace, Ian W; Warwick, Phillip E

2017-06-06

There is an increasing demand for rapid and effective analytical tools to support nuclear forensic investigations of seized or suspect materials. Some methods are simply adapted from other scientific disciplines and can effectively be used to rapidly prepare complex materials for subsequent analysis. A novel sample fusion method is developed, tested, and validated to produce homogeneous, flux-free glass beads of geochemical reference materials (GRMs), uranium ores, and uranium ore concentrates (UOC) prior to the analysis of 14 rare earth elements (REE) via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The novelty of the procedure is the production of glass beads using 9 parts high purity synthetic enstatite (MgSiO 3 ) as the glass former with 1 part of sample (sample mass ∼1.5 mg). The beads are rapidly prepared (∼10 min overall time) by fusing the blended mixture on an iridium strip resistance heater in an argon-purged chamber. Many elements can be measured in the glass bead, but the rare earth group in particular is a valuable series in nuclear forensic studies and is well-determined using LA-ICP-MS. The REE data obtained from the GRMs, presented as chondrite normalized patterns, are in very good agreement with consensus patterns. The UOCs have comparable patterns to solution ICP-MS methods and published data. The attractions of the current development are its conservation of sample, speed of preparation, and suitability for microbeam analysis, all of which are favorable for nuclear forensics practitioners and geochemists requiring REE patterns from scarce or valuable samples.

Characterization and application of automated in-vacuum PIXE/EBS system for direct analysis of chloride and sulfate ions attack in cementitious materials

NASA Astrophysics Data System (ADS)

Rihawy, M. S.; Alwazzeh, M.; Abbas, K.

2018-01-01

Ion beam analysis (IBA) techniques (Particle Induced X-ray Emission, PIXE and Elastic Backscattering Spectrometry, EBS), were applied to investigate chloride and sulfate ions diffusion into laboratory prepared mortar samples. Development and characterization of an automated in-vacuum macro PIXE/EBS system is thoroughly discussed. Depth profile information of both chloride and sulfate ions in laboratory prepared mortar samples, after immersion in sea water for nine months, was rapidly and easily obtained at fairly low cost and with standardless analysis, demonstrating the value of the application of IBA to elemental depth profiling in cementitious materials. Chloride and sulfate depth profiles were obtained for two sets of mortar samples, one prepared with different water/cement (W/C) ratios and the other with different sand/cement (S/C) ratios. Results showed higher diffusion rates of both chloride and sulfate ions when both ratios are increased. Additionally, the W/C ratio has a stronger influence in both sulfate and chloride penetration than the S/C ratio, and chloride ions penetrate faster than sulfates. Advantages and limitations of applying IBA techniques in this investigation are discussed. The comparison between PIXE and other X-ray based analytical techniques, namely X-ray fluorescence (XRF) and energy and wavelength dispersive X-rays (EDX/WDX), as well as other traditional wet chemical methods is reviewed, and industrial applications are discussed.

Effect of S-doping on structural, optical and electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

NASA Astrophysics Data System (ADS)

Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

2013-12-01

In this research, S-doped vanadium oxide thin films, with doping levels from 0 to 40 at.%, are prepared by spray pyrolysis technique on glass substrates. For electrochemical measurements, the films were deposited on florin-tin oxide coated glass substrates. The effect of S-doping on structural, electrical, optical and electrochemical properties of vanadium oxide thin films was studied. The x-ray diffractometer analysis indicated that most of the samples have cubic β-V2O5 phase structure with preferred orientation along [200]. With increase in the doping levels, the structure of the samples tends to be amorphous. The scanning electron microscopy images show that the structure of the samples is nanobelt-shaped and the width of the nanobelts decreases from nearly 100 to 40 nm with increase in the S concentration. With increase in the S-doping level, the sheet resistance and the optical band gap increase from 940 to 4015 kΩ/square and 2.41 to 2.7 eV, respectively. The cyclic voltammogram results obtained for different samples show that the undoped sample is expanded and the sample prepared at 20 at.% S-doping level has sharper anodic and cathodic peaks.

Automation of sample preparation for mass cytometry barcoding in support of clinical research: protocol optimization.

PubMed

Nassar, Ala F; Wisnewski, Adam V; Raddassi, Khadir

2017-03-01

Analysis of multiplexed assays is highly important for clinical diagnostics and other analytical applications. Mass cytometry enables multi-dimensional, single-cell analysis of cell type and state. In mass cytometry, the rare earth metals used as reporters on antibodies allow determination of marker expression in individual cells. Barcode-based bioassays for CyTOF are able to encode and decode for different experimental conditions or samples within the same experiment, facilitating progress in producing straightforward and consistent results. Herein, an integrated protocol for automated sample preparation for barcoding used in conjunction with mass cytometry for clinical bioanalysis samples is described; we offer results of our work with barcoding protocol optimization. In addition, we present some points to be considered in order to minimize the variability of quantitative mass cytometry measurements. For example, we discuss the importance of having multiple populations during titration of the antibodies and effect of storage and shipping of labelled samples on the stability of staining for purposes of CyTOF analysis. Data quality is not affected when labelled samples are stored either frozen or at 4 °C and used within 10 days; we observed that cell loss is greater if cells are washed with deionized water prior to shipment or are shipped in lower concentration. Once the labelled samples for CyTOF are suspended in deionized water, the analysis should be performed expeditiously, preferably within the first hour. Damage can be minimized if the cells are resuspended in phosphate-buffered saline (PBS) rather than deionized water while waiting for data acquisition.

Use of on-site high performance liquid chromatography to evaluate the magnitude and extent of organic contaminants in aquifers

USGS Publications Warehouse

Goerlitz, D.F.; Franks, B.J.

1989-01-01

Appraisal of ground water contaminated by organic substances raises problems of difficult sample collection and timely chemical analysis. High-performance liquid chromatography was evaluated for on-site determination of specific organic contaminants in ground water samples and was used at three study sites. Organic solutes were determined directly in water samples, with little or no preparation, and usually in less than an hour after collection. This information improved sampling efficiency and was useful in screening for subsequent laboratory analysis. On two occasions, on-site analysis revealed that samples were undergoing rapid change, with major solutes being upgraded and alteration products being formed. In addition to sample stability, this technique proved valuable for monitoring other sampling factors such as compositional changes with respect to pumping, filtration, and cross contamination. -Authors

Determination of free sulfites (SO3-2) in dried fruits processed with sulfur dioxide by ion chromatography through anion exchange column and conductivity detection.

PubMed

Liao, Benjamin S; Sram, Jacqueline C; Files, Darin J

2013-01-01

A simple and effective anion ion chromatography (IC) method with anion exchange column and conductivity detector has been developed to determine free sulfites (SO3-2) in dried fruits processed with sulfur dioxide. No oxidation agent, such as hydrogen peroxide, is used to convert sulfites to sulfates for IC analysis. In addition, no stabilizing agent, such as formaldehyde, fructose or EDTA, is required during the sample extraction. This method uses aqueous 0.2 N NaOH as the solvent for standard preparation and sample extraction. The sulfites, either prepared from standard sodium sulfite powder or extracted from food samples, are presumed to be unbound SO3-2 in aqueous 0.2 N NaOH (pH > 13), because the bound sulfites in the sample matrix are released at pH > 10. In this study, sulfites in the standard solutions were stable at room temperature (i.e., 15-25 degrees C) for up to 12 days. The lowest standard of the linear calibration curve is set at 1.59 microg/mL SO3-2 (equivalent to 6.36 microg/g sample with no dilution) for analysis of processed dried fruits that would contain high levels (>1000 microg/g) of sulfites. As a consequence, this method typically requires significant dilution of the sample extract. Samples are prepared with a simple procedure of sample compositing, extraction with aqueous 0.2 N NaOH, centrifugation, dilution as needed, and filtration prior to IC. The sulfites in these sample extracts are stable at room temperature for up to 20 h. Using anion IC, the sulfites are eluted under isocratic conditions with 10 mM aqueous sodium carbonate solution as the mobile phase passing through an anion exchange column. The sulfites are easily separated, with an analysis run time of 18 min, regardless of the dried fruit matrix. Recoveries from samples spiked with sodium sulfites were demonstrated to be between 81 and 105% for five different fruit matrixes (apricot, golden grape, white peach, fig, and mango). Overall, this method is simple to perform and effective for the determination of high levels of sulfites in dried fruits.

Measuring Parent Time Scarcity and Fatigue as Barriers to Meal Planning and Preparation: Quantitative Scale Development

ERIC Educational Resources Information Center

Storfer-Isser, Amy; Musher-Eizenman, Dara

2013-01-01

Objective: To examine the psychometric properties of 9 quantitative items that assess time scarcity and fatigue as parent barriers to planning and preparing meals for their children. Methods: A convenience sample of 342 parents of children aged 2-6 years completed a 20-minute online survey. Exploratory factor analysis was used to examine the…

Biomedical applications of laser-induced breakdown spectroscopy (LIBS)

NASA Astrophysics Data System (ADS)

Unnikrishnan, V. K.; Nayak, Rajesh; Bhat, Sujatha; Mathew, Stanley; Kartha, V. B.; Santhosh, C.

2015-03-01

LIBS has been proven to be a robust elemental analysis tool attracting interest because of the wide applications. LIBS can be used for analysis of any type of samples i.e. environmental/physiological, regardless of its state of matter. Conventional spectroscopy techniques are good in analytical performance, but their sample preparation method is mostly destructive and time consuming. Also, almost all these methods are incapable of analysing multi elements simaltaneously. On the other hand, LIBS has many potential advantages such as simplicity in the experimental setup, less sample preparation, less destructive analysis of sample etc. In this paper, we report some of the biomedical applications of LIBS. From the experiments carried out on clinical samples (calcified tissues or teeth and gall stones) for trace elemental mapping and detection, it was found that LIBS is a robust tool for such applications. It is seen that the presence and relative concentrations of major elements (calcium, phosphorus and magnesium) in human calcified tissue (tooth) can be easily determined using LIBS technique. The importance of this study comes in anthropology where tooth and bone are main samples from which reliable data can be easily retrieved. Similarly, elemental composition of bile juice and gall stone collected from the same subject using LIBS was found to be similar. The results show interesting prospects for LIBS to study cholelithiasis (the presence of stones in the gall bladder, is a common disease of the gastrointestinal tract) better.

Removal of BrO₃⁻ from drinking water samples using newly developed agricultural waste-based activated carbon and its determination by ultra-performance liquid chromatography-mass spectrometry.

PubMed

Naushad, Mu; Khan, Mohammad R; ALOthman, Zeid A; AlSohaimi, Ibrahim; Rodriguez-Reinoso, Francisco; Turki, Turki M; Ali, Rahmat

2015-10-01

Activated carbon was prepared from date pits via chemical activation with H3PO4. The effects of activating agent concentration and activation temperature on the yield and surface area were studied. The optimal activated carbon was prepared at 450 °C using 55 % H3PO4. The prepared activated carbon was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer, Emmett, and Teller (BET) surface area. The prepared date pit-based activated carbon (DAC) was used for the removal of bromate (BrO3 (-)). The concentration of BrO3 (-) was determined by ultra-performance liquid chromatography-mass tandem spectrometry (UPLC-MS/MS). The experimental equilibrium data for BrO3 (-) adsorption onto DAC was well fitted to the Langmuir isotherm model and showed maximum monolayer adsorption capacity of 25.64 mg g(-1). The adsorption kinetics of BrO3 (-) adsorption was very well represented by the pseudo-first-order equation. The analytical application of DAC for the analysis of real water samples was studied with very promising results.

Effect of sample preparation method on quantification of polymorphs using PXRD.

PubMed

Alam, Shahnwaz; Patel, Sarsvatkumar; Bansal, Arvind Kumar

2010-01-01

The purpose of this study was to improve the sensitivity and accuracy of quantitative analysis of polymorphic mixtures. Various techniques such as hand grinding and mixing (in mortar and pestle), air jet milling and ball milling for micronization of particle and mixing were used to prepare binary mixtures. Using these techniques, mixtures of form I and form II of clopidogrel bisulphate were prepared in various proportions from 0-5% w/w of form I in form II and subjected to x-ray powder diffraction analysis. In order to obtain good resolution in minimum time, step time and step size were varied to optimize scan rate. Among the six combinations, step size of 0.05 degrees with step time of 5 s demonstrated identification of maximum characteristic peaks of form I in form II. Data obtained from samples prepared using both grinding and mixing in ball mill showed good analytical sensitivity and accuracy compared to other methods. Powder x-ray diffraction method was reproducible, precise with LOD of 0.29% and LOQ of 0.91%. Validation results showed excellent correlation between actual and predicted concentration with R2 > 0.9999.

Author Contribution to the Pu Handbook II: Chapter 37 LLNL Integrated Sample Preparation Glovebox (TEM) Section

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wall, Mark A.

The development of our Integrated Actinide Sample Preparation Laboratory (IASPL) commenced in 1998 driven by the need to perform transmission electron microscopy studies on naturally aged plutonium and its alloys looking for the microstructural effects of the radiological decay process (1). Remodeling and construction of a laboratory within the Chemistry and Materials Science Directorate facilities at LLNL was required to turn a standard radiological laboratory into a Radiological Materials Area (RMA) and Radiological Buffer Area (RBA) containing type I, II and III workplaces. Two inert atmosphere dry-train glove boxes with antechambers and entry/exit fumehoods (Figure 1), having a baseline atmospheremore » of 1 ppm oxygen and 1 ppm water vapor, a utility fumehood and a portable, and a third double-walled enclosure have been installed and commissioned. These capabilities, along with highly trained technical staff, facilitate the safe operation of sample preparation processes and instrumentation, and sample handling while minimizing oxidation or corrosion of the plutonium. In addition, we are currently developing the capability to safely transfer small metallographically prepared samples to a mini-SEM for microstructural imaging and chemical analysis. The gloveboxes continue to be the most crucial element of the laboratory allowing nearly oxide-free sample preparation for a wide variety of LLNL-based characterization experiments, which includes transmission electron microscopy, electron energy loss spectroscopy, optical microscopy, electrical resistivity, ion implantation, X-ray diffraction and absorption, magnetometry, metrological surface measurements, high-pressure diamond anvil cell equation-of-state, phonon dispersion measurements, X-ray absorption and emission spectroscopy, and differential scanning calorimetry. The sample preparation and materials processing capabilities in the IASPL have also facilitated experimentation at world-class facilities such as the Advanced Photon Source at Argonne National Laboratory, the European Synchrotron Radiation Facility in Grenoble, France, the Stanford Synchrotron Radiation Facility, the National Synchrotron Light Source at Brookhaven National Laboratory, the Advanced Light Source at Lawrence Berkeley National Laboratory, and the Triumph Accelerator in Canada.« less

Measurements of 55Fe activity in activated steel samples with GEMPix

NASA Astrophysics Data System (ADS)

Curioni, A.; Dinar, N.; La Torre, F. P.; Leidner, J.; Murtas, F.; Puddu, S.; Silari, M.

2017-03-01

In this paper we present a novel method, based on the recently developed GEMPix detector, to measure the 55Fe content in samples of metallic material activated during operation of CERN accelerators and experimental facilities. The GEMPix, a gas detector with highly pixelated read-out, has been obtained by coupling a triple Gas Electron Multiplier (GEM) to a quad Timepix ASIC. Sample preparation, measurements performed on 45 samples and data analysis are described. The calibration factor (counts per second per unit specific activity) has been obtained via measurements of the 55Fe activity determined by radiochemical analysis of the same samples. Detection limit and sensitivity to the current Swiss exemption limit are calculated. Comparison with radiochemical analysis shows inconsistency for the sensitivity for only two samples, most likely due to underestimated uncertainties of the GEMPix analysis. An operative test phase of this technique is already planned at CERN.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gillespie, B.M.; Stromatt, R.W.; Ross, G.A.

This data package contains the results obtained by Pacific Northwest Laboratory (PNL) staff in the characterization of samples for the 101-SY Hydrogen Safety Project. The samples were submitted for analysis by Westinghouse Hanford Company (WHC) under the Technical Project Plan (TPP) 17667 and the Quality Assurance Plan MCS-027. They came from a core taken during Window C'' after the May 1991 gas release event. The analytical procedures required for analysis were defined in the Test Instructions (TI) prepared by the PNL 101-SY Analytical Chemistry Laboratory (ACL) Project Management Office in accordance with the TPP and the QA Plan. The requestedmore » analysis for these samples was volatile organic analysis. The quality control (QC) requirements for each sample are defined in the Test Instructions for each sample. The QC requirements outlined in the procedures and requested in the WHC statement of work were followed.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gillespie, B.M.; Stromatt, R.W.; Ross, G.A.

This data package contains the results obtained by Pacific Northwest Laboratory (PNL) staff in the characterization of samples for the 101-SY Hydrogen Safety Project. The samples were submitted for analysis by Westinghouse Hanford Company (WHC) under the Technical Project Plan (TPP) 17667 and the Quality Assurance Plan MCS-027. They came from a core taken during Window ``C`` after the May 1991 gas release event. The analytical procedures required for analysis were defined in the Test Instructions (TI) prepared by the PNL 101-SY Analytical Chemistry Laboratory (ACL) Project Management Office in accordance with the TPP and the QA Plan. The requestedmore » analysis for these samples was volatile organic analysis. The quality control (QC) requirements for each sample are defined in the Test Instructions for each sample. The QC requirements outlined in the procedures and requested in the WHC statement of work were followed.« less

Retrospective MicroRNA Sequencing: Complementary DNA Library Preparation Protocol Using Formalin-fixed Paraffin-embedded RNA Specimens.

PubMed

Loudig, Olivier; Liu, Christina; Rohan, Thomas; Ben-Dov, Iddo Z

2018-05-05

-Archived, clinically classified formalin-fixed paraffin-embedded (FFPE) tissues can provide nucleic acids for retrospective molecular studies of cancer development. By using non-invasive or pre-malignant lesions from patients who later develop invasive disease, gene expression analyses may help identify early molecular alterations that predispose to cancer risk. It has been well described that nucleic acids recovered from FFPE tissues have undergone severe physical damage and chemical modifications, which make their analysis difficult and generally requires adapted assays. MicroRNAs (miRNAs), however, which represent a small class of RNA molecules spanning only up to ~18-24 nucleotides, have been shown to withstand long-term storage and have been successfully analyzed in FFPE samples. Here we present a 3' barcoded complementary DNA (cDNA) library preparation protocol specifically optimized for the analysis of small RNAs extracted from archived tissues, which was recently demonstrated to be robust and highly reproducible when using archived clinical specimens stored for up to 35 years. This library preparation is well adapted to the multiplex analysis of compromised/degraded material where RNA samples (up to 18) are ligated with individual 3' barcoded adapters and then pooled together for subsequent enzymatic and biochemical preparations prior to analysis. All purifications are performed by polyacrylamide gel electrophoresis (PAGE), which allows size-specific selections and enrichments of barcoded small RNA species. This cDNA library preparation is well adapted to minute RNA inputs, as a pilot polymerase chain reaction (PCR) allows determination of a specific amplification cycle to produce optimal amounts of material for next-generation sequencing (NGS). This approach was optimized for the use of degraded FFPE RNA from specimens archived for up to 35 years and provides highly reproducible NGS data.

Environmental analysis of higher brominated diphenyl ethers and decabromodiphenyl ethane.

PubMed

Kierkegaard, Amelie; Sellström, Ulla; McLachlan, Michael S

2009-01-16

Methods for environmental analysis of higher brominated diphenyl ethers (PBDEs), in particular decabromodiphenyl ether (BDE209), and the recently discovered environmental contaminant decabromodiphenyl ethane (deBDethane) are reviewed. The extensive literature on analysis of BDE209 has identified several critical issues, including contamination of the sample, degradation of the analyte during sample preparation and GC analysis, and the selection of appropriate detection methods and surrogate standards. The limited experience with the analysis of deBDethane suggests that there are many commonalities with BDE209. The experience garnered from the analysis of BDE209 over the last 15 years will greatly facilitate progress in the analysis of deBDethane.

Global metabolic profiling procedures for urine using UPLC-MS.

PubMed

Want, Elizabeth J; Wilson, Ian D; Gika, Helen; Theodoridis, Georgios; Plumb, Robert S; Shockcor, John; Holmes, Elaine; Nicholson, Jeremy K

2010-06-01

The production of 'global' metabolite profiles involves measuring low molecular-weight metabolites (<1 kDa) in complex biofluids/tissues to study perturbations in response to physiological challenges, toxic insults or disease processes. Information-rich analytical platforms, such as mass spectrometry (MS), are needed. Here we describe the application of ultra-performance liquid chromatography-MS (UPLC-MS) to urinary metabolite profiling, including sample preparation, stability/storage and the selection of chromatographic conditions that balance metabolome coverage, chromatographic resolution and throughput. We discuss quality control and metabolite identification, as well as provide details of multivariate data analysis approaches for analyzing such MS data. Using this protocol, the analysis of a sample set in 96-well plate format, would take ca. 30 h, including 1 h for system setup, 1-2 h for sample preparation, 24 h for UPLC-MS analysis and 1-2 h for initial data processing. The use of UPLC-MS for metabolic profiling in this way is not faster than the conventional HPLC-based methods but, because of improved chromatographic performance, provides superior metabolome coverage.

Film analysis employing subtarget effect using 355 nm Nd-YAG laser-induced plasma at low pressure

NASA Astrophysics Data System (ADS)

Hedwig, Rinda; Budi, Wahyu Setia; Abdulmadjid, Syahrun Nur; Pardede, Marincan; Suliyanti, Maria Margaretha; Lie, Tjung Jie; Kurniawan, Davy Putra; Kurniawan, Koo Hendrik; Kagawa, Kiichiro; Tjia, May On

2006-12-01

The applicability of spectrochemical analysis for liquid and powder samples of minute amount in the form of thin film was investigated using ultraviolet Nd-YAG laser (355 nm) and low-pressure ambient air. A variety of organic samples such as commercial black ink usually used for stamp pad, ginseng extract, human blood, liquid milk and ginseng powder was prepared as film deposited on the surface of an appropriate hard substrate such as copper plate or glass slide. It was demonstrated that in all cases studied, good quality spectra were obtained with very low background and free from undesirable contamination by the substrate elements, featuring ppm or even sub-ppm sensitivity and worthy of application for quantitative analysis of organic samples. The proper preparation of the films was found to be crucial in achieving the high quality spectra. It was further shown that much inferior results were obtained when the atmospheric-pressure (101 kPa) operating condition of laser-induced breakdown spectroscopy or the fundamental wavelength of the Nd-YAG laser was employed due to the excessive or improper laser ablation process.

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y.; Mori, S.; Asthana R.

2016-01-01

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiskoot, R.J.J.

Accurate and reliable sampling systems are imperative when confirming natural gas' commercial value. Buyers and sellers need accurate hydrocarbon-composition information to conduct fair sale transactions. Because of poor sample extraction, preparation or analysis can invalidate the sale, more attention should be directed toward improving representative sampling. Consider all sampling components, i.e., gas types, line pressure and temperature, equipment maintenance and service needs, etc. The paper discusses gas sampling, design considerations (location, probe type, extraction devices, controller, and receivers), operating requirements, and system integration.

Methods for the preparation and analysis of solids and suspended solids for total mercury

USGS Publications Warehouse

Olund, Shane D.; DeWild, John F.; Olson, Mark L.; Tate, Michael T.

2004-01-01

The methods documented in this report are utilized by the Wisconsin District Mercury Lab for analysis of total mercury in solids (soils and sediments) and suspended solids (isolated on filters). Separate procedures are required for the different sample types. For solids, samples are prepared by room-temperature acid digestion and oxidation with aqua regia. The samples are brought up to volume with a 5 percent bromine monochloride solution to ensure complete oxidation and heated at 50?C in an oven overnight. Samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. A method detection limit of 0.3 ng of mercury per digestion bomb was established using multiple analyses of an environmental sample. Based on the range of masses processed, the minimum sample reporting limit varies from 0.6 ng/g to 6 ng/g. Suspended solids samples are oxidized with a 5 percent bromine monochloride solution and held at 50?C in an oven for 5 days. The samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. Using a certified reference material as a surrogate for an environmental sample, a method detection limit of 0.059 ng of mercury per filter was established. The minimum sample reporting limit varies from 0.059 ng/L to 1.18 ng/L, depending on the volume of water filtered.

Enhanced spot preparation for liquid extractive sampling and analysis

DOEpatents

Van Berkel, Gary J.; King, Richard C.

2015-09-22

A method for performing surface sampling of an analyte, includes the step of placing the analyte on a stage with a material in molar excess to the analyte, such that analyte-analyte interactions are prevented and the analyte can be solubilized for further analysis. The material can be a matrix material that is mixed with the analyte. The material can be provided on a sample support. The analyte can then be contacted with a solvent to extract the analyte for further processing, such as by electrospray mass spectrometry.

Application of inductively coupled plasma sector field mass spectrometry for low-level environmental americium-241 analysis.

PubMed

Varga, Zsolt

2007-03-28

An improved and novel sample preparation method for (241)Am analysis by inductively coupled plasma sector field mass spectrometry has been developed. The procedure involves a selective CaF(2) pre-concentration followed by an extraction chromatographic separation using TRU resin. The achieved absolute detection limit of 0.86 fg (0.11 mBq) is comparable to that of alpha spectrometry (0.1 mBq) and suitable for low-level environmental measurements. Analysis of different kinds of environmental standard reference materials (IAEA-384--Fangataufa lagoon sediment, IAEA-385--Irish Sea sediment and IAEA-308--Mixed seaweed from the Mediterranean Sea) and alpha spectrometry were used to validate the procedure. The chemical recovery of sample preparation ranged between 72 and 94%. The results obtained are in good agreement with reference values and those measured by alpha spectrometry. The proposed method offers a rapid and less labor-intensive possibility for environmental (241)Am analysis than the conventionally applied radioanalytical techniques.

Stability of an extemporaneously prepared tadalafil suspension.

PubMed

Pettit, Rebecca S; Johnson, Cary E; Caruthers, Regine L

2012-04-01

The stability of an extemporaneously prepared tadalafil oral suspension was studied. An oral suspension of tadalafil 5 mg/mL was prepared by thoroughly grinding 15 20-mg tadalafil tablets in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of Ora-Sweet were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and at 7, 14, 28, 57, and 91 days. After double dilution (1:10 and 0.1:5 v/v) to an expected concentration of 10 μg/mL with methanol and mobile phase, respectively, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH changes on each day of analysis. Taste evaluation was performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 99% of the initial tadalafil concentration remained throughout the 91-day study period. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. An extemporaneously prepared suspension of tadalafil 5 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet was stable for at least 91 days when stored in amber plastic bottles at room temperature.

Eigenvalue-eigenvector decomposition (EED) analysis of dissimilarity and covariance matrix obtained from total synchronous fluorescence spectral (TSFS) data sets of herbal preparations: Optimizing the classification approach

NASA Astrophysics Data System (ADS)

Tarai, Madhumita; Kumar, Keshav; Divya, O.; Bairi, Partha; Mishra, Kishor Kumar; Mishra, Ashok Kumar

2017-09-01

The present work compares the dissimilarity and covariance based unsupervised chemometric classification approaches by taking the total synchronous fluorescence spectroscopy data sets acquired for the cumin and non-cumin based herbal preparations. The conventional decomposition method involves eigenvalue-eigenvector analysis of the covariance of the data set and finds the factors that can explain the overall major sources of variation present in the data set. The conventional approach does this irrespective of the fact that the samples belong to intrinsically different groups and hence leads to poor class separation. The present work shows that classification of such samples can be optimized by performing the eigenvalue-eigenvector decomposition on the pair-wise dissimilarity matrix.

Phase II Tungsten Fate-and Transport Study for Camp Edwards

DTIC Science & Technology

2010-02-01

soil and water . However, previous studies at the Massachusetts Military Reservation (MMR) at Camp Edwards demonstrated that metallic tungsten used ...7.5-12.5 ft bwt) using a Waterra sampler. Unfiltered and filtered water samples were sent to ERDC-EL for analysis of tungsten and other metals... water for tungsten and metals using ICP-MS, following the USEPA Method 6020 for sample preparation by EPA Method 3005. Metals analysis included antimony

Rapid LC-MS method for the detection of common fragrances in personal care products without sample preparation.

PubMed

Famiglini, Giorgio; Termopoli, Veronica; Palma, Pierangela; Capriotti, Fabiana; Cappiello, Achille

2014-05-01

An LC-MS method for the analysis of personal care and household products without sample preparation is presented. The method takes advantage of the Direct-electron ionization (EI) LC-MS interface for the quantitation of principal components, as well as for the identification of unknown or undeclared ingredients. The technique has proven its inertness toward matrix effects and the electron ionization allows quantitation and library identification. Commercially available products (shower gel, perfume, and hand cream) were diluted with methanol and injected directly into a nano-LC column. Limonene, linalool, and citral were selected as target compounds because of their use as fragrances in toiletry and detergent products. These and all other fragrances are commonly determined with GC-MS analysis, prior to sample cleanup, a procedure that can lead to analytes loss. The selected compounds are not detected with ESI because of their poor or very low response. Figures of merit and validation studies were executed and special attention was devoted to matrix-effects evaluation, because a sample preparation procedure is not involved. No matrix effects were observed, and the repeatability was excellent even after several weeks of operation. Products composition was investigated in full scan mode to determine the presence of unknown or not listed ingredients. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Trumorph® system: The new universal technique for the observation and analysis of the morphology of living sperm. [corrected].

PubMed

Soler, C; García-Molina, A; Contell, J; Silvestre, M A; Sancho, M

2015-07-01

Evaluation of sperm morphology is a fundamental component of semen analysis, but its real significance has been obscured by a plethora of techniques that involve fixation and staining procedures that induce artefacts. Here we describe Trumorph℗®, a new method for sperm morphology assessment that is based upon examination of wet preparations of living spermatozoa immobilized by a short 60°C shock using negative phase contrast microscopy. We have observed samples from five animals of the following species: bull, boar, goat and rabbit. In every case, all the components of the sperm head and tail were perfectly defined, including the acrosome and midpiece (in all its length, including cytoplasmic droplets). A range of morphological forms was observed, similar to those found by conventional fixed and stained preparations, but other forms were found, distinguishable only by the optics used. The ease of preparation makes it a robust method applicable for analysis of living unmodified spermatozoa in a range of situations. Subsequent studies on well-characterized samples are required to describe the morphology of potentially fertilizing spermatozoa. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of Monitors for Assessing Exposure of Military Personnel to Toxic Chemicals.

DTIC Science & Technology

2000-01-01

Residues " S ampler Preparation 7 Transfer and Analysis 7 Temperature Effects on PIMS Sampling Rate 8 Environmental Air Sampling 8 Results and...of exposure and potential toxicity to personnel. While progress has been made in improving active water and air sampling technology, such devices...streams, 3) the apparatus is also applicable for use in air sampling deployments in indoor and outdoor scenarios, and 4) the apparatus is commercially

Evaluation of specimen preparation techniques for micro-PIXE localisation of elements in hyperaccumulating plants

NASA Astrophysics Data System (ADS)

Kachenko, Anthony G.; Siegele, Rainer; Bhatia, Naveen P.; Singh, Balwant; Ionescu, Mihail

2008-04-01

Hybanthus floribundus subsp. floribundus, a rare Australian Ni-hyperaccumulating shrub and Pityrogramma calomelanos var. austroamericana, an Australian naturalized As-hyperaccumulating fern are promising species for use in phytoremediation of contaminated sites. Micro-proton-induced X-ray emission (μ-PIXE) spectroscopy was used to map the elemental distribution of the accumulated metal(loid)s, Ca and K in leaf or pinnule tissues of the two plant species. Samples were prepared by two contrasting specimen preparation techniques: freeze-substitution in tetrahydrofuran (THF) and freeze-drying. The specimens were analysed to compare the suitability of each technique in preserving (i) the spatial elemental distribution and (ii) the tissue structure of the specimens. Further, the μ-PIXE results were compared with concentration of elements in the bulk tissue obtained by ICP-AES analysis. In H. floribundus subsp. floribundus, μ-PIXE analysis revealed Ni, Ca and K concentrations in freeze-dried leaf tissues were at par with bulk tissue concentrations. Elemental distribution maps illustrated that Ni was preferentially localised in the adaxial epidermal tissues (1% DW) and least concentration was found in spongy mesophyll tissues (0.53% DW). Conversely, elemental distribution maps of THF freeze-substituted tissues indicated significantly lower Ni, Ca and K concentrations than freeze-dried specimens and bulk tissue concentrations. Moreover, Ni concentrations were uniform across the whole specimen and no localisation was observed. In P. calomelanos var. austroamericana freeze-dried pinnule tissues, μ-PIXE revealed statistically similar As, Ca and K concentrations as compared to bulk tissue concentrations. Elemental distribution maps showed that As localisation was relatively uniform across the whole specimen. Once again, THF freeze-substituted tissues revealed a significant loss of As compared to freeze-dried specimens and the concentrations obtained by bulk tissue analysis. The results demonstrate that freeze-drying is a suitable sample preparation technique to study elemental distribution of ions in H. floribundus and P. calomelanos plant tissues using μ-PIXE spectroscopy. Furthermore, cellular structure was preserved in samples prepared using this technique.

Photolysis of RDX in Aqueous Solution, With and Without Ozone

DTIC Science & Technology

1979-02-09

and compared with a standard prepared from the same TNT solution and an accurately weighed RDX sample in acetone ( 40 ppm). The GC analysis of the...aqueous carbon-14 RDX agreed with the weight ( 40 ppm). A stock solution of carbon-12 RDX in tap water was prepared by stirring an excess of RDX in 2 liters...as volatiles 8.4% " i10 7, 77 Y 40 ’ NSWC/WOL TR 78-175 Chemical Analysis of Acidified Reaction Mixture Nitrate ion: 4.91 x 10- M Ammonia: 2.5 x 10 -4

Ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry based chemical profiling approach for the holistic quality control of complex Kang-Jing formula preparations.

PubMed

Yang, Xiao-Huan; Cheng, Xiao-Lan; Qin, Bing; Cai, Zhuo-Ya; Cai, Xiong; Liu, Shao; Wang, Qi; Qin, Yong

2016-05-30

The Kang-Jing (KJ) formula is a compound preparation made from 12 kinds of herbs. So far, four different methods (M1-M4) have been documented for KJ preparation, but the influence of preparation methods on the holistic quality of KJ have remained unknown. In this study, a strategy was proposed to investigate the influence of different preparation methods on the holistic quality of KJ using ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry (UHPLC-QTOF-MS/MS) based chemical profiling. A total of 101 compounds mainly belonging to flavonoids, tanshinones, monoterpene glycosides, triterpenoid saponins, alkaloids, phenolic acids and volatile oils, were identified. Among these compounds, glaucine was detected only in M3/M4 samples, while two dehydrocorydaline isomers merely detected in M2/M3/M4 samples. Tetrahydrocolumbamine, ethylic lithospermic acid, salvianolic acid E and rosmarimic acid were only detected in M1/M3/M4 samples. In the subsequent quantitative analysis, 12 major compounds were determined by UHPLC-MS/MS. The proposed method was validated with respect to linearity, accuracy, precision and recovery. It was found that the contents of marker compounds varied significantly in samples prepared by different methods. These results demonstrated that preparation method does significantly affect the holistic quality of KJ. UHPLC-QTOF-MS/MS based chemical profiling approach is efficient and reliable for comprehensive quality evaluation of KJ. Collectively, this study provide the chemical evidence for revealing the material basis of KJ, and establish a simple and accurate chemical profiling method for its quality control. Copyright © 2016 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Egorov, Oleg; O'Hara, Matthew J.; Grate, Jay W.

An automated fluidic instrument is described that rapidly determines the total 99Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the 99Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of 99Tc. We developed amore » preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of 99Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.« less

Capabilities of Direct Sample Introduction - Comprehensive Two-Dimensional Gas Chromatgraphy-Time-of-Flight Mass Spectrometry to Analyze Organic Chemicals of Interest in Fish Oils

USDA-ARS?s Scientific Manuscript database

Most analytical methods for persistent organic pollutants (POPs) focus on targeted analytes. Therefore, analysis of multiple classes of POPs typically entails several sample preparations, fractionations, and injections, whereas other chemicals of possible interest are neglected. To analyze a wider...

Associations among School Characteristics and Foodservice Practices in a Nationally Representative Sample of United States Schools

ERIC Educational Resources Information Center

Thomson, Jessica L.; Tussing-Humphreys, Lisa M.; Martin, Corby K.; LeBlanc, Monique M.; Onufrak, Stephen J.

2012-01-01

Objective: Determine school characteristics associated with healthy/unhealthy food service offerings or healthy food preparation practices. Design: Secondary analysis of cross-sectional data. Setting: Nationally representative sample of public and private elementary, middle, and high schools. Participants: Data from the 2006 School Health Policies…

Analysis of Whiskey by Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography/Mass Spectrometry: An Upper Division Analytical Chemistry Experiment Guided by Green Chemistry

ERIC Educational Resources Information Center

Owens, Janel E.; Zimmerman, Laura B.; Gardner, Michael A.; Lowe, Luis E.

2016-01-01

Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in…

Towards reconstruction of overlapping fingerprints using plasma spectroscopy

NASA Astrophysics Data System (ADS)

Yang, Jun-Ho; Choi, Soo-Jin; Yoh, Jack J.

2017-08-01

Chemical analysis is commonly used in the field of forensic science where the precise discrimination of primary evidence is of significant importance. Laser-Induced Breakdown Spectroscopy (LIBS) exceeds other spectroscopic methods in terms of the time required for pre- and post-sample preparation, the insensitivity to sample phase state be it solid, liquid, or gas, and the detection of two-dimensional spectral mapping from real time point measurements. In this research, fingerprint samples on various surface materials are considered in the chemical detection and reconstruction of fingerprints using the two-dimensional LIBS technique. Strong and distinct intensities of specific wavelengths represent visible ink, natural secretion of sweat, and contaminants from the environment, all of which can be present in latent fingerprints. The particular aim of the work presented here is to enhance the precision of the two-dimensional recreation of the fingerprints present on metal, plastic, and artificially prepared soil surface using LIBS with principal component analysis. By applying a distinct wavelength discrimination for two overlapping fingerprint samples, separation into two non-identical chemical fingerprints was successfully performed.

Sources of variability in collection and preparation of paint and lead-coating samples.

PubMed

Harper, S L; Gutknecht, W F

2001-06-01

Chronic exposure of children to lead (Pb) can result in permanent physiological impairment. Since surfaces coated with lead-containing paints and varnishes are potential sources of exposure, it is extremely important that reliable methods for sampling and analysis be available. The sources of variability in the collection and preparation of samples were investigated to improve the performance and comparability of methods and to ensure that data generated will be adequate for its intended use. Paint samples of varying sizes (areas and masses) were collected at different locations across a variety of surfaces including metal, plaster, concrete, and wood. A variety of grinding techniques were compared. Manual mortar and pestle grinding for at least 1.5 min and mechanized grinding techniques were found to generate similar homogenous particle size distributions required for aliquots as small as 0.10 g. When 342 samples were evaluated for sample weight loss during mortar and pestle grinding, 4% had 20% or greater loss with a high of 41%. Homogenization and sub-sampling steps were found to be the principal sources of variability related to the size of the sample collected. Analysis of samples from different locations on apparently identical surfaces were found to vary by more than a factor of two both in Pb concentration (mg cm-2 or %) and areal coating density (g cm-2). Analyses of substrates were performed to determine the Pb remaining after coating removal. Levels as high as 1% Pb were found in some substrate samples, corresponding to more than 35 mg cm-2 Pb. In conclusion, these sources of variability must be considered in development and/or application of any sampling and analysis methodologies.

Chemical profile and anti-leishmanial activity of three Ecuadorian propolis samples from Quito, Guayaquil and Cotacachi regions.

PubMed

Cuesta-Rubio, Osmany; Campo Fernández, Mercedes; Márquez Hernández, Ingrid; Jaramillo, Carmita Gladys Jaramillo; González, Victor Hugo; Montes De Oca Porto, Rodny; Marrero Delange, David; Monzote Fidalgo, Lianet; Piccinelli, Anna Lisa; Campone, Luca; Rastrelli, Luca

2017-07-01

Three propolis samples were collected from different regions of Ecuador (Quito, Guayaquil and Cotacachi) and their methanolic extracts were prepared. Preliminary information supplied by TLC and NMR data, allowed us to define two main types of propolis: Cotacachi propoli sample (CPS), rich in flavonoids and Quito and Guayaquil samples (QPS and GPS) containing triterpenic alcohols and acetyl triterpenes as the main constituents. Two different approaches based on RP-HPLC preparative procedure and NMR structural determination (CPS) and GC-MS analysis (QPS and GPS) were successfully used for the chemical characterization of their major compounds. All three propolis extracts were able to inhibit Leishmania amazonensis growth but propolis sample rich in flavonoids was the most active (IC 50 =17.1±1.7μg/mL). In the literature this is the first study on propolis from Ecuador. Copyright © 2017. Published by Elsevier B.V.

Rugged large volume injection for sensitive capillary LC-MS environmental monitoring

NASA Astrophysics Data System (ADS)

Roberg-Larsen, Hanne; Abele, Silvija; Demir, Deniz; Dzabijeva, Diana; Amundsen, Sunniva F.; Wilson, Steven R.; Bartkevics, Vadims; Lundanes, Elsa

2017-08-01

A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g. injection of 100 non-filtrated water samples would did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 µm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for environmental water samples was demonstrated with various pharmaceutical products, which had detection limits (LOD) in the 0.05 - 12.5 ng/L range. Between-day and within-day repeatability of selected analytes were < 20% RSD.

USE OF NATURAL WATERS AS U. S. GEOLOGICAL SURVEY REFERENCE SAMPLES.

USGS Publications Warehouse

Janzer, Victor J.

1985-01-01

The U. S. Geological Survey conducts research and collects hydrologic data relating to the Nation's water resources. Seven types of natural matrix reference water samples are prepared for use in the Survey's quality assurance program. These include samples containing major constituents, trace metals, nutrients, herbicides, insecticides, trace metals in a water and suspended-sediment mixture, and precipitation (snowmelt). To prepare these reference samples, natural water is collected in plastic drums and the sediment is allowed to settle. The water is then filtered, selected constituents are added, and if necessary the water is acidified and sterilized by ultraviolet irradiation before bottling in plastic or glass. These reference samples are distributed twice yearly to more than 100 laboratories for chemical analysis. The most probable values for each constituent are determined by evaluating the data submitted by the laboratories using statistical techniques recommended by ASTM.

The counting of native blood cells by digital microscopy

NASA Astrophysics Data System (ADS)

Torbin, S. O.; Doubrovski, V. A.; Zabenkov, I. V.; Tsareva, O. E.

2017-03-01

An algorithm for photographic images processing of blood samples in its native state was developed to determine the concentration of erythrocytes, leukocytes and platelets without individual separate preparation of cells' samples. Special "photo templates" were suggested to use in order to identify red blood cells. The effect of "highlighting" of leukocytes, which was found by authors, was used to increase the accuracy of this type of cells counting. Finally to raise the resolution of platelets from leukocytes the areas of their photo images were used, but not their sizes. It is shown that the accuracy of cells counting for native blood samples may be comparable with the accuracy of similar studies for smears. At the same time the proposed native blood analysis simplifies greatly the procedure of sample preparation in comparison to smear, permits to move from the detection of blood cells ratio to the determination of their concentrations in the sample.

Parker THM Analyzer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hassan, Kazi; Siegal, Michael; Mowry, Curtis

This easy-to-operate, cost-effective, tabletop purge-and-trap gas chromatograph ensures safe drinking water and monitors disinfection by-product formation at water utilities in real-time without sample preparation or off-site analysis.

Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

PubMed

Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

2017-12-01

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO 3 , HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL -1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg -1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg -1 which were below the limits of 300, 200 and 100µgkg -1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Fluid control structures in microfluidic devices

DOEpatents

Mathies, Richard A.; Grover, William H.; Skelley, Alison; Lagally, Eric; Liu, Chung N.

2008-11-04

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Fluid control structures in microfluidic devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mathies, Richard A.; Grover, William H.; Skelley, Alison

2017-05-09

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Fluid control structures in microfluidic devices

NASA Technical Reports Server (NTRS)

Skelley, Alison (Inventor); Mathies, Richard A. (Inventor); Lagally, Eric (Inventor); Grover, William H. (Inventor); Liu, Chung N. (Inventor)

2008-01-01

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

NASA Astrophysics Data System (ADS)

Hu, Li; Zhao, Nanjing; Liu, Wenqing; Meng, Deshuo; Fang, Li; Wang, Yin; Yu, Yang; Ma, Mingjun

2015-08-01

Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection. supported by National Natural Science Foundation of China (No. 60908018), National High Technology Research and Development Program of China (No. 2013AA065502) and Anhui Province Outstanding Youth Science Fund of China (No. 1108085J19)

Tank 241-B-108, cores 172 and 173 analytical results for the final report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nuzum, J.L., Fluoro Daniel Hanford

1997-03-04

The Data Summary Table (Table 3) included in this report compiles analytical results in compliance with all applicable DQOS. Liquid subsamples that were prepared for analysis by an acid adjustment of the direct subsample are indicated by a `D` in the A column in Table 3. Solid subsamples that were prepared for analysis by performing a fusion digest are indicated by an `F` in the A column in Table 3. Solid subsamples that were prepared for analysis by performing a water digest are indicated by a I.wl. or an `I` in the A column of Table 3. Due to poormore » precision and accuracy in original analysis of both Lower Half Segment 2 of Core 173 and the core composite of Core 173, fusion and water digests were performed for a second time. Precision and accuracy improved with the repreparation of Core 173 Composite. Analyses with the repreparation of Lower Half Segment 2 of Core 173 did not show improvement and suggest sample heterogeneity. Results from both preparations are included in Table 3.« less

Quality control evaluation of Keshamasi, Keshanjana and Keshamasi eye ointment.

PubMed

Dhiman, Kartar Singh; Shukla, Vinay J; Bhalodia, Nayan R; Sharma, Vinay R

2014-01-01

Keshanjana (collyrium) is a well known Ayurvedic preparation prepared out of Keshamasi (ash prepared by scalp hairs) mixed with Goghrita (cow's ghee). This medicine is indicated for the treatment of Shushkakshipaka (dry eye syndrome) in the classical literature of Ayurveda; hence, it was under taken for standardization and clinical evaluation in an extra-mural research project from Central Council for Research in Ayurvedic Sciences, Department of AYUSH, New Delhi. To develop standard quality parameters for the Keshamasi, Keshanjana and Keshamasi ointment. Scalp hairs of male and females collected from saloons were converted to classical Masi Kalpana and mixed with cow ghee and petrolatum in the ratio of 1:5 to prepare the Keshanjana and Keshamasi ointment respectively. Standard Operation Procedure (SOP) were adopted and recorded accordingly. The raw material, furnished products and plain Goghrita were subjected for quality control parameters i.e., physico-chemical evaluation, anti-microbial study, particle size analysis, heavy metal analysis through inductive couple plasma spectroscopy with high performance thin layer liquid chromatography fingerprints. Rancidity was negative in all the samples, indicating that the physico-chemical parameters are in acceptable range. Lead and zinc were present in most of the samples; while all samples are were free from microbial contamination. As no standards are available to compare the results of the current study, the observations cannot be compared. Thus the profile generated in the current study can be considered as standard to refer in future studies.

Quality control evaluation of Keshamasi, Keshanjana and Keshamasi eye ointment

PubMed Central

Dhiman, Kartar Singh; Shukla, Vinay J.; Bhalodia, Nayan R.; Sharma, Vinay R.

2014-01-01

Background: Keshanjana (collyrium) is a well known Ayurvedic preparation prepared out of Keshamasi (ash prepared by scalp hairs) mixed with Goghrita (cow's ghee). This medicine is indicated for the treatment of Shushkakshipaka (dry eye syndrome) in the classical literature of Ayurveda; hence, it was under taken for standardization and clinical evaluation in an extra-mural research project from Central Council for Research in Ayurvedic Sciences, Department of AYUSH, New Delhi. Aim: To develop standard quality parameters for the Keshamasi, Keshanjana and Keshamasi ointment. Materials and Methods: Scalp hairs of male and females collected from saloons were converted to classical Masi Kalpana and mixed with cow ghee and petrolatum in the ratio of 1:5 to prepare the Keshanjana and Keshamasi ointment respectively. Standard Operation Procedure (SOP) were adopted and recorded accordingly. The raw material, furnished products and plain Goghrita were subjected for quality control parameters i.e., physico-chemical evaluation, anti-microbial study, particle size analysis, heavy metal analysis through inductive couple plasma spectroscopy with high performance thin layer liquid chromatography fingerprints. Results: Rancidity was negative in all the samples, indicating that the physico-chemical parameters are in acceptable range. Lead and zinc were present in most of the samples; while all samples are were free from microbial contamination. Conclusion: As no standards are available to compare the results of the current study, the observations cannot be compared. Thus the profile generated in the current study can be considered as standard to refer in future studies. PMID:25364202

An accurate bacterial DNA quantification assay for HTS library preparation of human biological samples.

PubMed

Seashols-Williams, Sarah; Green, Raquel; Wohlfahrt, Denise; Brand, Angela; Tan-Torres, Antonio Limjuco; Nogales, Francy; Brooks, J Paul; Singh, Baneshwar

2018-05-17

Sequencing and classification of microbial taxa within forensically relevant biological fluids has the potential for applications in the forensic science and biomedical fields. The quantity of bacterial DNA from human samples is currently estimated based on quantity of total DNA isolated. This method can miscalculate bacterial DNA quantity due to the mixed nature of the sample, and consequently library preparation is often unreliable. We developed an assay that can accurately and specifically quantify bacterial DNA within a mixed sample for reliable 16S ribosomal DNA (16S rDNA) library preparation and high throughput sequencing (HTS). A qPCR method was optimized using universal 16S rDNA primers, and a commercially available bacterial community DNA standard was used to develop a precise standard curve. Following qPCR optimization, 16S rDNA libraries from saliva, vaginal and menstrual secretions, urine, and fecal matter were amplified and evaluated at various DNA concentrations; successful HTS data were generated with as low as 20 pg of bacterial DNA. Changes in bacterial DNA quantity did not impact observed relative abundances of major bacterial taxa, but relative abundance changes of minor taxa were observed. Accurate quantification of microbial DNA resulted in consistent, successful library preparations for HTS analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrical field-induced extraction and separation techniques: promising trends in analytical chemistry--a review.

PubMed

Yamini, Yadollah; Seidi, Shahram; Rezazadeh, Maryam

2014-03-03

Sample preparation is an important issue in analytical chemistry, and is often a bottleneck in chemical analysis. So, the major incentive for the recent research has been to attain faster, simpler, less expensive, and more environmentally friendly sample preparation methods. The use of auxiliary energies, such as heat, ultrasound, and microwave, is one of the strategies that have been employed in sample preparation to reach the above purposes. Application of electrical driving force is the current state-of-the-art, which presents new possibilities for simplifying and shortening the sample preparation process as well as enhancing its selectivity. The electrical driving force has scarcely been utilized in comparison with other auxiliary energies. In this review, the different roles of electrical driving force (as a powerful auxiliary energy) in various extraction techniques, including liquid-, solid-, and membrane-based methods, have been taken into consideration. Also, the references have been made available, relevant to the developments in separation techniques and Lab-on-a-Chip (LOC) systems. All aspects of electrical driving force in extraction and separation methods are too specific to be treated in this contribution. However, the main aim of this review is to provide a brief knowledge about the different fields of analytical chemistry, with an emphasis on the latest efforts put into the electrically assisted membrane-based sample preparation systems. The advantages and disadvantages of these approaches as well as the new achievements in these areas have been discussed, which might be helpful for further progress in the future. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of preparation methods and doping on the structural and tunable emissions of CdS

NASA Astrophysics Data System (ADS)

Mohamed, Mohamed Bakr; Abdel-Kader, M. H.; Alhazime, Ali A.; Almarashi, Jamal Q. M.

2018-03-01

Fe, Mn and Mg doped CdS samples were prepared by thermolysis method in air and under flow of nitrogen. Structural, compositional and optical properties of the prepared samples were investigated using x-ray powder diffraction (XRD), scanning electron microscope (SEM/EDS mapping), Fourier transform infrared red (FTIR), UV-vis absorption and photoluminescence (PL) spectroscopes. Rietveld refinement of x-ray data showed that all the undoped and doped CdS samples prepared in air and under flow of nitrogen have both cubic and hexagonal structures. The percentages of hexagonal and cubic phases for all prepared samples were determined. The crystallite size increased for CdS prepared under flow of N2 compared with the sample prepared in air. The energy gap of all the samples was calculated using UV data. The intensity of PL emission changed according to the method of preparation and the kind of doping elements. PL emission revealed a blue shift for CdS prepared in air compared with CdS prepared under flow of nitrogen; also all doped samples showed a red shift of PL spectra compared with undoped samples. Undoped and doped CdS with Fe and Mg samples emitted violet and blue sub-spectra. Mn doped CdS prepared in air revealed violet, blue and yellow sub-spectra, while the sample prepared under flow of N2 emitted violet, blue and green sub-spectra.

Effect of chlorine in clay-mineral specimens prepared on silver metal-membrane mounts for X-ray powder diffraction analysis

USGS Publications Warehouse

Poppe, L.J.; Commeau, J.A.; Pense, G.M.

1989-01-01

Silver metal-membrane filters are commonly used as substrates in the preparation of oriented clay-mineral specimens for X-ray powder diffraction (XRD). They are relatively unaffected by organic solvent treatments and specimens can be prepared rapidly. The filter mounts are adaptable to automatic sample changers, have few discrete reflections at higher 20 angles, and, because of the high atomic number of silver, produce a relatively low overall background compared with other membrane filters, such as cellulose (Poppe and Hathaway, 1979). The silver metal-membrane filters, however, present some problems after heat treatment if either the filters or the samples contain significant amounts of chlorine. At elevated temperature, the chloride ions react with the silver substrate to form crystalline compounds. These compounds change the mass-absorption coefficient of the sample, reducing peak intensities and areas and, therefore, complicating the semiquantitative estimation of clay minerals. A simple procedure that eliminates most of the chloride from a sample and the silver metal-membrane substrate is presented here.

Immuno-magnetic beads-based extraction-capillary zone electrophoresis-deep UV laser-induced fluorescence analysis of erythropoietin.

PubMed

Wang, Heye; Dou, Peng; Lü, Chenchen; Liu, Zhen

2012-07-13

Erythropoietin (EPO) is an important glycoprotein hormone. Recombinant human EPO (rhEPO) is an important therapeutic drug and can be also used as doping reagent in sports. The analysis of EPO glycoforms in pharmaceutical and sports areas greatly challenges analytical scientists from several aspects, among which sensitive detection and effective and facile sample preparation are two essential issues. Herein, we investigated new possibilities for these two aspects. Deep UV laser-induced fluorescence detection (deep UV-LIF) was established to detect the intrinsic fluorescence of EPO while an immuno-magnetic beads-based extraction (IMBE) was developed to specifically extract EPO glycoforms. Combined with capillary zone electrophoresis (CZE), CZE-deep UV-LIF allows high resolution glycoform profiling with improved sensitivity. The detection sensitivity was improved by one order of magnitude as compared with UV absorbance detection. An additional advantage is that the original glycoform distribution can be completely preserved because no fluorescent labeling is needed. By combining IMBE with CZE-deep UV-LIF, the overall detection sensitivity was 1.5 × 10⁻⁸ mol/L, which was enhanced by two orders of magnitude relative to conventional CZE with UV absorbance detection. It is applicable to the analysis of pharmaceutical preparations of EPO, but the sensitivity is insufficient for the anti-doping analysis of EPO in blood and urine. IMBE can be straightforward and effective approach for sample preparation. However, antibodies with high specificity were the key for application to urine samples because some urinary proteins can severely interfere the immuno-extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

Light scattering and transmission measurement using digital imaging for online analysis of constituents in milk

NASA Astrophysics Data System (ADS)

Jain, Pranay; Sarma, Sanjay E.

2015-05-01

Milk is an emulsion of fat globules and casein micelles dispersed in an aqueous medium with dissolved lactose, whey proteins and minerals. Quantification of constituents in milk is important in various stages of the dairy supply chain for proper process control and quality assurance. In field-level applications, spectrophotometric analysis is an economical option due to the low-cost of silicon photodetectors, sensitive to UV/Vis radiation with wavelengths between 300 - 1100 nm. Both absorption and scattering are witnessed as incident UV/Vis radiation interacts with dissolved and dispersed constituents in milk. These effects can in turn be used to characterize the chemical and physical composition of a milk sample. However, in order to simplify analysis, most existing instrument require dilution of samples to avoid effects of multiple scattering. The sample preparation steps are usually expensive, prone to human errors and unsuitable for field-level and online analysis. This paper introduces a novel digital imaging based method of online spectrophotometric measurements on raw milk without any sample preparation. Multiple LEDs of different emission spectra are used as discrete light sources and a digital CMOS camera is used as an image sensor. The extinction characteristic of samples is derived from captured images. The dependence of multiple scattering on power of incident radiation is exploited to quantify scattering. The method has been validated with experiments for response with varying fat concentrations and fat globule sizes. Despite of the presence of multiple scattering, the method is able to unequivocally quantify extinction of incident radiation and relate it to the fat concentrations and globule sizes of samples.

Metabolomic analysis using porcine skin: a pilot study of analytical techniques.

PubMed

Wu, Julie; Fiehn, Oliver; Armstrong, April W

2014-06-15

Metabolic byproducts serve as indicators of the chemical processes and can provide valuable information on pathogenesis by measuring the amplified output. Standardized techniques for metabolome extraction of skin samples serve as a critical foundation to this field but have not been developed. We sought to determine the optimal cell lysage techniques for skin sample preparation and to compare GC-TOF-MS and UHPLC-QTOF-MS for metabolomic analysis. Using porcine skin samples, we pulverized the skin via various combinations of mechanical techniques for cell lysage. After extraction, the samples were subjected to GC-TOF-MS and/or UHPLC-QTOF-MS. Signal intensities from GC-TOF-MS analysis showed that ultrasonication (2.7x107) was most effective for cell lysage when compared to mortar-and-pestle (2.6x107), ball mill followed by ultrasonication (1.6x107), mortar-and-pestle followed by ultrasonication (1.4x107), and homogenization (trial 1: 8.4x106; trial 2: 1.6x107). Due to the similar signal intensities, ultrasonication and mortar-and-pestle were applied to additional samples and subjected to GC-TOF-MS and UHPLC-QTOF-MS. Ultrasonication yielded greater signal intensities than mortar-and-pestle for 92% of detected metabolites following GC-TOF-MS and for 68% of detected metabolites following UHPLC-QTOF-MS. Overall, ultrasonication is the preferred method for efficient cell lysage of skin tissue for both metabolomic platforms. With standardized sample preparation, metabolomic analysis of skin can serve as a powerful tool in elucidating underlying biological processes in dermatological conditions.

Colorimetric assay for urinary track infection disease diagnostic on flexible substrate

NASA Astrophysics Data System (ADS)

Safavieh, Mohammadali; Ahmed, Minhaz Uddin; Zourob, Mohammed

2012-10-01

We are presenting cassette as a novel point of care diagnostic device. This device is easy to use, low cost to prepare, high throughput and can analyze several samples at the same time. We first, demonstrate the preparation method of the device. Then, fabrication of the flexible substrate has been presented. The device has been used for detection of the real sample of E.coli bacteria following by colorimetric detection. We have shown that we could detect 30 cfu/ml bacteria and 100 fg/μl of Staphylococous aureus DNA in 1 hr using LAMP amplification technique. This device will be helpful in hospitals and doctor's office for analysis of several patients' samples at the same time.

RNA-Seq workflow: gene-level exploratory analysis and differential expression

PubMed Central

Love, Michael I.; Anders, Simon; Kim, Vladislav; Huber, Wolfgang

2015-01-01

Here we walk through an end-to-end gene-level RNA-Seq differential expression workflow using Bioconductor packages. We will start from the FASTQ files, show how these were aligned to the reference genome, and prepare a count matrix which tallies the number of RNA-seq reads/fragments within each gene for each sample. We will perform exploratory data analysis (EDA) for quality assessment and to explore the relationship between samples, perform differential gene expression analysis, and visually explore the results. PMID:26674615

Analysis of Explosives in Soil Using Solid Phase Microextraction and Gas Chromatography: Environmental Analysis

DTIC Science & Technology

2006-01-01

ENVIRONMENTAL ANALYSIS Analysis of Explosives in Soil Using Solid Phase Microextraction and Gas Chromatography Howard T. Mayfield Air Force Research...Abstract: Current methods for the analysis of explosives in soils utilize time consuming sample preparation workups and extractions. The method detection...chromatography/mass spectrometry to provide a con- venient and sensitive analysis method for explosives in soil. Keywords: Explosives, TNT, solid phase

Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

ERIC Educational Resources Information Center

Palmer, Peter T.

2011-01-01

Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

Determination of the aflatoxin AFB1 from corn by direct analysis in real time-mass spectrometry (DART-MS)

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to a high resolution mass spectrometer (MS) was used for screening of aflatoxins from a variety of surfaces and the rapid quantitative analysis of a common form of aflatoxin, AFB1, extracted from corn. Sample preparation procedure and instrument...

Determination of T-2 and HT-2 toxins from maize by direct analysis in real time mass spectrometry

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to mass spectrometry (MS) was used for the rapid quantitative analysis of T-2 toxin, and the related HT-2 toxin, extracted from corn. Sample preparation procedures and instrument parameters were optimized to obtain sensitive and accurate determi...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nieroda, Pawel; Zybala, Rafal; Wojciechowski, Krzysztof T.

The aim of the study was to develop a fast and simple method for preparation of polycrystalline Mg{sub 2}Si. For this purpose a Spark Plasma Sintering (SPS) method was used and synthesis conditions were adjusted in such a manner that no excess Mg was required. Materials were synthesized by the direct reaction of Mg and Si raw powders. To determine the phase and chemical composition, the fabricated samples were studied by X-ray diffraction and SEM microscopy coupled with EDX chemical analysis. Thermoelectric properties of samples (thermal conductivity, electrical conductivity and Seebeck coefficient) were measured all over temperature range of 300-650more » K. The analysis by the scanning thermoelectric microprobe (STM) shows that samples have uniform distribution of Seebeck coefficient with mean value of about -405 {mu}VK{sup -1} and standard deviation of 94 {mu}VK{sup -1}. Prepared materials have intrinsic band gap of 0.45 eV and thermal conductivity {lambda}= 7.5 Wm{sup -1}K{sup -1} at room temperature.« less

Development and validation of a multiclass method for the quantification of veterinary drug residues in honey and royal jelly by liquid chromatography-tandem mass spectrometry.

PubMed

Jin, Yue; Zhang, Jinzhen; Zhao, Wen; Zhang, Wenwen; Wang, Lin; Zhou, Jinhui; Li, Yi

2017-04-15

The aim of this study was to develop an analytical method for the analysis of a wide range of veterinary drugs in honey and royal jelly. A modified sample preparation procedure based on the quick, easy, cheap, effective, rugged and safe (QuEChERS) method was developed, followed by liquid chromatography tandem mass spectrometry determination. Use of the single sample preparation method for analysis of 42 veterinary drugs becomes more valuable because honey and royal jelly belong to completely different complex matrices. Another main advantage of the proposed method is its ability to identify and quantify 42 veterinary drugs with higher sensitivity than reference methods of China. This work has shown that the reported method was demonstrated to be convenient and reliable for the quick monitoring of veterinary drugs in honey and royal jelly samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Structural analysis and ferroelectric properties of Fe doped BaTiO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mishra, Ashutosh, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Mansuri, Amantulla, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Dwivedi, J. P.

2016-05-23

The polycrystalline samples of Fe doped BaTiO{sub 3} (BTO) with compositional formula BaTi{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.03, 0.04 and 0.05) were prepared by solid-state reaction route. The influence of the Fe content on the structural, vibrational and electric properties of BaTiO{sub 3} was investigated using X-ray powder diffraction (XRD), Raman spectroscopy and Polarization techniques. XRD analysis indicates the formation of single-phase tetragonal structure for all the prepared samples. Tetragonal cubic structure with space group P4mm of all samples is further approved by Rietveld refinement. Room temperature Raman spectra of pure BaTiO{sub 3} show four active modes ofmore » vibration whose intensity decreases with increasing Fe doping. Small shift in Raman modes and increment in the line width has been observed with the doping ions. The hysteresis loop is very well performed with regular sharp characteristic of ferroelectric materials.« less

Dried Blood Spot Proteomics: Surface Extraction of Endogenous Proteins Coupled with Automated Sample Preparation and Mass Spectrometry Analysis

NASA Astrophysics Data System (ADS)

Martin, Nicholas J.; Bunch, Josephine; Cooper, Helen J.

2013-08-01

Dried blood spots offer many advantages as a sample format including ease and safety of transport and handling. To date, the majority of mass spectrometry analyses of dried blood spots have focused on small molecules or hemoglobin. However, dried blood spots are a potentially rich source of protein biomarkers, an area that has been overlooked. To address this issue, we have applied an untargeted bottom-up proteomics approach to the analysis of dried blood spots. We present an automated and integrated method for extraction of endogenous proteins from the surface of dried blood spots and sample preparation via trypsin digestion by use of the Advion Biosciences Triversa Nanomate robotic platform. Liquid chromatography tandem mass spectrometry of the resulting digests enabled identification of 120 proteins from a single dried blood spot. The proteins identified cross a concentration range of four orders of magnitude. The method is evaluated and the results discussed in terms of the proteins identified and their potential use as biomarkers in screening programs.

Preparation, physicochemical characterisation and magnetic properties of Cu-Al layered double hydroxides with CO 32- and anionic surfactants with different alkyl chains in the interlayer

NASA Astrophysics Data System (ADS)

Trujillano, Raquel; Holgado, María Jesús; Pigazo, Fernando; Rives, Vicente

2006-03-01

Layered double hydroxides with the hydrotalcite-like structure, containing Cu(II) and Al(III) in the layers, and different alkyl sulphonates in the interlayer, have been prepared and characterised by powder X-ray diffraction, FT-IR spectroscopy, differential thermal analysis and thermogravimetric analysis. Their magnetic properties have been also studied. Except for the sample containing octadecanesulphonate in the interlayer, for which an excess of sulphonate exists, pure crystalline phases have been obtained in the other cases. Upon heating, combustion of the organic chain takes place at lower temperature than for the corresponding sodium salts. A two-dimensional antiferromagnetic behaviour is observed at 200 K in all samples containing intercalated sulphonate. The χT value is lower for the samples containing interlayer sulphonates (with layer-layer distances in the 21-31 Å range), than for a carbonate-containing analogue (basal spacing 7.51 Å).

A novel sample preparation method to avoid influence of embedding medium during nano-indentation

NASA Astrophysics Data System (ADS)

Meng, Yujie; Wang, Siqun; Cai, Zhiyong; Young, Timothy M.; Du, Guanben; Li, Yanjun

2013-02-01

The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of non-embedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic material during nano-indentation can modify cell-wall properties. This leads to structural and chemical changes in the cell-wall constituents, changes that may significantly alter the material properties. Further investigation was carried out to detect the influence of different vacuum times on the cell-wall mechanical properties during the embedding procedure. Interpretation of the statistical analysis revealed no linear relationships between vacuum time and the mechanical properties of cell walls. The quantitative measurements confirm that low-viscosity resin has a rapid penetration rate early in the curing process. Finally, a novel sample preparation method aimed at preventing resin diffusion into lignocellulosic cell walls was developed using a plastic film to wrap the sample before embedding. This method proved to be accessible and straightforward for many kinds of lignocellulosic material, but is especially suitable for small, soft samples.

Preparation of highly multiplexed small RNA sequencing libraries.

PubMed

Persson, Helena; Søkilde, Rolf; Pirona, Anna Chiara; Rovira, Carlos

2017-08-01

MicroRNAs (miRNAs) are ~22-nucleotide-long small non-coding RNAs that regulate the expression of protein-coding genes by base pairing to partially complementary target sites, preferentially located in the 3´ untranslated region (UTR) of target mRNAs. The expression and function of miRNAs have been extensively studied in human disease, as well as the possibility of using these molecules as biomarkers for prognostication and treatment guidance. To identify and validate miRNAs as biomarkers, their expression must be screened in large collections of patient samples. Here, we develop a scalable protocol for the rapid and economical preparation of a large number of small RNA sequencing libraries using dual indexing for multiplexing. Combined with the use of off-the-shelf reagents, more samples can be sequenced simultaneously on large-scale sequencing platforms at a considerably lower cost per sample. Sample preparation is simplified by pooling libraries prior to gel purification, which allows for the selection of a narrow size range while minimizing sample variation. A comparison with publicly available data from benchmarking of miRNA analysis platforms showed that this method captures absolute and differential expression as effectively as commercially available alternatives.

Investigation on structural properties of M-type strontium hexaferrite synthesized in presence of neem and aloe-vera plant leaves extract

NASA Astrophysics Data System (ADS)

Solanki, Neha; Jotania, Rajshree B.

2017-05-01

M-type strontium hexaferrite powder samples were synthesized using a green synthesis route with and without presence of Aloe vera and Neem leaves extract. The dry brownish precursors of strontium hexaferrite were recovered from a mixed solution of metal salts and leaves extract, heated at 100 °C. The obtained precursors were pre-heated at 500 °C for 4 hrs. followed by final heating at 950 °C for 4 hrs. in a muffle furnace to obtain SrFe12O19 hexaferrite powder. The obtained SrFe12O19 hexaferrite powder samples characterized at room temperature in order to check phase purity and structural properties. XRD analysis confirms that samples prepared without and with Aloe vera leaves extract (heated at 950 °C for 4 hrs.) show formation of α-Fe2O3 and M-phase; while the sample prepared in presence of Neem leaves extract (heated at 950 °C for 4 hrs.) show formation of mono phase of strontium hexaferrite. Lattice parameter (a) and cell volume (V) are found to increase in the samples prepared in presence of Aloe vera and Neem leaves extract.

A new comprehensive technique of catheterisation, blood sampling, sample preparation and sample analysis by means of high-pressure liquid chromatography for pharmacokinetic studies with estradiol-linked nitrosoureas and their metabolites.

PubMed

Betsch, B; Berger, M R; Spiegelhalder, B

1990-09-01

Estradiol-linked nitrosoureas are offering new perspectives in the antineoplastic chemotherapy of estradiol-receptor positive mammary carcinomas. In such a molecule estradiol has the function of a carrier which brings about a specific accumulation of the anticancer drug in estradiol-receptor containing tumor cells. However, there is only little knowledge about the pharmacokinetic behavior of this new group of anticancer agents. For that reason a new comprehensive technique of catheterisation, blood sampling, sample preparation and sample analysis with high-pressure liquid chromatography (HPLC) for preclinical pharmacokinetic studies with estradiol-linked nitrosoureas and their metabolites has been developed. N-(2-Chloroethyl)-N-nitroso-carbamoyl-L-alanine-estradiol-17-ester (CNC-alanine-estradiol-17-ester) and N-(2-chloroethyl)-N-nitroso-carbamoyl-L-alanine (CNC-alanine) were used as test compounds. The drugs were tested in female Sprague-Dawley rats with chemically induced mammary carcinomas. The laboratory animals were supplied with two catheters prior to the pharmacokinetic experiments. The blood samples were drawn from the vena cava catheter after the drug had been applied through a vena jugularis catheter. The compounds were extracted from plasma with C18 silicagel reversed phase cartridges. The clean-up technique delivered clear samples only slightly contaminated with the biological matrix. The recovery from plasma was 75 +/- 5% for the hormone-linked CNC-alanine-estradiol-17-ester and 70 +/- 5% for the unlinked CNC-alanine. The analysis was carried out by means of HPLC.(ABSTRACT TRUNCATED AT 250 WORDS)

ARC-2006-ACD06-0091-001

NASA Image and Video Library

2006-06-05

Space shuttle STS-121 FIT (Fly Immunity and Tumors) payload. Using Drosophila (fruit fly) to complete the experiments. Matt Lera doing sample preparation for post light analysis of Drosophila melanogaster (fruit fly) larva

Polysialylated N-Glycans Identified in Human Serum Through Combined Developments in Sample Preparation, Separations and Electrospray ionization-mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kronewitter, Scott R.; Marginean, Ioan; Cox, Jonathan T.

The N-glycan diversity of human serum glycoproteins, i.e. the human blood serum N-glycome, is complex due to the range of glycan structures potentially synthesizable by human glycosylation enzymes. The reported glycome, however, is limited by methods of sample preparation, available analytical platforms, e.g., based upon electrospray ionization-mass spectrometry (ESI-MS), and software tools for data analysis. In this report, several improvements have been implemented in sample preparation and analysis to extend ESI-MS glycan characterization and to provide an improved view of glycan diversity. Sample preparation improvements include acidified, microwave-accelerated, PNGase F N-glycan release, and sodium borohydride reduction were optimized to improvemore » quantitative yields and conserve the number of glycoforms detected. Two-stage desalting (during solid phase extraction and on the analytical column) increased the sensitivity by reducing analyte signal division between multiple reducing-end-forms or cation adducts. On-line separations were improved by using extended length graphitized carbon columns and adding TFA as an acid modifier to a formic acid/reversed phase gradient which provides additional resolving power and significantly improved desorption of both large and heavily sialylated glycans. To improve MS sensitivity and provide gentler ionization conditions at the source-MS interface, subambient pressure ionization with nanoelectrospray (SPIN) has been utilized. When method improvements are combined together with the Glycomics Quintavariate Informed Quantification (GlyQ-IQ) recently described1 these technologies demonstrate the ability to significantly extend glycan detection sensitivity and provide expanded glycan coverage. We demonstrate application of these advances in the context of the human serum glycome, and for which our initial observations include detection of a new class of heavily sialylated N-glycans, including polysialylated N-glycans.« less

Pressure-Assisted Chelating Extraction as a Teaching Tool in Instrumental Analysis

ERIC Educational Resources Information Center

Sadik, Omowunmi A.; Wanekaya, Adam K.; Yevgeny, Gelfand

2004-01-01

A novel instrumental-digestion technique using pressure-assisted chelating extraction (PACE), for undergraduate laboratory is reported. This procedure is used for exposing students to safe sample-preparation techniques, for correlating wet-chemical methods with modern instrumental analysis and comparing the performance of PACE with conventional…

Chlorine Analysis - Water. Training Module 5.260.2.77.

ERIC Educational Resources Information Center

Kirkwood Community Coll., Cedar Rapids, IA.

This document is an instructional module package prepared in objective form for use by an instructor familiar with the procedures for chlorine residual analysis. It includes objectives, an instructor guide, and student handouts. The module addresses the determination of combined and free residual chlorine in water supply samples using three…

Methods for Chemical Analysis of Fresh Waters.

ERIC Educational Resources Information Center

Golterman, H. L.

This manual, one of a series prepared for the guidance of research workers conducting studies as part of the International Biological Programme, contains recommended methods for the analysis of fresh water. The techniques are grouped in the following major sections: Sample Taking and Storage; Conductivity, pH, Oxidation-Reduction Potential,…

Utility of the summation chromatographic peak integration function to avoid manual reintegrations in the analysis of targeted analytes

USDA-ARS?s Scientific Manuscript database

As sample preparation and analytical techniques have improved, data handling has become the main limitation in automated high-throughput analysis of targeted chemicals in many applications. Conventional chromatographic peak integration functions rely on complex software and settings, but untrustwor...

Multiresidue analysis of pesticides in straw roughage by liquid chromatography - tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

A multiresidue analytical method using a modification of the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) sample preparation approach combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS) analysis was established and validated for the rapid determination of 69 pesti...

Carbon ions irradiation on nano- and microcrystalline CaSO4 : Dy

NASA Astrophysics Data System (ADS)

Salah, Numan

2008-08-01

Nanoparticles of CaSO4 : Dy phosphor with a particle size of around 30 nm have been prepared by the chemical co-precipitation technique. Pellet samples of the nanomaterials were irradiated by a 75 MeV C6+ ion beam at the fluence range 1 × 109-1 × 1013 ions cm-2. Thermoluminescence (TL) glow curves of the irradiated samples were recorded and studied. The microcrystalline form of this sample is also included in the study with the aim of reporting a comparative measurement. The TL analysis shows that the glow curve of the nanomaterial has two peaks at around 166 and 210 °C. These peaks are similar to those induced in the microcrystalline sample with a slight difference in their TL response. The second peak is more prominent in the case of the microcrystalline sample at low fluences, while the first one dominates in the nanostructured sample mainly at higher fluences. The TRIM code based on Monte Carlo simulation was also used for calculating some ion beam parameters. Dosimetric properties of the carbon ion beam irradiated materials show that the nanostructure material has excellent features such as a simple glow curve structure and a linear TL response over a wider range than the corresponding microcrystalline sample. These results show that the nanostructure form of CaSO4 : Dy might be useful for detecting the high doses of carbon ions used in radiotherapy. Thermal analysis of the prepared nano- and microcrystalline materials was also done in the range 50-500 °C using thermogravimetry analysis and differential thermal analysis. No phase transitions within this range of heating for both the materials are observed.

A novel platelet concentrate: titanium-prepared platelet-rich fibrin.

PubMed

Tunalı, Mustafa; Özdemir, Hakan; Küçükodacı, Zafer; Akman, Serhan; Yaprak, Emre; Toker, Hülya; Fıratlı, Erhan

2014-01-01

We developed a new product called titanium-prepared platelet-rich fibrin (T-PRF). The T-PRF method is based on the hypothesis that titanium may be more effective in activating platelets than the silica activators used with glass tubes in Chouckroun's leukocyte- and platelet-rich fibrin (L-PRF) method. In this study, we aimed to define the structural characteristics of T-PRF and compare it with L-PRF. Blood samples were collected from 10 healthy male volunteers. The blood samples were drawn using a syringe. Nine milliliters was transferred to a dry glass tube, and 9 mL was transferred to a titanium tube. Half of each clot (i.e., the blood that was clotted using T-PRF or L-PRF) was processed with a scanning electron microscope (SEM). The other half of each clot was processed for fluorescence microscopy analysis and light microscopy analysis. The T-PRF samples seemed to have a highly organized network with continuous integrity compared to the other L-PRF samples. Histomorphometric analysis showed that T-PRF fibrin network covers larger area than L-PRF fibrin network; also fibrin seemed thicker in the T-PRF samples. This is the first human study to define T-PRF as an autogenous leukocyte- and platelet-rich fibrin product. The platelet activation by titanium seems to offer some high characteristics to T-PRF.

High-performance thin-layer chromatography analysis of steviol glycosides in Stevia formulations and sugar-free food products, and benchmarking with (ultra) high-performance liquid chromatography.

PubMed

Morlock, Gertrud E; Meyer, Stephanie; Zimmermann, Benno F; Roussel, Jean-Marc

2014-07-11

A high-performance TLC (HPTLC) method was newly developed and validated for analysis of 7 steviol glycosides in 6 different types of food and Stevia formulations. After a minimized one-step sample preparation, 21 samples were developed in parallel, allowing an effective food screening. Depending on the sample application volume, the method was suited to analyze food sample concentrations in the mg/kg range. LOQs of stevioside in natural yoghurt matrix spiked at 0.02, 0.13 and 0.2% were determined by the calibration curve method to be 12ng/band (peak height). ANOVA was successfully passed to prove data homogeneity in the working range (30-600ng/band). The accuracy (recovery tolerance limit, 92-120%), repeatability (3.1-5.4%) and intermediate precision (4.0-8.4%) were determined for stevioside in milk-based matrix including sample preparation and recovery rates at 3 different concentration levels. For the first time, the recording of HPTLC-ESI-MS spectra via the TLC-MS Interface was demonstrated for rebaudioside A. HPTLC contents for rebaudioside A were compared with results of two (U)HPLC methods. The running costs and analysis time of the three different methods were discussed in detail with regard to screening of food products. Copyright © 2014 Elsevier B.V. All rights reserved.

Tunable microwave absorbing nano-material for X-band applications

NASA Astrophysics Data System (ADS)

Sadiq, Imran; Naseem, Shahzad; Ashiq, Muhammad Naeem; Khan, M. A.; Niaz, Shanawer; Rana, M. U.

2016-03-01

The effect of rare earth elements substitution in Sr1.96RE0.04Co2Fe27.80Mn0.2O46 (RE=Ce, Gd, Nd, La and Sm) X-type hexagonal ferrites prepared by using sol gel autocombustion method was studied. The XRD and FTIR analysis show the single phase of the prepared material. The lattice constants a (Å) and c (Å) varies with the additives. The particle size measured by Scherer formula for all the samples varies in the range of 54-100 nm and confirmed by the TEM analysis. The average grain size measured by SEM analysis lies in the range of 0.672-1.01 μm for all the samples. The Gd-substituted ferrite has higher value of coercivity (526.06 G) among all the samples which could be a good material for longitudinal recording media. The results also indicate that the Gd-substituted sample has maximum reflection loss of -25.2 dB at 11.878 GHz, can exhibit the best microwave absorption properties among all the substituted samples. Furthermore, the minimum value of reflection loss shifts towards the lower and higher frequencies with the substitution of rare earth elements which confirms that the microwave absorption properties can be tuned with the substitution of rare earth elements in pure ferrites. The peak value of attenuation constant at higher frequency agrees well the reflection loss data.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection.

PubMed

Alexandrou, Lydon D; Meehan, Barry J; Morrison, Paul D; Jones, Oliver A H

2017-05-15

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid-liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9-9.3 µg/L).

Optimisation and validation of a rapid and efficient microemulsion liquid chromatographic (MELC) method for the determination of paracetamol (acetaminophen) content in a suppository formulation.

PubMed

McEvoy, Eamon; Donegan, Sheila; Power, Joe; Altria, Kevin

2007-05-09

A rapid and efficient oil-in-water microemulsion liquid chromatographic method has been optimised and validated for the analysis of paracetamol in a suppository formulation. Excellent linearity, accuracy, precision and assay results were obtained. Lengthy sample pre-treatment/extraction procedures were eliminated due to the solubilising power of the microemulsion and rapid analysis times were achieved. The method was optimised to achieve rapid analysis time and relatively high peak efficiencies. A standard microemulsion composition of 33 g SDS, 66 g butan-1-ol, 8 g n-octane in 1l of 0.05% TFA modified with acetonitrile has been shown to be suitable for the rapid analysis of paracetamol in highly hydrophobic preparations under isocratic conditions. Validated assay results and overall analysis time of the optimised method was compared to British Pharmacopoeia reference methods. Sample preparation and analysis times for the MELC analysis of paracetamol in a suppository were extremely rapid compared to the reference method and similar assay results were achieved. A gradient MELC method using the same microemulsion has been optimised for the resolution of paracetamol and five of its related substances in approximately 7 min.

Fully Automated Sample Preparation for Ultrafast N-Glycosylation Analysis of Antibody Therapeutics.

PubMed

Szigeti, Marton; Lew, Clarence; Roby, Keith; Guttman, Andras

2016-04-01

There is a growing demand in the biopharmaceutical industry for high-throughput, large-scale N-glycosylation profiling of therapeutic antibodies in all phases of product development, but especially during clone selection when hundreds of samples should be analyzed in a short period of time to assure their glycosylation-based biological activity. Our group has recently developed a magnetic bead-based protocol for N-glycosylation analysis of glycoproteins to alleviate the hard-to-automate centrifugation and vacuum-centrifugation steps of the currently used protocols. Glycan release, fluorophore labeling, and cleanup were all optimized, resulting in a <4 h magnetic bead-based process with excellent yield and good repeatability. This article demonstrates the next level of this work by automating all steps of the optimized magnetic bead-based protocol from endoglycosidase digestion, through fluorophore labeling and cleanup with high-throughput sample processing in 96-well plate format, using an automated laboratory workstation. Capillary electrophoresis analysis of the fluorophore-labeled glycans was also optimized for rapid (<3 min) separation to accommodate the high-throughput processing of the automated sample preparation workflow. Ultrafast N-glycosylation analyses of several commercially relevant antibody therapeutics are also shown and compared to their biosimilar counterparts, addressing the biological significance of the differences. © 2015 Society for Laboratory Automation and Screening.

Development of a micropulverized extraction method for rapid toxicological analysis of methamphetamine in hair.

PubMed

Miyaguchi, Hajime; Kakuta, Masaya; Iwata, Yuko T; Matsuda, Hideaki; Tazawa, Hidekatsu; Kimura, Hiroko; Inoue, Hiroyuki

2007-09-07

We developed a rapid sample preparation method for the toxicological analysis of methamphetamine and amphetamine (the major metabolite of methamphetamine) in human hair by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), to facilitate fast screening and quantitation. Two milligrams of hair were mechanically micropulverized for 5 min in a 2-ml plastic tube together with 100 microl of an aqueous solvent containing 10% acetonitrile, 100 mM trifluoroacetic acid and the corresponding deuterium analogues as internal standards. The pulverizing highly disintegrated the hair components, simultaneously allowing the extraction of any drugs present in the hair. After filtering the suspension with a membrane-filter unit, the clear filtrate was directly analyzed by HPLC-MS/MS. No evaporation processes were required for sample preparation. Method optimization and validation study were carried out using real-case specimens and fortified samples in which the drugs had been artificially absorbed, respectively. Concentration ranges for quantitation were 0.040-125 and 0.040-25 ng/mg for methamphetamine and amphetamine, respectively. Real-case specimens were analyzed by the method presented here and by conventional ones to verify the applicability of our method to real-world analysis. Our method took less than 30 min for a set of chromatograms to be obtained from a washed hair sample.

Desulfurization of Cysteine-Containing Peptides Resulting from Sample Preparation for Protein Characterization by MS

PubMed Central

Wang, Zhouxi; Rejtar, Tomas; Zhou, Zhaohui Sunny; Karger, Barry L.

2010-01-01

In this paper, we have examined two cysteine modifications resulting from sample preparation for protein characterization by MS: (1) a previously observed conversion of cysteine to dehydroalanine, now found in the case of disulfide mapping and (2) a novel modification corresponding to conversion of cysteine to alanine. Using model peptides, the conversion of cysteine to dehydroalanine via β-elimination of a disulfide bond was seen to result from the conditions of typical tryptic digestion (37 °C, pH 7.0– 9.0) without disulfide reduction and alkylation.. Furthermore, the surprising conversion of cysteine to alanine was shown to occur by heating cysteine containing peptides in the presence of a phosphine (TCEP). The formation of alanine from cysteine, investigated by performing experiments in H2O or D2O, suggested a radical-based desulfurization mechanism unrelated to β-elimination. Importantly, an understanding of the mechanism and conditions favorable for cysteine desulfurization provides insight for the establishment of improved sample preparation procedures of protein analysis. PMID:20049891

Preparation and Thermoelectric Properties of IR(sub x)Co(sub 1-x)Sb(sub 2) Alloys

NASA Technical Reports Server (NTRS)

Caillat, Thierry

1995-01-01

The preparation and characterization of the binary arsenopyrite compounds CoSb2 and IrSb2 and IrxCo1-xSb2 alloys is reported. Single crystals of CoSb2 were grown by the vertical gradient freeze technique from solution rich in antimony. Polycrystalline samples of IrSb2 and IrxCo1-xSb2 alloys were prepared by hot-pressing of prereacted elemental powders. Samples were investigated by X-ray diffractometry, microprobe analysis and density measurements. It was found that a range of solid solution exist in the system IrxCo1-xSb2 for 0.1

Quantitation of Mycotoxins Using Direct Analysis in Real Time Mass Spectrometry (DART-MS).

PubMed

Busman, Mark

2018-05-01

Ambient ionization represents a new generation of MS ion sources and is used for the rapid ionization of small molecules under ambient conditions. The combination of ambient ionization and MS allows the analysis of multiple food samples with simple or no sample treatment or in conjunction with prevailing sample preparation methods. Two ambient ionization methods, desorptive electrospray ionization (DESI) and direct analysis in real time (DART) have been adapted for food safety application. Both ionization techniques provide unique advantages and capabilities. DART has been used for a variety of qualitative and quantitative applications. In particular, mycotoxin contamination of food and feed materials has been addressed by DART-MS. Applications to mycotoxin analysis by ambient ionization MS and particularly DART-MS are summarized.

[Prognostic value on recovery rates for the application of sperm preparation techniques and their evaluation in sperm function].

PubMed

Barroso, Gerardo; Chaya, Miguel; Bolaños, Rubén; Rosado, Yadira; García León, Fernando; Ibarrola, Eduardo

2005-05-01

To evaluate sperm recovery and total sperm motility in three different sperm preparation techniques (density gradient, simple washing and swim-up). A total of 290 subjects were randomly evaluated from November 2001 to March 2003. The density gradient method required Isolate (upper and lower layers). Centrifugation was performed at 400 g for 10 minutes and evaluation was done using the Makler counting chamber. The simple washing method included the use of HTF-M complemented with 7.5% of SSS, with centrifugation at 250 g, obtaining at the end 0.5 mL of the sperm sample. The swim-up method required HTF-M complemented with 7.5% of SSS, with an incubation period of 60 minutes at 37 degrees C. The demographic characteristics evaluated through their standard error, 95% ICC, and 50th percentile were similar. The application of multiple comparison tests and analysis of variance showed significant differences between the sperm preparations before and after capacitation. It was observed a superior recovery rate with the density gradient and swim-up methods; nevertheless, the samples used for the simple washing method showed a diminished sperm recovery from the original sample. Sperm preparation techniques have become very useful in male infertility treatments allowing higher sperm recovery and motility rates. The seminal parameters evaluated from the original sperm sample will determine the best sperm preparation technique in those patients who require it.

Preparation of C18 composite solid-phase microextraction fiber and its application to the determination of organochlorine pesticides in water samples.

PubMed

Li, Siyan; Lu, Chengwei; Zhu, Fang; Jiang, Ruifen; Ouyang, Gangfeng

2015-05-11

In this work, a C18 composite solid-phase microextraction (SPME) fiber was prepared with a new method and applied to the analysis of organochlorine pesticides (OCPs) in water sample. A stainless steel wire (o.d. 127 μm) was used as the substrate, and a mixture of the C18 particle (3.5 μm) and the 184 silicone was used as the coating material. During the process of fiber preparation, a section of capillary column was used to fix the mixture onto the stainless steel wire and to ensure the constant of coating thickness. The prepared fiber showed excellent thermal stability and solvent resistance. By coupling with gas chromatography-mass spectrometry (GC-MS), the fiber exhibited wide linearity (2-500 ng L(-1)) and good sensitivity for the determination of six OCPs in water samples, the OCPs tested included hexachlorobezene, trans-chlordane, cis-chlordane, o,p-DDT, p,p-DDT and mirex. Not only the extraction performance of the newly prepared fiber was more than seven times higher than those of commercial fibers, the limits of detections (LODs) (0.059-0.151 ng L(-1)) for OCPs achieved under optimized conditions were also lower than those of reported SPME methods. The fiber was successfully applied to the determination of OCPs in real water samples by using developed SPME-GC-MS method. Copyright © 2015 Elsevier B.V. All rights reserved.

Eigenvalue-eigenvector decomposition (EED) analysis of dissimilarity and covariance matrix obtained from total synchronous fluorescence spectral (TSFS) data sets of herbal preparations: Optimizing the classification approach.

PubMed

Tarai, Madhumita; Kumar, Keshav; Divya, O; Bairi, Partha; Mishra, Kishor Kumar; Mishra, Ashok Kumar

2017-09-05

The present work compares the dissimilarity and covariance based unsupervised chemometric classification approaches by taking the total synchronous fluorescence spectroscopy data sets acquired for the cumin and non-cumin based herbal preparations. The conventional decomposition method involves eigenvalue-eigenvector analysis of the covariance of the data set and finds the factors that can explain the overall major sources of variation present in the data set. The conventional approach does this irrespective of the fact that the samples belong to intrinsically different groups and hence leads to poor class separation. The present work shows that classification of such samples can be optimized by performing the eigenvalue-eigenvector decomposition on the pair-wise dissimilarity matrix. Copyright © 2017 Elsevier B.V. All rights reserved.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Hasegawa, Y.; Tsuda, H.; Mori, S.; Halbig, M. C.; Asthana, R.; Singh, M.

2017-01-01

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

The Sampling and Analysis Plan, Galena Airport and Kalakaket Creek Radio Relay Station, Alaska. Addendum

DTIC Science & Technology

1994-09-08

information deactivated during 1993. Currently, approximately 30 required in a QAPP per the U.S. Environmental caretakers are present at the facility...the total analytical cost. A subset of those Galena Airport-The current environmental samples collected and screened will be sent to an investigative...sampling report United States Environmental Protection Agency (US preparation. EPA), USAF, state, and local requirements. Ms. Sandy Smith is

Do centrally pre-prepared solutions achieve more reliable drug concentrations than solutions prepared on the ward?

PubMed

Dehmel, Carola; Braune, Stephan A; Kreymann, Georg; Baehr, Michael; Langebrake, Claudia; Hilgarth, Heike; Nierhaus, Axel; Dartsch, Dorothee C; Kluge, Stefan

2011-08-01

To compare the concentration conformity of infusion solutions manually prepared on intensive care units (ICU) with solutions from pharmacy-based, automated production. A prospective observational study conducted in a university hospital in Germany. Drug concentrations of 100 standardised infusion solutions manually prepared in the ICU and 100 matching solutions from automated production containing amiodarone, noradrenaline or hydrocortisone were measured by high-performance liquid chromatography analysis. Deviations from stated concentrations were calculated, and the quality of achieved concentration conformity of the two production methods was compared. Actual concentrations of 53% of the manually prepared and 16% of the machine-made solutions deviated by >5% above or below the stated concentration. A deviation of >10% was measured in 22% of the manually prepared samples and in 5% of samples from automated production. Of the manually prepared solutions, 15% deviated by >15% above or below the intended concentration. The mean concentration of the manually prepared solutions was 97.2% (SD 12.7%, range 45-129%) and of the machine-made solutions was 101.1% (SD 4.3%, range 90-114%) of the target concentration (p < 0.01). In this preliminary study, ward-based, manually prepared infusion solutions showed clinically relevant deviations in concentration conformity significantly more often than pharmacy-prepared, machine-made solutions. Centralised, automated preparation of standardised infusion solutions may be an effective means to reduce this type of medication error. Further confirmatory studies in larger settings and under conditions of routine automated production are required.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Rigaku ZSX Mini II (ZSX Mini II) XRF Services x-ray fluorescence (XRF) analyzer was demon-strated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the ZSX Mini II analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the ZSX Mini II analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element con