Hanford analytical sample projections FY 1998 - FY 2002

International Nuclear Information System (INIS)

Joyce, S.M.

1997-01-01

Sample projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Sample projections are categorized by radiation level, protocol, sample matrix and Program. Analyses requirements are also presented

Navigating the Benford Labyrinth: A big-data analytic protocol illustrated using the academic library context

Directory of Open Access Journals (Sweden)

Michael Halperin

2016-03-01

Full Text Available Objective: Big Data Analytics is a panoply of techniques the principal intention of which is to ferret out dimensions or factors from certain data streamed or available over the WWW. We offer a subset or “second” stage protocol of Big Data Analytics (BDA that uses these dimensional datasets as benchmarks for profiling related data. We call this Specific Context Benchmarking (SCB. Method: In effecting this benchmarking objective, we have elected to use a Digital Frequency Profiling (DFP technique based upon the work of Newcomb and Benford, who have developed a profiling benchmark based upon the Log10 function. We illustrate the various stages of the SCB protocol using the data produced by the Academic Research Libraries to enhance insights regarding the details of the operational benchmarking context and so offer generalizations needed to encourage adoption of SCB across other functional domains. Results: An illustration of the SCB protocol is offered using the recently developed Benford Practical Profile as the Conformity Benchmarking Measure. ShareWare: We have developed a Decision Support System called: SpecificContextAnalytics (SCA:DSS to create the various information sets presented in this paper. The SCA:DSS, programmed in Excel VBA, is available from the corresponding author as a free download without restriction to its use. Conclusions: We note that SCB effected using the DFPs is an enhancement not a replacement for the usual statistical and analytic techniques and fits very well in the BDA milieu.

Paper-Based Analytical Device for Zinc Ion Quantification in Water Samples with Power-Free Analyte Concentration

Directory of Open Access Journals (Sweden)

Hiroko Kudo

2017-04-01

Full Text Available Insufficient sensitivity is a general issue of colorimetric paper-based analytical devices (PADs for trace analyte detection, such as metal ions, in environmental water. This paper demonstrates the colorimetric detection of zinc ions (Zn2+ on a paper-based analytical device with an integrated analyte concentration system. Concentration of Zn2+ ions from an enlarged sample volume (1 mL has been achieved with the aid of a colorimetric Zn2+ indicator (Zincon electrostatically immobilized onto a filter paper substrate in combination with highly water-absorbent materials. Analyte concentration as well as sample pretreatment, including pH adjustment and interferent masking, has been elaborated. The resulting device enables colorimetric quantification of Zn2+ in environmental water samples (tap water, river water from a single sample application. The achieved detection limit of 0.53 μM is a significant improvement over that of a commercial colorimetric Zn2+ test paper (9.7 μM, demonstrating the efficiency of the developed analyte concentration system not requiring any equipment.

Development of analytical techniques for safeguards environmental samples at JAEA

International Nuclear Information System (INIS)

Sakurai, Satoshi; Magara, Masaaki; Usuda, Shigekazu; Watanabe, Kazuo; Esaka, Fumitaka; Hirayama, Fumio; Lee, Chi-Gyu; Yasuda, Kenichiro; Inagawa, Jun; Suzuki, Daisuke; Iguchi, Kazunari; Kokubu, Yoko S.; Miyamoto, Yutaka; Ohzu, Akira

2007-01-01

JAEA has been developing, under the auspices of the Ministry of Education, Culture, Sports, Science and Technology of Japan, analytical techniques for ultra-trace amounts of nuclear materials in environmental samples in order to contribute to the strengthened safeguards system. Development of essential techniques for bulk and particle analysis, as well as screening, of the environmental swipe samples has been established as ultra-trace analytical methods of uranium and plutonium. In January 2003, JAEA was qualified, including its quality control system, as a member of the JAEA network analytical laboratories for environmental samples. Since 2004, JAEA has conducted the analysis of domestic and the IAEA samples, through which JAEA's analytical capability has been verified and improved. In parallel, advanced techniques have been developed in order to expand the applicability to the samples of various elemental composition and impurities and to improve analytical accuracy and efficiency. This paper summarizes the trace of the technical development in environmental sample analysis at JAEA, and refers to recent trends of research and development in this field. (author)

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Turbidity sampling and analytical... § 141.22 Turbidity sampling and analytical requirements. The requirements in this section apply to... the water distribution system at least once per day, for the purposes of making turbidity measurements...

Hanford analytical sample projections FY 1996 - FY 2001. Revision 4

Energy Technology Data Exchange (ETDEWEB)

Joyce, S.M.

1997-07-02

This document summarizes the biannual Hanford sample projections for fiscal year 1997-2001. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Wastes Remediation Systems, Solid Wastes, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition to this revision, details on Laboratory scale technology (development), Sample management, and Data management activities were requested. This information will be used by the Hanford Analytical Services program and the Sample Management Working Group to assure that laboratories and resources are available and effectively utilized to meet these documented needs.

Pre-analytical and post-analytical evaluation in the era of molecular diagnosis of sexually transmitted diseases: cellularity control and internal control

Directory of Open Access Journals (Sweden)

Loria Bianchi

2014-06-01

Full Text Available Background. Increase of molecular tests performed on DNA extracted from various biological materials should not be carried out without an adequate standardization of the pre-analytical and post-analytical phase. Materials and Methods. Aim of this study was to evaluate the role of internal control (IC to standardize pre-analytical phase and the role of cellularity control (CC in the suitability evaluation of biological matrices, and their influence on false negative results. 120 cervical swabs (CS were pre-treated and extracted following 3 different protocols. Extraction performance was evaluated by amplification of: IC, added in each mix extraction; human gene HPRT1 (CC with RT-PCR to quantify sample cellularity; L1 region of HPV with SPF10 primers. 135 urine, 135 urethral swabs, 553 CS and 332 ThinPrep swabs (TP were tested for C. trachomatis (CT and U. parvum (UP with RT-PCR and for HPV by endpoint-PCR. Samples were also tested for cellularity. Results. Extraction protocol with highest average cellularity (Ac/sample showed lowest number of samples with inhibitors; highest HPV positivity was achieved by protocol with greatest Ac/PCR. CS and TP under 300.000 cells/sample showed a significant decrease of UP (P<0.01 and HPV (P<0.005 positivity. Female urine under 40.000 cells/mL were inadequate to detect UP (P<0.05. Conclusions. Our data show that IC and CC allow optimization of pre-analytical phase, with an increase of analytical quality. Cellularity/sample allows better sample adequacy evaluation, crucial to avoid false negative results, while cellularity/PCR allows better optimization of PCR amplification. Further data are required to define the optimal cut-off for result normalization.

A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index.

Science.gov (United States)

Płotka-Wasylka, J

2018-05-01

A new means for assessing analytical protocols relating to green analytical chemistry attributes has been developed. The new tool, called GAPI (Green Analytical Procedure Index), evaluates the green character of an entire analytical methodology, from sample collection to final determination, and was created using such tools as the National Environmental Methods Index (NEMI) or Analytical Eco-Scale to provide not only general but also qualitative information. In GAPI, a specific symbol with five pentagrams can be used to evaluate and quantify the environmental impact involved in each step of an analytical methodology, mainly from green through yellow to red depicting low, medium to high impact, respectively. The proposed tool was used to evaluate analytical procedures applied in the determination of biogenic amines in wine samples, and polycyclic aromatic hydrocarbon determination by EPA methods. GAPI tool not only provides an immediately perceptible perspective to the user/reader but also offers exhaustive information on evaluated procedures. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of bull trout sampling protocols

Science.gov (United States)

R. F. Thurow; J. T. Peterson; J. W. Guzevich

2001-01-01

This report describes results of research conducted in Washington in 2000 through Interagency Agreement #134100H002 between the U.S. Fish and Wildlife Service (USFWS) and the U.S. Forest Service Rocky Mountain Research Station (RMRS). The purpose of this agreement is to develop a bull trout (Salvelinus confluentus) sampling protocol by integrating...

Contemporary sample stacking in analytical electrophoresis

Czech Academy of Sciences Publication Activity Database

Šlampová, Andrea; Malá, Zdeňka; Pantůčková, Pavla; Gebauer, Petr; Boček, Petr

2013-01-01

Roč. 34, č. 1 (2013), s. 3-18 ISSN 0173-0835 R&D Projects: GA ČR GAP206/10/1219 Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

Contemporary sample stacking in analytical electrophoresis

Czech Academy of Sciences Publication Activity Database

Malá, Zdeňka; Šlampová, Andrea; Křivánková, Ludmila; Gebauer, Petr; Boček, Petr

2015-01-01

Roč. 36, č. 1 (2015), s. 15-35 ISSN 0173-0835 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.482, year: 2015

[Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

Science.gov (United States)

Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

2015-09-01

Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

Biofluid infrared spectro-diagnostics: pre-analytical considerations for clinical applications.

Science.gov (United States)

Lovergne, L; Bouzy, P; Untereiner, V; Garnotel, R; Baker, M J; Thiéfin, G; Sockalingum, G D

2016-06-23

Several proof-of-concept studies on the vibrational spectroscopy of biofluids have demonstrated that the methodology has promising potential as a clinical diagnostic tool. However, these studies also show that there is a lack of a standardised protocol in sample handling and preparation prior to spectroscopic analysis. One of the most important sources of analytical errors is the pre-analytical phase. For the technique to be translated into clinics, it is clear that a very strict protocol needs to be established for such biological samples. This study focuses on some of the aspects of the pre-analytical phase in the development of the high-throughput Fourier Transform Infrared (FTIR) spectroscopy of some of the most common biofluids such as serum, plasma and bile. Pre-analytical considerations that can impact either the samples (solvents, anti-coagulants, freeze-thaw cycles…) and/or spectroscopic analysis (sample preparation such as drying, deposit methods, volumes, substrates, operators dependence…) and consequently the quality and the reproducibility of spectral data will be discussed in this report.

[Patient identification errors and biological samples in the analytical process: Is it possible to improve patient safety?].

Science.gov (United States)

Cuadrado-Cenzual, M A; García Briñón, M; de Gracia Hills, Y; González Estecha, M; Collado Yurrita, L; de Pedro Moro, J A; Fernández Pérez, C; Arroyo Fernández, M

2015-01-01

Patient identification errors and biological samples are one of the problems with the highest risk factor in causing an adverse event in the patient. To detect and analyse the causes of patient identification errors in analytical requests (PIEAR) from emergency departments, and to develop improvement strategies. A process and protocol was designed, to be followed by all professionals involved in the requesting and performing of laboratory tests. Evaluation and monitoring indicators of PIEAR were determined, before and after the implementation of these improvement measures (years 2010-2014). A total of 316 PIEAR were detected in a total of 483,254 emergency service requests during the study period, representing a mean of 6.80/10,000 requests. Patient identification failure was the most frequent in all the 6-monthly periods assessed, with a significant difference (Perrors. However, we must continue working with this strategy, promoting a culture of safety for all the professionals involved, and trying to achieve the goal that 100% of the analytical and samples are properly identified. Copyright © 2015 SECA. Published by Elsevier Espana. All rights reserved.

Recommendations for sampling for prevention of hazards in civil defense. On analytics of chemical, biological and radioactive contaminations. Brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling; Empfehlungen fuer die Probenahme zur Gefahrenabwehr im Bevoelkerungsschutz. Zur Analytik von chemischen, biologischen und radioaktiven Kontaminationen. Kurzanleitung fuer die CBRN-Probenahme

Energy Technology Data Exchange (ETDEWEB)

Bachmann, Udo; Biederbick, Walter; Derakshani, Nahid (and others)

2010-07-01

The recommendation for sampling for prevention of hazards in civil defense is describing the analytics of chemical, biological and radioactive contaminations and includes detail information on the sampling, protocol preparation and documentation procedures. The volume includes a separate brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling.

Evaluation of storage and filtration protocols for alpine/subalpine lake water quality samples

Science.gov (United States)

John L. Korfmacher; Robert C. Musselman

2007-01-01

Many government agencies and other organizations sample natural alpine and subalpine surface waters using varying protocols for sample storage and filtration. Simplification of protocols would be beneficial if it could be shown that sample quality is unaffected. In this study, samples collected from low ionic strength waters in alpine and subalpine lake inlets...

Analytical laboratory and mobile sampling platform

International Nuclear Information System (INIS)

Stetzenbach, K.; Smiecinski, A.

1996-01-01

This is the final report for the Analytical Laboratory and Mobile Sampling Platform project. This report contains only major findings and conclusions resulting from this project. Detailed reports of all activities performed for this project were provided to the Project Office every quarter since the beginning of the project. This report contains water chemistry data for samples collected in the Nevada section of Death Valley National Park (Triangle Area Springs), Nevada Test Site springs, Pahranagat Valley springs, Nevada Test Site wells, Spring Mountain springs and Crater Flat and Amargosa Valley wells

Recommendations for sampling for prevention of hazards in civil defense. On analytics of chemical, biological and radioactive contaminations. 2. ed.; Empfehlungen fuer die Probenahme zur Gefahrenabwehr im Bevoelkerungsschutz. Zur Analytik von chemischen, biologischen und radioaktiven Kontaminationen

Energy Technology Data Exchange (ETDEWEB)

Bachmann, Udo; Derakshani, Nahid; Drobig, Matthias; Koenig, Mario; Mentfewitz, Joachim; Prast, Hartmut; Uelpenich, Gerhard; Vidmayer, Marc; Wilbert, Stefan; Wolf, Manfred

2016-07-01

The recommendations for sampling for prevention of hazards in civil defense (analytics of chemical, biological and radioactive contaminations) cover the following topics: Requirements for sampling, description of the materials (chemical, biological and radioactive contaminated materials), decontamination, sample transport and protocol documents.

Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

Science.gov (United States)

Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

2014-07-01

Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

Urine sample collection protocols for bioassay samples

Energy Technology Data Exchange (ETDEWEB)

MacLellan, J.A.; McFadden, K.M.

1992-11-01

In vitro radiobioassay analyses are used to measure the amount of radioactive material excreted by personnel exposed to the potential intake of radioactive material. The analytical results are then used with various metabolic models to estimate the amount of radioactive material in the subject`s body and the original intake of radioactive material. Proper application of these metabolic models requires knowledge of the excretion period. It is normal practice to design the bioassay program based on a 24-hour excretion sample. The Hanford bioassay program simulates a total 24-hour urine excretion sample with urine collection periods lasting from one-half hour before retiring to one-half hour after rising on two consecutive days. Urine passed during the specified periods is collected in three 1-L bottles. Because the daily excretion volume given in Publication 23 of the International Commission on Radiological Protection (ICRP 1975, p. 354) for Reference Man is 1.4 L, it was proposed to use only two 1-L bottles as a cost-saving measure. This raised the broader question of what should be the design capacity of a 24-hour urine sample kit.

Urine sample collection protocols for bioassay samples

Energy Technology Data Exchange (ETDEWEB)

MacLellan, J.A.; McFadden, K.M.

1992-11-01

In vitro radiobioassay analyses are used to measure the amount of radioactive material excreted by personnel exposed to the potential intake of radioactive material. The analytical results are then used with various metabolic models to estimate the amount of radioactive material in the subject's body and the original intake of radioactive material. Proper application of these metabolic models requires knowledge of the excretion period. It is normal practice to design the bioassay program based on a 24-hour excretion sample. The Hanford bioassay program simulates a total 24-hour urine excretion sample with urine collection periods lasting from one-half hour before retiring to one-half hour after rising on two consecutive days. Urine passed during the specified periods is collected in three 1-L bottles. Because the daily excretion volume given in Publication 23 of the International Commission on Radiological Protection (ICRP 1975, p. 354) for Reference Man is 1.4 L, it was proposed to use only two 1-L bottles as a cost-saving measure. This raised the broader question of what should be the design capacity of a 24-hour urine sample kit.

Sources of pre-analytical variations in yield of DNA extracted from blood samples: analysis of 50,000 DNA samples in EPIC.

Directory of Open Access Journals (Sweden)

Elodie Caboux

Full Text Available The European Prospective Investigation into Cancer and nutrition (EPIC is a long-term, multi-centric prospective study in Europe investigating the relationships between cancer and nutrition. This study has served as a basis for a number of Genome-Wide Association Studies (GWAS and other types of genetic analyses. Over a period of 5 years, 52,256 EPIC DNA samples have been extracted using an automated DNA extraction platform. Here we have evaluated the pre-analytical factors affecting DNA yield, including anthropometric, epidemiological and technical factors such as center of subject recruitment, age, gender, body-mass index, disease case or control status, tobacco consumption, number of aliquots of buffy coat used for DNA extraction, extraction machine or procedure, DNA quantification method, degree of haemolysis and variations in the timing of sample processing. We show that the largest significant variations in DNA yield were observed with degree of haemolysis and with center of subject recruitment. Age, gender, body-mass index, cancer case or control status and tobacco consumption also significantly impacted DNA yield. Feedback from laboratories which have analyzed DNA with different SNP genotyping technologies demonstrate that the vast majority of samples (approximately 88% performed adequately in different types of assays. To our knowledge this study is the largest to date to evaluate the sources of pre-analytical variations in DNA extracted from peripheral leucocytes. The results provide a strong evidence-based rationale for standardized recommendations on blood collection and processing protocols for large-scale genetic studies.

Waste minimization in analytical chemistry through innovative sample preparation techniques

International Nuclear Information System (INIS)

Smith, L. L.

1998-01-01

Because toxic solvents and other hazardous materials are commonly used in analytical methods, characterization procedures result in significant and costly amount of waste. We are developing alternative analytical methods in the radiological and organic areas to reduce the volume or form of the hazardous waste produced during sample analysis. For the radiological area, we have examined high-pressure, closed-vessel microwave digestion as a way to minimize waste from sample preparation operations. Heated solutions of strong mineral acids can be avoided for sample digestion by using the microwave approach. Because reactivity increases with pressure, we examined the use of less hazardous solvents to leach selected contaminants from soil for subsequent analysis. We demonstrated the feasibility of this approach by extracting plutonium from a NET reference material using citric and tartaric acids with microwave digestion. Analytical results were comparable to traditional digestion methods, while hazardous waste was reduced by a factor often. We also evaluated the suitability of other natural acids, determined the extraction performance on a wider variety of soil types, and examined the extraction efficiency of other contaminants. For the organic area, we examined ways to minimize the wastes associated with the determination of polychlorinated biphenyls (PCBs) in environmental samples. Conventional methods for analyzing semivolatile organic compounds are labor intensive and require copious amounts of hazardous solvents. For soil and sediment samples, we have a method to analyze PCBs that is based on microscale extraction using benign solvents (e.g., water or hexane). The extraction is performed at elevated temperatures in stainless steel cells containing the sample and solvent. Gas chromatography-mass spectrometry (GC/MS) was used to quantitate the analytes in the isolated extract. More recently, we developed a method utilizing solid-phase microextraction (SPME) for natural

Analytical characterization of high-level mixed wastes using multiple sample preparation treatments

International Nuclear Information System (INIS)

King, A.G.; Baldwin, D.L.; Urie, M.W.; McKinley, S.G.

1994-01-01

The Analytical Chemistry Laboratory at the Pacific Northwest Laboratory in Richland, Washington, is actively involved in performing analytical characterization of high-level mixed waste from Hanford's single shell and double shell tank characterization programs. A full suite of analyses is typically performed on homogenized tank core samples. These analytical techniques include inductively-coupled plasma-atomic emission spectroscopy, total organic carbon methods and radiochemistry methods, as well as many others, all requiring some type of remote sample-preparation treatment to solubilize the tank sludge material for analysis. Most of these analytical methods typically use a single sample-preparation treatment, inherently providing elemental information only. To better understand and interpret tank chemistry and assist in identifying chemical compounds, selected analytical methods are performed using multiple sample-preparation treatments. The sample preparation treatments used at Pacific Northwest Laboratory for this work with high-level mixed waste include caustic fusion, acid digestion, and water leach. The type of information available by comparing results from different sample-prep treatments includes evidence for the presence of refractory compounds, acid-soluble compounds, or water-soluble compounds. Problems unique to the analysis of Hanford tank wastes are discussed. Selected results from the Hanford single shell ferrocyanide tank, 241-C-109, are presented, and the resulting conclusions are discussed

Analytical approach to cross-layer protocol optimization in wireless sensor networks

Science.gov (United States)

Hortos, William S.

2008-04-01

In the distributed operations of route discovery and maintenance, strong interaction occurs across mobile ad hoc network (MANET) protocol layers. Quality of service (QoS) requirements of multimedia service classes must be satisfied by the cross-layer protocol, along with minimization of the distributed power consumption at nodes and along routes to battery-limited energy constraints. In previous work by the author, cross-layer interactions in the MANET protocol are modeled in terms of a set of concatenated design parameters and associated resource levels by multivariate point processes (MVPPs). Determination of the "best" cross-layer design is carried out using the optimal control of martingale representations of the MVPPs. In contrast to the competitive interaction among nodes in a MANET for multimedia services using limited resources, the interaction among the nodes of a wireless sensor network (WSN) is distributed and collaborative, based on the processing of data from a variety of sensors at nodes to satisfy common mission objectives. Sensor data originates at the nodes at the periphery of the WSN, is successively transported to other nodes for aggregation based on information-theoretic measures of correlation and ultimately sent as information to one or more destination (decision) nodes. The "multimedia services" in the MANET model are replaced by multiple types of sensors, e.g., audio, seismic, imaging, thermal, etc., at the nodes; the QoS metrics associated with MANETs become those associated with the quality of fused information flow, i.e., throughput, delay, packet error rate, data correlation, etc. Significantly, the essential analytical approach to MANET cross-layer optimization, now based on the MVPPs for discrete random events occurring in the WSN, can be applied to develop the stochastic characteristics and optimality conditions for cross-layer designs of sensor network protocols. Functional dependencies of WSN performance metrics are described in

A multigear protocol for sampling crayfish assemblages in Gulf of Mexico coastal streams

Science.gov (United States)

William R. Budnick; William E. Kelso; Susan B. Adams; Michael D. Kaller

2018-01-01

Identifying an effective protocol for sampling crayfish in streams that vary in habitat and physical/chemical characteristics has proven problematic. We evaluated an active, combined-gear (backpack electrofishing and dipnetting) sampling protocol in 20 Coastal Plain streams in Louisiana. Using generalized linear models and rarefaction curves, we evaluated environmental...

Identification of clinical biomarkers for pre-analytical quality control of blood samples.

Science.gov (United States)

Kang, Hyun Ju; Jeon, Soon Young; Park, Jae-Sun; Yun, Ji Young; Kil, Han Na; Hong, Won Kyung; Lee, Mee-Hee; Kim, Jun-Woo; Jeon, Jae-Pil; Han, Bok Ghee

2013-04-01

Pre-analytical conditions are key factors in maintaining the high quality of biospecimens. They are necessary for accurate reproducibility of experiments in the field of biomarker discovery as well as achieving optimal specificity of laboratory tests for clinical diagnosis. In research at the National Biobank of Korea, we evaluated the impact of pre-analytical conditions on the stability of biobanked blood samples by measuring biochemical analytes commonly used in clinical laboratory tests. We measured 10 routine laboratory analytes in serum and plasma samples from healthy donors (n = 50) with a chemistry autoanalyzer (Hitachi 7600-110). The analyte measurements were made at different time courses based on delay of blood fractionation, freezing delay of fractionated serum and plasma samples, and at different cycles (0, 1, 3, 6, 9) of freeze-thawing. Statistically significant changes from the reference sample mean were determined using the repeated-measures ANOVA and the significant change limit (SCL). The serum levels of GGT and LDH were changed significantly depending on both the time interval between blood collection and fractionation and the time interval between fractionation and freezing of serum and plasma samples. The glucose level was most sensitive only to the elapsed time between blood collection and centrifugation for blood fractionation. Based on these findings, a simple formula (glucose decrease by 1.387 mg/dL per hour) was derived to estimate the length of time delay after blood collection. In addition, AST, BUN, GGT, and LDH showed sensitive responses to repeated freeze-thaw cycles of serum and plasma samples. These results suggest that GGT and LDH measurements can be used as quality control markers for certain pre-analytical conditions (eg, delayed processing or repeated freeze-thawing) of blood samples which are either directly used in the laboratory tests or stored for future research in the biobank.

The perils of straying from protocol: sampling bias and interviewer effects.

Directory of Open Access Journals (Sweden)

Carrie J Ngongo

Full Text Available Fidelity to research protocol is critical. In a contingent valuation study in an informal urban settlement in Nairobi, Kenya, participants responded differently to the three trained interviewers. Interviewer effects were present during the survey pilot, then magnified at the start of the main survey after a seemingly slight adaptation of the survey sampling protocol allowed interviewers to speak with the "closest neighbor" in the event that no one was home at a selected household. This slight degree of interviewer choice led to inferred sampling bias. Multinomial logistic regression and post-estimation tests revealed that the three interviewers' samples differed significantly from one another according to six demographic characteristics. The two female interviewers were 2.8 and 7.7 times less likely to talk with respondents of low socio-economic status than the male interviewer. Systematic error renders it impossible to determine which of the survey responses might be "correct." This experience demonstrates why researchers must take care to strictly follow sampling protocols, consistently train interviewers, and monitor responses by interview to ensure similarity between interviewers' groups and produce unbiased estimates of the parameters of interest.

Sampling and analyte enrichment strategies for ambient mass spectrometry.

Science.gov (United States)

Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

2018-01-01

Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

Science.gov (United States)

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the

Lead Sampling Protocols: Why So Many and What Do They Tell You?

Science.gov (United States)

Sampling protocols can be broadly categorized based on their intended purpose of 1) Pb regulatory compliance/corrosion control efficacy, 2) Pb plumbing source determination or Pb type identification, and 3) Pb exposure assessment. Choosing the appropriate protocol is crucial to p...

The Gas Sampling Interval Effect on V˙O2peak Is Independent of Exercise Protocol.

Science.gov (United States)

Scheadler, Cory M; Garver, Matthew J; Hanson, Nicholas J

2017-09-01

There is a plethora of gas sampling intervals available during cardiopulmonary exercise testing to measure peak oxygen consumption (V˙O2peak). Different intervals can lead to altered V˙O2peak. Whether differences are affected by the exercise protocol or subject sample is not clear. The purpose of this investigation was to determine whether V˙O2peak differed because of the manipulation of sampling intervals and whether differences were independent of the protocol and subject sample. The first subject sample (24 ± 3 yr; V˙O2peak via 15-breath moving averages: 56.2 ± 6.8 mL·kg·min) completed the Bruce and the self-paced V˙O2max protocols. The second subject sample (21.9 ± 2.7 yr; V˙O2peak via 15-breath moving averages: 54.2 ± 8.0 mL·kg·min) completed the Bruce and the modified Astrand protocols. V˙O2peak was identified using five sampling intervals: 15-s block averages, 30-s block averages, 15-breath block averages, 15-breath moving averages, and 30-s block averages aligned to the end of exercise. Differences in V˙O2peak between intervals were determined using repeated-measures ANOVAs. The influence of subject sample on the sampling effect was determined using independent t-tests. There was a significant main effect of sampling interval on V˙O2peak (first sample Bruce and self-paced V˙O2max P sample Bruce and modified Astrand P sampling intervals followed a similar pattern for each protocol and subject sample, with 15-breath moving average presenting the highest V˙O2peak. The effect of manipulating gas sampling intervals on V˙O2peak appears to be protocol and sample independent. These findings highlight our recommendation that the clinical and scientific community request and report the sampling interval whenever metabolic data are presented. The standardization of reporting would assist in the comparison of V˙O2peak.

Green sample preparation for liquid chromatography and capillary electrophoresis of anionic and cationic analytes.

Science.gov (United States)

Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

2015-04-21

A sample preparation device for the simultaneous enrichment and separation of cationic and anionic analytes was designed and implemented in an eight-channel configuration. The device is based on the use of an electric field to transfer the analytes from a large volume of sample into small volumes of electrolyte that was suspended into two glass micropipettes using a conductive hydrogel. This simple, economical, fast, and green (no organic solvent required) sample preparation scheme was evaluated using cationic and anionic herbicides as test analytes in water. The analytical figures of merit and ecological aspects were evaluated against the state-of-the-art sample preparation, solid-phase extraction. A drastic reduction in both sample preparation time (94% faster) and resources (99% less consumables used) was observed. Finally, the technique in combination with high-performance liquid chromatography and capillary electrophoresis was applied to analysis of quaternary ammonium and phenoxypropionic acid herbicides in fortified river water as well as drinking water (at levels relevant to Australian guidelines). The presented sustainable sample preparation approach could easily be applied to other charged analytes or adopted by other laboratories.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS

NARCIS (Netherlands)

Lou, X.; Waal, de B.F.M.; Milroy, L.G.; Dongen, van J.L.J.

2015-01-01

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

Analytical Methodology for the Determination of Radium Isotopes in Environmental Samples

International Nuclear Information System (INIS)

2010-01-01

Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is an extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004, the environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Measurements of radium isotopes are important for radiological and environmental protection, geochemical and geochronological investigations, hydrology, etc. The suite of isotopes creates and stimulates continuing interest in the development of new methods for determination of radium in various media. In this publication, the four most routinely used analytical methods for radium determination in biological and environmental samples, i.e. alpha spectrometry, gamma spectrometry, liquid scintillation spectrometry and mass spectrometry, are reviewed

A modified FASP protocol for high-throughput preparation of protein samples for mass spectrometry.

Directory of Open Access Journals (Sweden)

Jeremy Potriquet

Full Text Available To facilitate high-throughput proteomic analyses we have developed a modified FASP protocol which improves the rate at which protein samples can be processed prior to mass spectrometry. Adapting the original FASP protocol to a 96-well format necessitates extended spin times for buffer exchange due to the low centrifugation speeds tolerated by these devices. However, by using 96-well plates with a more robust polyethersulfone molecular weight cutoff membrane, instead of the cellulose membranes typically used in these devices, we could use isopropanol as a wetting agent, decreasing spin times required for buffer exchange from an hour to 30 minutes. In a typical work flow used in our laboratory this equates to a reduction of 3 hours per plate, providing processing times similar to FASP for the processing of up to 96 samples per plate. To test whether our modified protocol produced similar results to FASP and other FASP-like protocols we compared the performance of our modified protocol to the original FASP and the more recently described eFASP and MStern-blot. We show that all FASP-like methods, including our modified protocol, display similar performance in terms of proteins identified and reproducibility. Our results show that our modified FASP protocol is an efficient method for the high-throughput processing of protein samples for mass spectral analysis.

OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

Directory of Open Access Journals (Sweden)

Maja Vrkljan

2004-12-01

Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

Quality assurance in the pre-analytical phase of human urine samples by (1)H NMR spectroscopy.

Science.gov (United States)

Budde, Kathrin; Gök, Ömer-Necmi; Pietzner, Maik; Meisinger, Christine; Leitzmann, Michael; Nauck, Matthias; Köttgen, Anna; Friedrich, Nele

2016-01-01

Metabolomic approaches investigate changes in metabolite profiles, which may reflect changes in metabolic pathways and provide information correlated with a specific biological process or pathophysiology. High-resolution (1)H NMR spectroscopy is used to identify metabolites in biofluids and tissue samples qualitatively and quantitatively. This pre-analytical study evaluated the effects of storage time and temperature on (1)H NMR spectra from human urine in two settings. Firstly, to evaluate short time effects probably due to acute delay in sample handling and secondly, the effect of prolonged storage up to one month to find markers of sample miss-handling. A number of statistical procedures were used to assess the differences between samples stored under different conditions, including Projection to Latent Structure Discriminant Analysis (PLS-DA), non-parametric testing as well as mixed effect linear regression analysis. The results indicate that human urine samples can be stored at 10 °C for 24 h or at -80 °C for 1 month, as no relevant changes in (1)H NMR fingerprints were observed during these time periods and temperature conditions. However, some metabolites most likely of microbial origin showed alterations during prolonged storage but without facilitating classification. In conclusion, the presented protocol for urine sample handling and semi-automatic metabolite quantification is suitable for large-scale epidemiological studies. Copyright © 2015 Elsevier Inc. All rights reserved.

[Sampling, storage and transport of biological materials collected from living and deceased subjects for determination of concentration levels of ethyl alcohol and similarly acting substances. A proposal of updating the blood and urine sampling protocol].

Science.gov (United States)

Wiergowski, Marek; Reguła, Krystyna; Pieśniak, Dorota; Galer-Tatarowicz, Katarzyna; Szpiech, Beata; Jankowski, Zbigniew

2007-01-01

The present paper emphasizes the most common mistakes committed at the beginning of an analytical procedure. To shorten the time and decrease the cost of determinations of substances with similar to alcohol activity, it is postulated to introduce mass-scale screening analysis of saliva collected from a living subject at the site of the event, with all positive results confirmed in blood or urine samples. If no saliva sample is collected for toxicology, a urine sample, allowing for a stat fast screening analysis, and a blood sample, to confirm the result, should be ensured. Inappropriate storage of a blood sample in the tube without a preservative can cause sample spilling and its irretrievable loss. The authors propose updating the "Blood/urine sampling protocol", with the updated version to be introduced into practice following consultations and revisions.

A Robust PCR Protocol for HIV Drug Resistance Testing on Low-Level Viremia Samples

Directory of Open Access Journals (Sweden)

Shivani Gupta

2017-01-01

Full Text Available The prevalence of drug resistance (DR mutations in people with HIV-1 infection, particularly those with low-level viremia (LLV, supports the need to improve the sensitivity of amplification methods for HIV DR genotyping in order to optimize antiretroviral regimen and facilitate HIV-1 DR surveillance and relevant research. Here we report on a fully validated PCR-based protocol that achieves consistent amplification of the protease (PR and reverse transcriptase (RT regions of HIV-1 pol gene across many HIV-1 subtypes from LLV plasma samples. HIV-spiked plasma samples from the External Quality Assurance Program Oversight Laboratory (EQAPOL, covering various HIV-1 subtypes, as well as clinical specimens were used to optimize and validate the protocol. Our results demonstrate that this protocol has a broad HIV-1 subtype coverage and viral load span with high sensitivity and reproducibility. Moreover, the protocol is robust even when plasma sample volumes are limited, the HIV viral load is unknown, and/or the HIV subtype is undetermined. Thus, the protocol is applicable for the initial amplification of the HIV-1 PR and RT genes required for subsequent genotypic DR assays.

A simplified field protocol for genetic sampling of birds using buccal swabs

Science.gov (United States)

Vilstrup, Julia T.; Mullins, Thomas D.; Miller, Mark P.; McDearman, Will; Walters, Jeffrey R.; Haig, Susan M.

2018-01-01

DNA sampling is an essential prerequisite for conducting population genetic studies. For many years, blood sampling has been the preferred method for obtaining DNA in birds because of their nucleated red blood cells. Nonetheless, use of buccal swabs has been gaining favor because they are less invasive yet still yield adequate amounts of DNA for amplifying mitochondrial and nuclear markers; however, buccal swab protocols often include steps (e.g., extended air-drying and storage under frozen conditions) not easily adapted to field settings. Furthermore, commercial extraction kits and swabs for buccal sampling can be expensive for large population studies. We therefore developed an efficient, cost-effective, and field-friendly protocol for sampling wild birds after comparing DNA yield among 3 inexpensive buccal swab types (2 with foam tips and 1 with a cotton tip). Extraction and amplification success was high (100% and 97.2% respectively) using inexpensive generic swabs. We found foam-tipped swabs provided higher DNA yields than cotton-tipped swabs. We further determined that omitting a drying step and storing swabs in Longmire buffer increased efficiency in the field while still yielding sufficient amounts of DNA for detailed population genetic studies using mitochondrial and nuclear markers. This new field protocol allows time- and cost-effective DNA sampling of juveniles or small-bodied birds for which drawing blood may cause excessive stress to birds and technicians alike.

Analytical study on the determination of boron in environmental water samples

International Nuclear Information System (INIS)

Lopez, F.J.; Gimenez, E.; Hernandez, F.

1993-01-01

An analytical study on the determination of boron in environmental water samples was carried out. The curcumin and carmine standard methods were compared with the most recent Azomethine-H method in order to evaluate their analytical characteristics and feasibility for the analysis of boron in water samples. Analyses of synthetic water, ground water, sea water and waste water samples were carried out and a statistical evaluation of the results was made. The Azomethine-H method was found to be the most sensitive (detection limit 0.02 mg l -1 ) and selective (no interference of commonly occurring ions in water was observed), showing also the best precision (relative standard deviation lower than 4%). Moreover, it gave good results for all types of samples analyzed. The accuracy of this method was tested by the addition of known amounts of standard solutions to different types of water samples. The slopes of standard additions and direct calibration graphs were similar and recoveries of added boron ranged from 99 to 107%. (orig.)

Discrepancies in sample size calculations and data analyses reported in randomised trials: comparison of publications with protocols

DEFF Research Database (Denmark)

Chan, A.W.; Hrobjartsson, A.; Jorgensen, K.J.

2008-01-01

OBJECTIVE: To evaluate how often sample size calculations and methods of statistical analysis are pre-specified or changed in randomised trials. DESIGN: Retrospective cohort study. Data source Protocols and journal publications of published randomised parallel group trials initially approved...... in 1994-5 by the scientific-ethics committees for Copenhagen and Frederiksberg, Denmark (n=70). MAIN OUTCOME MEASURE: Proportion of protocols and publications that did not provide key information about sample size calculations and statistical methods; proportion of trials with discrepancies between...... of handling missing data was described in 16 protocols and 49 publications. 39/49 protocols and 42/43 publications reported the statistical test used to analyse primary outcome measures. Unacknowledged discrepancies between protocols and publications were found for sample size calculations (18/34 trials...

Quantification of theobromine and caffeine in saliva, plasma and urine via liquid chromatography-tandem mass spectrometry: a single analytical protocol applicable to cocoa intervention studies.

Science.gov (United States)

Ptolemy, Adam S; Tzioumis, Emma; Thomke, Arjun; Rifai, Sami; Kellogg, Mark

2010-02-01

Targeted analyses of clinically relevant metabolites in human biofluids often require extensive sample preparation (e.g., desalting, protein removal and/or preconcentration) prior to quantitation. In this report, a single ultra-centrifugation based sample pretreatment combined with a designed liquid chromatography-tandem mass spectrometry (LC-MS/MS) protocol provides selective quantification of 3,7-dimethylxanthine (theobromine) and 1,3,7-trimethylxanthine (caffeine) in human saliva, plasma and urine samples. The optimized chromatography permitted elution of both analytes within 1.3 min of the applied gradient. Positive-mode electrospray ionization and a triple quadruple MS/MS instrument operated in multiple reaction mode were used for detection. (13)C(3) isotopically labeled caffeine was included as an internal standard to improve accuracy and precision. Implementing a 20-fold dilution of the isolated low MW biofluid fraction prior to injection effectively minimized the deleterious contributions of all three matrices to quantitation. The assay was linear over a 160-fold concentration range from 2.5 to 400 micromol L(-1) for both theobromine (average R(2) 0.9968) and caffeine (average R(2) 0.9997) respectively. Analyte peak area variations for 2.5 micromol L(-1) caffeine and theobromine in saliva, plasma and urine ranged from 5 and 10% (intra-day, N=10) to 9 and 13% (inter-day, N=25) respectively. The intra- and inter-day precision of theobromine and caffeine elution times were 3 and theobromine ranged from 114 to 118% and 99 to 105% at concentration levels of 10 and 300 micromol L(-1). This validated protocol also permitted the relative saliva, plasma and urine distribution of both theobromine and caffeine to be quantified following a cocoa intervention. 2009 Elsevier B.V. All rights reserved.

Metal-organic frameworks for analytical chemistry: from sample collection to chromatographic separation.

Science.gov (United States)

Gu, Zhi-Yuan; Yang, Cheng-Xiong; Chang, Na; Yan, Xiu-Ping

2012-05-15

In modern analytical chemistry researchers pursue novel materials to meet analytical challenges such as improvements in sensitivity, selectivity, and detection limit. Metal-organic frameworks (MOFs) are an emerging class of microporous materials, and their unusual properties such as high surface area, good thermal stability, uniform structured nanoscale cavities, and the availability of in-pore functionality and outer-surface modification are attractive for diverse analytical applications. This Account summarizes our research on the analytical applications of MOFs ranging from sampling to chromatographic separation. MOFs have been either directly used or engineered to meet the demands of various analytical applications. Bulk MOFs with microsized crystals are convenient sorbents for direct application to in-field sampling and solid-phase extraction. Quartz tubes packed with MOF-5 have shown excellent stability, adsorption efficiency, and reproducibility for in-field sampling and trapping of atmospheric formaldehyde. The 2D copper(II) isonicotinate packed microcolumn has demonstrated large enhancement factors and good shape- and size-selectivity when applied to on-line solid-phase extraction of polycyclic aromatic hydrocarbons in water samples. We have explored the molecular sieving effect of MOFs for the efficient enrichment of peptides with simultaneous exclusion of proteins from biological fluids. These results show promise for the future of MOFs in peptidomics research. Moreover, nanosized MOFs and engineered thin films of MOFs are promising materials as novel coatings for solid-phase microextraction. We have developed an in situ hydrothermal growth approach to fabricate thin films of MOF-199 on etched stainless steel wire for solid-phase microextraction of volatile benzene homologues with large enhancement factors and wide linearity. Their high thermal stability and easy-to-engineer nanocrystals make MOFs attractive as new stationary phases to fabricate MOF

Determination of 237Np in environmental and nuclear samples: A review of the analytical method

International Nuclear Information System (INIS)

Thakur, P.; Mulholland, G.P.

2012-01-01

A number of analytical methods has been developed and used for the determination of neptunium in environmental and nuclear fuel samples using alpha, ICP–MS spectrometry, and other analytical techniques. This review summarizes and discusses development of the radiochemical procedures for separation of neptunium (Np), since the beginning of the nuclear industry, followed by a more detailed discussion on recent trends in the separation of neptunium. This article also highlights the progress in analytical methods and issues associated with the determination of neptunium in environmental samples. - Highlights: ► Determination of Np in environmental and nuclear samples is reviewed. ► Various analytical methods used for the determination of Np are listed. ► Progress and issues associated with the determination of Np are discussed.

Pre-analytical sample quality: metabolite ratios as an intrinsic marker for prolonged room temperature exposure of serum samples.

Directory of Open Access Journals (Sweden)

Gabriele Anton

Full Text Available Advances in the "omics" field bring about the need for a high number of good quality samples. Many omics studies take advantage of biobanked samples to meet this need. Most of the laboratory errors occur in the pre-analytical phase. Therefore evidence-based standard operating procedures for the pre-analytical phase as well as markers to distinguish between 'good' and 'bad' quality samples taking into account the desired downstream analysis are urgently needed. We studied concentration changes of metabolites in serum samples due to pre-storage handling conditions as well as due to repeated freeze-thaw cycles. We collected fasting serum samples and subjected aliquots to up to four freeze-thaw cycles and to pre-storage handling delays of 12, 24 and 36 hours at room temperature (RT and on wet and dry ice. For each treated aliquot, we quantified 127 metabolites through a targeted metabolomics approach. We found a clear signature of degradation in samples kept at RT. Storage on wet ice led to less pronounced concentration changes. 24 metabolites showed significant concentration changes at RT. In 22 of these, changes were already visible after only 12 hours of storage delay. Especially pronounced were increases in lysophosphatidylcholines and decreases in phosphatidylcholines. We showed that the ratio between the concentrations of these molecule classes could serve as a measure to distinguish between 'good' and 'bad' quality samples in our study. In contrast, we found quite stable metabolite concentrations during up to four freeze-thaw cycles. We concluded that pre-analytical RT handling of serum samples should be strictly avoided and serum samples should always be handled on wet ice or in cooling devices after centrifugation. Moreover, serum samples should be frozen at or below -80°C as soon as possible after centrifugation.

Analytical characterization using surface-enhanced Raman scattering (SERS) and microfluidic sampling

International Nuclear Information System (INIS)

Wang, Chao; Yu, Chenxu

2015-01-01

With the rapid development of analytical techniques, it has become much easier to detect chemical and biological analytes, even at very low detection limits. In recent years, techniques based on vibrational spectroscopy, such as surface enhanced Raman spectroscopy (SERS), have been developed for non-destructive detection of pathogenic microorganisms. SERS is a highly sensitive analytical tool that can be used to characterize chemical and biological analytes interacting with SERS-active substrates. However, it has always been a challenge to obtain consistent and reproducible SERS spectroscopic results at complicated experimental conditions. Microfluidics, a tool for highly precise manipulation of small volume liquid samples, can be used to overcome the major drawbacks of SERS-based techniques. High reproducibility of SERS measurement could be obtained in continuous flow generated inside microfluidic devices. This article provides a thorough review of the principles, concepts and methods of SERS-microfluidic platforms, and the applications of such platforms in trace analysis of chemical and biological analytes. (topical review)

Robowell: An automated process for monitoring ground water quality using established sampling protocols

Science.gov (United States)

Granato, G.E.; Smith, K.P.

1999-01-01

Robowell is an automated process for monitoring selected ground water quality properties and constituents by pumping a well or multilevel sampler. Robowell was developed and tested to provide a cost-effective monitoring system that meets protocols expected for manual sampling. The process uses commercially available electronics, instrumentation, and hardware, so it can be configured to monitor ground water quality using the equipment, purge protocol, and monitoring well design most appropriate for the monitoring site and the contaminants of interest. A Robowell prototype was installed on a sewage treatment plant infiltration bed that overlies a well-studied unconfined sand and gravel aquifer at the Massachusetts Military Reservation, Cape Cod, Massachusetts, during a time when two distinct plumes of constituents were released. The prototype was operated from May 10 to November 13, 1996, and quality-assurance/quality-control measurements demonstrated that the data obtained by the automated method was equivalent to data obtained by manual sampling methods using the same sampling protocols. Water level, specific conductance, pH, water temperature, dissolved oxygen, and dissolved ammonium were monitored by the prototype as the wells were purged according to U.S Geological Survey (USGS) ground water sampling protocols. Remote access to the data record, via phone modem communications, indicated the arrival of each plume over a few days and the subsequent geochemical reactions over the following weeks. Real-time availability of the monitoring record provided the information needed to initiate manual sampling efforts in response to changes in measured ground water quality, which proved the method and characterized the screened portion of the plume in detail through time. The methods and the case study described are presented to document the process for future use.

Analytical simulation of RBS spectra of nanowire samples

Energy Technology Data Exchange (ETDEWEB)

Barradas, Nuno P., E-mail: nunoni@ctn.ist.utl.pt [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); García Núñez, C. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Redondo-Cubero, A. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Centro de Micro-Análisis de Materiales, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Shen, G.; Kung, P. [Department of Electrical and Computer Engineering, The University of Alabama, AL 35487 (United States); Pau, J.L. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain)

2016-03-15

Almost all, if not all, general purpose codes for analysis of Ion Beam Analysis data have been originally developed to handle laterally homogeneous samples only. This is the case of RUMP, NDF, SIMNRA, and even of the Monte Carlo code Corteo. General-purpose codes usually include only limited support for lateral inhomogeneity. In this work, we show analytical simulations of samples that consist of a layer of parallel oriented nanowires on a substrate, using a model implemented in NDF. We apply the code to real samples, made of vertical ZnO nanowires on a sapphire substrate. Two configurations of the nanowires were studied: 40 nm diameter, 4.1 μm height, 3.5% surface coverage; and 55 nm diameter, 1.1 μm height, 42% surface coverage. We discuss the accuracy and limits of applicability of the analysis.

Reducing the sampling periods required in protocols for establishing ammonia emissions from pig fattening buildings using measurements and modelling

NARCIS (Netherlands)

Mosquera Losada, J.; Ogink, N.W.M.

2011-01-01

Ammonia (NH(3)) emission factors for animal housing systems in the Netherlands are based on measurements using standardised measurement protocols. Both the original Green Label (GL) protocol and the newly developed multi-site sampling protocol are based on year-round sampling periods. The objective

A rapid and efficient DNA extraction protocol from fresh and frozen human blood samples.

Science.gov (United States)

Guha, Pokhraj; Das, Avishek; Dutta, Somit; Chaudhuri, Tapas Kumar

2018-01-01

Different methods available for extraction of human genomic DNA suffer from one or more drawbacks including low yield, compromised quality, cost, time consumption, use of toxic organic solvents, and many more. Herein, we aimed to develop a method to extract DNA from 500 μL of fresh or frozen human blood. Five hundred microliters of fresh and frozen human blood samples were used for standardization of the extraction procedure. Absorbance at 260 and 280 nm, respectively, (A 260 /A 280 ) were estimated to check the quality and quantity of the extracted DNA sample. Qualitative assessment of the extracted DNA was checked by Polymerase Chain reaction and double digestion of the DNA sample. Our protocol resulted in average yield of 22±2.97 μg and 20.5±3.97 μg from 500 μL of fresh and frozen blood, respectively, which were comparable to many reference protocols and kits. Besides yielding bulk amount of DNA, our protocol is rapid, economical, and avoids toxic organic solvents such as Phenol. Due to unaffected quality, the DNA is suitable for downstream applications. The protocol may also be useful for pursuing basic molecular researches in laboratories having limited funds. © 2017 Wiley Periodicals, Inc.

Development of a protocol for sampling and analysis of ballast water in Jamaica

Directory of Open Access Journals (Sweden)

Achsah A Mitchell

2014-09-01

Full Text Available The transfer of ballast by the international shipping industry has negatively impacted the environment. To design such a protocol for the area, the ballast water tanks of seven bulk cargo vessels entering a Jamaican port were sampled between January 28, 2010 and August 17, 2010. Vessels originated from five ports and used three main routes, some of which conducted ballast water exchange. Twenty-six preserved and 22 live replicate zooplankton samples were obtained. Abundance and richness were higher than at temperate ports. Exchange did not alter the biotic composition but reduced the abundance. Two of the live sample replicates, containing 31.67 and 16.75 viable individuals m-3, were non-compliant with the International Convention for the Control and Management of Ships’ Ballast Water and Sediments. Approximately 12% of the species identified in the ballast water were present in the waters nearest the port in 1995 and 11% were present in the entire bay in 2005. The protocol designed from this study can be used to aid the establishment of a ballast water management system in the Caribbean or used as a foundation for the development of further protocols.

Tank 214-AW-105, grab samples, analytical results for the final report

International Nuclear Information System (INIS)

Esch, R.A.

1997-01-01

This document is the final report for tank 241-AW-105 grab samples. Twenty grabs samples were collected from risers 10A and 15A on August 20 and 21, 1996, of which eight were designated for the K Basin sludge compatibility and mixing studies. This document presents the analytical results for the remaining twelve samples. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DO). The results for the previous sampling of this tank were reported in WHC-SD-WM-DP-149, Rev. 0, 60-Day Waste Compatibility Safety Issue and Final Results for Tank 241-A W-105, Grab Samples 5A W-95-1, 5A W-95-2 and 5A W-95-3. Three supernate samples exceeded the TOC notification limit (30,000 microg C/g dry weight). Appropriate notifications were made. No immediate notifications were required for any other analyte. The TSAP requested analyses for polychlorinated biphenyls (PCB) for all liquids and centrifuged solid subsamples. The PCB analysis of the liquid samples has been delayed and will be presented in a revision to this document

Toward greener analytical techniques for the absolute quantification of peptides in pharmaceutical and biological samples.

Science.gov (United States)

Van Eeckhaut, Ann; Mangelings, Debby

2015-09-10

Peptide-based biopharmaceuticals represent one of the fastest growing classes of new drug molecules. New reaction types included in the synthesis strategies to reduce the rapid metabolism of peptides, along with the availability of new formulation and delivery technologies, resulted in an increased marketing of peptide drug products. In this regard, the development of analytical methods for quantification of peptides in pharmaceutical and biological samples is of utmost importance. From the sample preparation step to their analysis by means of chromatographic or electrophoretic methods, many difficulties should be tackled to analyze them. Recent developments in analytical techniques emphasize more and more on the use of green analytical techniques. This review will discuss the progresses in and challenges observed during green analytical method development for the quantification of peptides in pharmaceutical and biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Use of robotic systems for radiochemical sample changing and for analytical sample preparation

International Nuclear Information System (INIS)

Delmastro, J.R.; Hartenstein, S.D.; Wade, M.A.

1989-01-01

Two uses of the Perkin-Elmer (PE) robotic system will be presented. In the first, a PE robot functions as an automatic sample changer for up to five low energy photon spectrometry (LEPS) detectors operated with a Nuclear Data ND 6700 system. The entire system, including the robot, is controlled by an IBM PC-AT using software written in compiled BASIC. Problems associated with the development of the system and modifications to the robot will be presented. In the second, an evaluation study was performed to assess the abilities of the PE robotic system for performing complex analytical sample preparation procedures. For this study, a robotic system based upon the PE robot and auxiliary devices was constructed and programmed to perform the preparation of final product samples (UO 3 ) for accountability and impurity specification analyses. These procedures require sample dissolution, dilution, and liquid-liquid extraction steps. The results of an in-depth evaluation of all system components will be presented

33 CFR 159.317 - Sampling and reporting.

Science.gov (United States)

2010-07-01

... Section 159.317 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Operations § 159.317 Sampling and reporting. (a) The owner, operator, master or other person in charge of a... protocols, including chain of custody; (2) Laboratory analytical information including methods used...

Centrifugation protocols: tests to determine optimal lithium heparin and citrate plasma sample quality.

Science.gov (United States)

Dimeski, Goce; Solano, Connie; Petroff, Mark K; Hynd, Matthew

2011-05-01

Currently, no clear guidelines exist for the most appropriate tests to determine sample quality from centrifugation protocols for plasma sample types with both lithium heparin in gel barrier tubes for biochemistry testing and citrate tubes for coagulation testing. Blood was collected from 14 participants in four lithium heparin and one serum tube with gel barrier. The plasma tubes were centrifuged at four different centrifuge settings and analysed for potassium (K(+)), lactate dehydrogenase (LD), glucose and phosphorus (Pi) at zero time, poststorage at six hours at 21 °C and six days at 2-8°C. At the same time, three citrate tubes were collected and centrifuged at three different centrifuge settings and analysed immediately for prothrombin time/international normalized ratio, activated partial thromboplastin time, derived fibrinogen and surface-activated clotting time (SACT). The biochemistry analytes indicate plasma is less stable than serum. Plasma sample quality is higher with longer centrifugation time, and much higher g force. Blood cells present in the plasma lyse with time or are damaged when transferred in the reaction vessels, causing an increase in the K(+), LD and Pi above outlined limits. The cells remain active and consume glucose even in cold storage. The SACT is the only coagulation parameter that was affected by platelets >10 × 10(9)/L in the citrate plasma. In addition to the platelet count, a limited but sensitive number of assays (K(+), LD, glucose and Pi for biochemistry, and SACT for coagulation) can be used to determine appropriate centrifuge settings to consistently obtain the highest quality lithium heparin and citrate plasma samples. The findings will aid laboratories to balance the need to provide the most accurate results in the best turnaround time.

Microsystems for liquid-liquid extraction of radionuclides in the analytical protocols

International Nuclear Information System (INIS)

Helle, Gwendolyne

2014-01-01

Radiochemical analyses are necessary to numerous steps for nuclear wastes management and for the control of the environment. An analytical protocol generally includes different steps of chemical separations which are lengthy, manual and complicated to implement because of their confinement in glove boxes and because of the hostile chemical and radiochemical media. Thus there is a huge importance to propose innovative and robust solutions to automate these steps but also to reduce the volumes of the radioactive and chemical wastes at the end of the analytical cycle. One solution consists in the miniaturization of the analyses through the use of lab-on-chip. The objective of this thesis work was to propose a rational approach to the conception of separative microsystems for the liquid-liquid extraction of radionuclides. To achieve this, the hydrodynamic behavior as well as the extraction performances have been investigated in one chip for three different chemical systems: Eu(III)-HNO 3 /DMDBTDMA, Eu(III)-AcO(H,Na)-HNO 3 /HDEHP and U(VI)-HCl/Aliquat336. A methodology has been developed for the implementation of the liquid-liquid extraction in micro-system for each chemical system. The influence of various geometric parameters such as channel length or specific interfacial area has been studied and the comparison of the liquid-liquid extraction performances has led to highlight the influence of the phases viscosities ratio on the flows. Thanks to the modeling of both hydrodynamics and mass transfer in micro-system, the criteria related to physical and kinetic properties of the chemical systems have been distinguished to propose a rational conception of tailor-made chips. Finally, several examples of the liquid-liquid extraction implementation in micro-system have been described for analytical applications in the nuclear field: U/Co separation by Aliquat336, Eu/Sm separation by DMDBTDMA or even the coupling between a liquid-liquid extraction chip and the system of

A GPU code for analytic continuation through a sampling method

Directory of Open Access Journals (Sweden)

Johan Nordström

2016-01-01

Full Text Available We here present a code for performing analytic continuation of fermionic Green’s functions and self-energies as well as bosonic susceptibilities on a graphics processing unit (GPU. The code is based on the sampling method introduced by Mishchenko et al. (2000, and is written for the widely used CUDA platform from NVidia. Detailed scaling tests are presented, for two different GPUs, in order to highlight the advantages of this code with respect to standard CPU computations. Finally, as an example of possible applications, we provide the analytic continuation of model Gaussian functions, as well as more realistic test cases from many-body physics.

40 CFR 90.421 - Dilute gaseous exhaust sampling and analytical system description.

Science.gov (United States)

2010-07-01

... gas mixture temperature, measured at a point immediately ahead of the critical flow venturi, must be... analytical system description. (a) General. The exhaust gas sampling system described in this section is... requirements are as follows: (1) This sampling system requires the use of a Positive Displacement Pump—Constant...

Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

Directory of Open Access Journals (Sweden)

Abuzar Kabir

2017-12-01

Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

Interpolation and sampling in spaces of analytic functions

CERN Document Server

Seip, Kristian

2004-01-01

The book is about understanding the geometry of interpolating and sampling sequences in classical spaces of analytic functions. The subject can be viewed as arising from three classical topics: Nevanlinna-Pick interpolation, Carleson's interpolation theorem for H^\\infty, and the sampling theorem, also known as the Whittaker-Kotelnikov-Shannon theorem. The book aims at clarifying how certain basic properties of the space at hand are reflected in the geometry of interpolating and sampling sequences. Key words for the geometric descriptions are Carleson measures, Beurling densities, the Nyquist rate, and the Helson-Szegő condition. The book is based on six lectures given by the author at the University of Michigan. This is reflected in the exposition, which is a blend of informal explanations with technical details. The book is essentially self-contained. There is an underlying assumption that the reader has a basic knowledge of complex and functional analysis. Beyond that, the reader should have some familiari...

Means of introducing an analyte into liquid sampling atmospheric pressure glow discharge

Science.gov (United States)

Marcus, R. Kenneth; Quarles, Jr., Charles Derrick; Russo, Richard E.; Koppenaal, David W.; Barinaga, Charles J.; Carado, Anthony J.

2017-01-03

A liquid sampling, atmospheric pressure, glow discharge (LS-APGD) device as well as systems that incorporate the device and methods for using the device and systems are described. The LS-APGD includes a hollow capillary for delivering an electrolyte solution to a glow discharge space. The device also includes a counter electrode in the form of a second hollow capillary that can deliver the analyte into the glow discharge space. A voltage across the electrolyte solution and the counter electrode creates the microplasma within the glow discharge space that interacts with the analyte to move it to a higher energy state (vaporization, excitation, and/or ionization of the analyte).

Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality: A novel statistical approach for quality scoring.

Science.gov (United States)

Kooijman, Pieter C; Kok, Sander J; Weusten, Jos J A M; Honing, Maarten

2016-05-05

Preparation of samples according to an optimized method is crucial for accurate determination of polymer sample characteristics by Matrix-Assisted Laser Desorption Ionization (MALDI) analysis. Sample preparation conditions such as matrix choice, cationization agent, deposition technique or even the deposition volume should be chosen to suit the sample of interest. Many sample preparation protocols have been developed and employed, yet finding the optimal sample preparation protocol remains a challenge. Because an objective comparison between the results of diverse protocols is not possible, "gut-feeling" or "good enough" is often decisive in the search for an optimum. This implies that sub-optimal protocols are used, leading to a loss of mass spectral information quality. To address this problem a novel analytical strategy based on MALDI imaging and statistical data processing was developed in which eight parameters were formulated to objectively quantify the quality of sample deposition and optimal MALDI matrix composition and finally sum up to an overall quality score of the sample deposition. These parameters can be established in a fully automated way using commercially available mass spectrometry imaging instruments without any hardware adjustments. With the newly developed analytical strategy the highest quality MALDI spots were selected, resulting in more reproducible and more valuable spectra for PEG in a variety of matrices. Moreover, our method enables an objective comparison of sample preparation protocols for any analyte and opens up new fields of investigation by presenting MALDI performance data in a clear and concise way. Copyright © 2016 Elsevier B.V. All rights reserved.

An analytical protocol for the determination of total mercury concentrations in solid peat samples

DEFF Research Database (Denmark)

Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A

2002-01-01

Traditional peat sample preparation methods such as drying at high temperatures and milling may be unsuitable for Hg concentration determination in peats due to the possible presence of volatile Hg species, which could be lost during drying. Here, the effects of sample preparation and natural.......12 and 8.52 ng kg(-1) h(-1), respectively). Fertilising the peat slightly increased Hg loss (3.08 ng kg(-1) h(-1) in NPK-fertilised peat compared to 0.28 ng kg(-1) h(-1) in unfertilised peat, when averaged over all temperatures used). Homogenising samples by grinding in a machine also caused a loss of Hg....... A comparison of two Hg profiles from an Arctic peat core, measured in frozen samples and in air-dried samples, revealed that no Hg losses occurred upon air-drying. A comparison of Hg concentrations in several plant species that make up peat, showed that some species (Pinus mugo, Sphagnum recurvum...

Rapid Gamma Screening of Shipments of Analytical Samples to Meet DOT Regulations

International Nuclear Information System (INIS)

Wojtaszek, P.A.; Remington, D.L.; Ideker-Mulligan, V.

2006-01-01

The accelerated closure program at Rocky Flats required the capacity to ship up to 1000 analytical samples per week to off-site commercial laboratories, and to conduct such shipment within 24 hours of sample collection. During a period of near peak activity in the closure project, a regulatory change significantly increased the level of radionuclide data required for shipment of each package. In order to meet these dual challenges, a centralized and streamlined sample management program was developed which channeled analytical samples through a single, high-throughput radiological screening facility. This trailerized facility utilized high purity germanium (HPGe) gamma spectrometers to conduct screening measurements of entire packages of samples at once, greatly increasing throughput compared to previous methods. The In Situ Object Counting System (ISOCS) was employed to calibrate the HPGe systems to accommodate the widely varied sample matrices and packing configurations encountered. Optimum modeling and configuration parameters were determined. Accuracy of the measurements of grouped sample jars was confirmed with blind samples in multiple configurations. Levels of radionuclides not observable by gamma spectroscopy were calculated utilizing a spreadsheet program that can accommodate isotopic ratios for large numbers of different waste streams based upon acceptable knowledge. This program integrated all radionuclide data and output all information required for shipment, including the shipping class of the package. (authors)

Optimization of a sample processing protocol for recovery of Bacillus anthracis spores from soil

Science.gov (United States)

Silvestri, Erin E.; Feldhake, David; Griffin, Dale; Lisle, John T.; Nichols, Tonya L.; Shah, Sanjiv; Pemberton, A; Schaefer III, Frank W

2016-01-01

Following a release of Bacillus anthracis spores into the environment, there is a potential for lasting environmental contamination in soils. There is a need for detection protocols for B. anthracis in environmental matrices. However, identification of B. anthracis within a soil is a difficult task. Processing soil samples helps to remove debris, chemical components, and biological impurities that can interfere with microbiological detection. This study aimed to optimize a previously used indirect processing protocol, which included a series of washing and centrifugation steps. Optimization of the protocol included: identifying an ideal extraction diluent, variation in the number of wash steps, variation in the initial centrifugation speed, sonication and shaking mechanisms. The optimized protocol was demonstrated at two laboratories in order to evaluate the recovery of spores from loamy and sandy soils. The new protocol demonstrated an improved limit of detection for loamy and sandy soils over the non-optimized protocol with an approximate matrix limit of detection at 14 spores/g of soil. There were no significant differences overall between the two laboratories for either soil type, suggesting that the processing protocol will be robust enough to use at multiple laboratories while achieving comparable recoveries.

An automated baseline correction protocol for infrared spectra of atmospheric aerosols collected on polytetrafluoroethylene (Teflon) filters

Science.gov (United States)

Kuzmiakova, Adele; Dillner, Ann M.; Takahama, Satoshi

2016-06-01

A growing body of research on statistical applications for characterization of atmospheric aerosol Fourier transform infrared (FT-IR) samples collected on polytetrafluoroethylene (PTFE) filters (e.g., Russell et al., 2011; Ruthenburg et al., 2014) and a rising interest in analyzing FT-IR samples collected by air quality monitoring networks call for an automated PTFE baseline correction solution. The existing polynomial technique (Takahama et al., 2013) is not scalable to a project with a large number of aerosol samples because it contains many parameters and requires expert intervention. Therefore, the question of how to develop an automated method for baseline correcting hundreds to thousands of ambient aerosol spectra given the variability in both environmental mixture composition and PTFE baselines remains. This study approaches the question by detailing the statistical protocol, which allows for the precise definition of analyte and background subregions, applies nonparametric smoothing splines to reproduce sample-specific PTFE variations, and integrates performance metrics from atmospheric aerosol and blank samples alike in the smoothing parameter selection. Referencing 794 atmospheric aerosol samples from seven Interagency Monitoring of PROtected Visual Environment (IMPROVE) sites collected during 2011, we start by identifying key FT-IR signal characteristics, such as non-negative absorbance or analyte segment transformation, to capture sample-specific transitions between background and analyte. While referring to qualitative properties of PTFE background, the goal of smoothing splines interpolation is to learn the baseline structure in the background region to predict the baseline structure in the analyte region. We then validate the model by comparing smoothing splines baseline-corrected spectra with uncorrected and polynomial baseline (PB)-corrected equivalents via three statistical applications: (1) clustering analysis, (2) functional group quantification

Nuclear analytical techniques and their application to environmental samples

International Nuclear Information System (INIS)

Lieser, K.H.

1986-01-01

A survey is given on nuclear analytical techniques and their application to environmental samples. Measurement of the inherent radioactivity of elements or radionuclides allows determination of natural radioelements (e.g. Ra), man-made radioelements (e.g. Pu) and radionuclides in the environment. Activation analysis, in particular instrumental neutron activation analysis, is a very reliable and sensitive method for determination of a great number of trace elements in environmental samples, because the most abundant main constituents are not activated. Tracer techniques are very useful for studies of the behaviour and of chemical reactions of trace elements and compounds in the environment. Radioactive sources are mainly applied for excitation of characteristic X-rays (X-ray fluorescence analysis). (author)

Results Of Analytical Sample Crosschecks For Next Generation Solvent Extraction Samples Isopar L Concentration And pH

International Nuclear Information System (INIS)

Peters, T.; Fink, S.

2011-01-01

As part of the implementation process for the Next Generation Cesium Extraction Solvent (NGCS), SRNL and F/H Lab performed a series of analytical cross-checks to ensure that the components in the NGCS solvent system do not constitute an undue analytical challenge. For measurement of entrained Isopar(reg s ign) L in aqueous solutions, both labs performed similarly with results more reliable at higher concentrations (near 50 mg/L). Low bias occurred in both labs, as seen previously for comparable blind studies for the baseline solvent system. SRNL recommends consideration to use of Teflon(trademark) caps on all sample containers used for this purpose. For pH measurements, the labs showed reasonable agreement but considerable positive bias for dilute boric acid solutions. SRNL recommends consideration of using an alternate analytical method for qualification of boric acid concentrations.

Analytic continuation of quantum Monte Carlo data. Stochastic sampling method

Energy Technology Data Exchange (ETDEWEB)

Ghanem, Khaldoon; Koch, Erik [Institute for Advanced Simulation, Forschungszentrum Juelich, 52425 Juelich (Germany)

2016-07-01

We apply Bayesian inference to the analytic continuation of quantum Monte Carlo (QMC) data from the imaginary axis to the real axis. Demanding a proper functional Bayesian formulation of any analytic continuation method leads naturally to the stochastic sampling method (StochS) as the Bayesian method with the simplest prior, while it excludes the maximum entropy method and Tikhonov regularization. We present a new efficient algorithm for performing StochS that reduces computational times by orders of magnitude in comparison to earlier StochS methods. We apply the new algorithm to a wide variety of typical test cases: spectral functions and susceptibilities from DMFT and lattice QMC calculations. Results show that StochS performs well and is able to resolve sharp features in the spectrum.

Preoperative vestibular assessment protocol of cochlear implant surgery: an analytical descriptive study.

Science.gov (United States)

Bittar, Roseli Saraiva Moreira; Sato, Eduardo Setsuo; Ribeiro, Douglas Jósimo Silva; Tsuji, Robinson Koji

Cochlear implants are undeniably an effective method for the recovery of hearing function in patients with hearing loss. To describe the preoperative vestibular assessment protocol in subjects who will be submitted to cochlear implants. Our institutional protocol provides the vestibular diagnosis through six simple tests: Romberg and Fukuda tests, assessment for spontaneous nystagmus, Head Impulse Test, evaluation for Head Shaking Nystagmus and caloric test. 21 patients were evaluated with a mean age of 42.75±14.38 years. Only 28% of the sample had all normal test results. The presence of asymmetric vestibular information was documented through the caloric test in 32% of the sample and spontaneous nystagmus was an important clue for the diagnosis. Bilateral vestibular areflexia was present in four subjects, unilateral arreflexia in three and bilateral hyporeflexia in two. The Head Impulse Test was a significant indicator for the diagnosis of areflexia in the tested ear (p=0.0001). The sensitized Romberg test using a foam pad was able to diagnose severe vestibular function impairment (p=0.003). The six clinical tests were able to identify the presence or absence of vestibular function and function asymmetry between the ears of the same individual. Copyright © 2016 Associação Brasileira de Otorrinolaringologia e Cirurgia Cérvico-Facial. Published by Elsevier Editora Ltda. All rights reserved.

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

Science.gov (United States)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging.

Science.gov (United States)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed. Graphical Abstract ᅟ.

Minimal sampling protocol for accurate estimation of urea production: a study with oral [13C]urea in fed and fasted piglets

NARCIS (Netherlands)

Oosterveld, Michiel J. S.; Gemke, Reinoud J. B. J.; Dainty, Jack R.; Kulik, Willem; Jakobs, Cornelis; de Meer, Kees

2005-01-01

An oral [13C]urea protocol may provide a simple method for measurement of urea production. The validity of single pool calculations in relation to a reduced sampling protocol was assessed. In eight fed and five fasted piglets, plasma urea enrichments from a 10 h sampling protocol were measured

Recent bibliography on analytical and sampling problems of a PWR primary coolant

International Nuclear Information System (INIS)

Illy, H.

1980-07-01

An extensive bibliography on the problems of analysis and sampling of the primary cooling water of PWRs is presented. The aim was to collect the analytical methods for dissolved gases. The sampling and preparation are also taken into account. last 8-10 years is included. The bibliography is arranged into alphabetical order by topics. The most important topics are as follows: boric acid, gas analysis, hydrogen isotopes, iodine, noble gases, radiation monitoring, sampling and preparation, water chemistry. (R.J.)

MoonDB — A Data System for Analytical Data of Lunar Samples

Science.gov (United States)

Lehnert, K.; Ji, P.; Cai, M.; Evans, C.; Zeigler, R.

2018-04-01

MoonDB is a data system that makes analytical data from the Apollo lunar sample collection and lunar meteorites accessible by synthesizing published and unpublished datasets in a relational database with an online search interface.

SPIDIA-RNA: second external quality assessment for the pre-analytical phase of blood samples used for RNA based analyses.

Directory of Open Access Journals (Sweden)

Francesca Malentacchi

Full Text Available One purpose of the EC funded project, SPIDIA, is to develop evidence-based quality guidelines for the pre-analytical handling of blood samples for RNA molecular testing. To this end, two pan-European External Quality Assessments (EQAs were implemented. Here we report the results of the second SPIDIA-RNA EQA. This second study included modifications in the protocol related to the blood collection process, the shipping conditions and pre-analytical specimen handling for participants. Participating laboratories received two identical proficiency blood specimens collected in tubes with or without an RNA stabilizer. For pre-defined specimen storage times and temperatures, laboratories were asked to perform RNA extraction from whole blood according to their usual procedure and to return extracted RNA to the SPIDIA facility for further analysis. These RNA samples were evaluated for purity, yield, integrity, stability, presence of interfering substances, and gene expression levels for the validated markers of RNA stability: FOS, IL1B, IL8, GAPDH, FOSB and TNFRSF10c. Analysis of the gene expression results of FOS, IL8, FOSB, and TNFRSF10c, however, indicated that the levels of these transcripts were significantly affected by blood collection tube type and storage temperature. These results demonstrated that only blood collection tubes containing a cellular RNA stabilizer allowed reliable gene expression analysis within 48 h from blood collection for all the genes investigated. The results of these two EQAs have been proposed for use in the development of a Technical Specification by the European Committee for Standardization.

Zoonoses action plan Salmonella monitoring programme: an investigation of the sampling protocol.

Science.gov (United States)

Snary, E L; Munday, D K; Arnold, M E; Cook, A J C

2010-03-01

The Zoonoses Action Plan (ZAP) Salmonella Programme was established by the British Pig Executive to monitor Salmonella prevalence in quality-assured British pigs at slaughter by testing a sample of pigs with a meat juice enzyme-linked immunosorbent assay for antibodies against group B and C(1) Salmonella. Farms were assigned a ZAP level (1 to 3) depending on the monitored prevalence, and ZAP 2 or 3 farms were required to act to reduce the prevalence. The ultimate goal was to reduce the risk of human salmonellosis attributable to British pork. A mathematical model has been developed to describe the ZAP sampling protocol. Results show that the probability of assigning a farm the correct ZAP level was high, except for farms that had a seroprevalence close to the cutoff points between different ZAP levels. Sensitivity analyses identified that the probability of assigning a farm to the correct ZAP level was dependent on the sensitivity and specificity of the test, the number of batches taken to slaughter each quarter, and the number of samples taken per batch. The variability of the predicted seroprevalence was reduced as the number of batches or samples increased and, away from the cutoff points, the probability of being assigned the correct ZAP level increased as the number of batches or samples increased. In summary, the model described here provided invaluable insight into the ZAP sampling protocol. Further work is required to understand the impact of the program for Salmonella infection in British pig farms and therefore on human health.

Analytical and sampling problems in primary coolant circuits of PWR-type reactors

International Nuclear Information System (INIS)

Illy, H.

1980-10-01

Details of recent analytical methods on the analysis and sampling of a PWR primary coolant are given in the order as follows: sampling and preparation; analysis of the gases dissolved in the water; monitoring of radiating substances; checking of boric acid concentration which controls the reactivity. The bibliography of this work and directions for its use are published in a separate report: KFKI-80-48 (1980). (author)

New method development in prehistoric stone tool research: evaluating use duration and data analysis protocols.

Science.gov (United States)

Evans, Adrian A; Macdonald, Danielle A; Giusca, Claudiu L; Leach, Richard K

2014-10-01

Lithic microwear is a research field of prehistoric stone tool (lithic) analysis that has been developed with the aim to identify how stone tools were used. It has been shown that laser scanning confocal microscopy has the potential to be a useful quantitative tool in the study of prehistoric stone tool function. In this paper, two important lines of inquiry are investigated: (1) whether the texture of worn surfaces is constant under varying durations of tool use, and (2) the development of rapid objective data analysis protocols. This study reports on the attempt to further develop these areas of study and results in a better understanding of the complexities underlying the development of flexible analytical algorithms for surface analysis. The results show that when sampling is optimised, surface texture may be linked to contact material type, independent of use duration. Further research is needed to validate this finding and test an expanded range of contact materials. The use of automated analytical protocols has shown promise but is only reliable if sampling location and scale are defined. Results suggest that the sampling protocol reports on the degree of worn surface invasiveness, complicating the ability to investigate duration related textural characterisation. Copyright © 2014. Published by Elsevier Ltd.

An analytical examination of distortions in power spectra due to sampling errors

International Nuclear Information System (INIS)

Njau, E.C.

1982-06-01

Distortions introduced into spectral energy densities of sinusoid signals as well as those of more complex signals through different forms of errors in signal sampling are developed and shown analytically. The approach we have adopted in doing this involves, firstly, developing for each type of signal and for the corresponding form of sampling errors an analytical expression that gives the faulty digitization process involved in terms of the features of the particular signal. Secondly, we take advantage of a method described elsewhere [IC/82/44] to relate, as much as possible, the true spectral energy density of the signal and the corresponding spectral energy density of the faulty digitization process. Thirdly, we then develop expressions which reveal the distortions that are formed in the directly computed spectral energy density of the digitized signal. It is evident from the formulations developed herein that the types of sampling errors taken into consideration may create false peaks and other distortions that are of non-negligible concern in computed power spectra. (author)

Sampling analytical tests and destructive tests for quality assurance

International Nuclear Information System (INIS)

Saas, A.; Pasquini, S.; Jouan, A.; Angelis, de; Hreen Taywood, H.; Odoj, R.

1990-01-01

In the context of the third programme of the European Communities on the monitoring of radioactive waste, various methods have been developed for the performance of sampling and measuring tests on encapsulated waste of low and medium level activity, on the one hand, and of high level activity, on the other hand. The purpose was to provide better quality assurance for products to be stored on an interim or long-term basis. Various testing sampling means are proposed such as: - sampling of raw waste before conditioning and determination of the representative aliquot, - sampling of encapsulated waste on process output, - sampling of core specimens subjected to measurement before and after cutting. Equipment suitable for these sampling procedures have been developed and, in the case of core samples, a comparison of techniques has been made. The results are described for the various analytical tests carried out on the samples such as: - mechanical tests, - radiation resistance, - fire resistance, - lixiviation, - determination of free water, - biodegradation, - water resistance, - chemical and radiochemical analysis. Every time it was possible, these tests were compared with non-destructive tests on full-scale packages and some correlations are given. This word has made if possible to improve and clarify sample optimization, with fine sampling techniques and methodologies and draw up characterization procedures. It also provided an occasion for a first collaboration between the laboratories responsible for these studies and which will be furthered in the scope of the 1990-1994 programme

Hanford transuranic analytical capability

International Nuclear Information System (INIS)

McVey, C.B.

1995-01-01

With the current DOE focus on ER/WM programs, an increase in the quantity of waste samples that requires detailed analysis is forecasted. One of the prime areas of growth is the demand for DOE environmental protocol analyses of TRU waste samples. Currently there is no laboratory capacity to support analysis of TRU waste samples in excess of 200 nCi/gm. This study recommends that an interim solution be undertaken to provide these services. By adding two glove boxes in room 11A of 222S the interim waste analytical needs can be met for a period of four to five years or until a front end facility is erected at or near the 222-S facility. The yearly average of samples is projected to be approximately 600 samples. The figure has changed significantly due to budget changes and has been downgraded from 10,000 samples to the 600 level. Until these budget and sample projection changes become firmer, a long term option is not recommended at this time. A revision to this document is recommended by March 1996 to review the long term option and sample projections

Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

Directory of Open Access Journals (Sweden)

Zoraida Sosa-Ferrera

2013-01-01

Full Text Available Endocrine-disruptor compounds (EDCs can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented.

EDXRF applied to the chemical element determination of small invertebrate samples

International Nuclear Information System (INIS)

Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de

2015-01-01

Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E n Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

Soil sampling and analytical strategies for mapping fallout in nuclear emergencies based on the Fukushima Dai-ichi Nuclear Power Plant accident

International Nuclear Information System (INIS)

Onda, Yuichi; Kato, Hiroaki; Hoshi, Masaharu; Takahashi, Yoshio; Nguyen, Minh-Long

2015-01-01

The Fukushima Dai-ichi Nuclear Power Plant (FDNPP) accident resulted in extensive radioactive contamination of the environment via deposited radionuclides such as radiocesium and 131 I. Evaluating the extent and level of environmental contamination is critical to protecting citizens in affected areas and to planning decontamination efforts. However, a standardized soil sampling protocol is needed in such emergencies to facilitate the collection of large, tractable samples for measuring gamma-emitting radionuclides. In this study, we developed an emergency soil sampling protocol based on preliminary sampling from the FDNPP accident-affected area. We also present the results of a preliminary experiment aimed to evaluate the influence of various procedures (e.g., mixing, number of samples) on measured radioactivity. Results show that sample mixing strongly affects measured radioactivity in soil samples. Furthermore, for homogenization, shaking the plastic sample container at least 150 times or disaggregating soil by hand-rolling in a disposable plastic bag is required. Finally, we determined that five soil samples within a 3 m × 3-m area are the minimum number required for reducing measurement uncertainty in the emergency soil sampling protocol proposed here. - Highlights: • Emergency soil sampling protocol was proposed for nuclear hazards. • Various sampling procedures were tested and evaluated in Fukushima area. • Soil sample mixing procedure was of key importance for measured radioactivity. • Minimum number of sampling was determined for reducing measurement uncertainty

Computerized Analytical Data Management System and Automated Analytical Sample Transfer System at the COGEMA Reprocessing Plants in La Hague

International Nuclear Information System (INIS)

Flament, T.; Goasmat, F.; Poilane, F.

2002-01-01

Managing the operation of large commercial spent nuclear fuel reprocessing plants, such as UP3 and UP2-800 in La Hague, France, requires an extensive analytical program and the shortest possible analysis response times. COGEMA, together with its engineering subsidiary SGN, decided to build high-performance laboratories to support operations in its plants. These laboratories feature automated equipment, safe environments for operators, and short response times, all in centralized installations. Implementation of a computerized analytical data management system and a fully automated pneumatic system for the transfer of radioactive samples was a key factor contributing to the successful operation of the laboratories and plants

A review of blood sample handling and pre-processing for metabolomics studies.

Science.gov (United States)

Hernandes, Vinicius Veri; Barbas, Coral; Dudzik, Danuta

2017-09-01

Metabolomics has been found to be applicable to a wide range of clinical studies, bringing a new era for improving clinical diagnostics, early disease detection, therapy prediction and treatment efficiency monitoring. A major challenge in metabolomics, particularly untargeted studies, is the extremely diverse and complex nature of biological specimens. Despite great advances in the field there still exist fundamental needs for considering pre-analytical variability that can introduce bias to the subsequent analytical process and decrease the reliability of the results and moreover confound final research outcomes. Many researchers are mainly focused on the instrumental aspects of the biomarker discovery process, and sample related variables sometimes seem to be overlooked. To bridge the gap, critical information and standardized protocols regarding experimental design and sample handling and pre-processing are highly desired. Characterization of a range variation among sample collection methods is necessary to prevent results misinterpretation and to ensure that observed differences are not due to an experimental bias caused by inconsistencies in sample processing. Herein, a systematic discussion of pre-analytical variables affecting metabolomics studies based on blood derived samples is performed. Furthermore, we provide a set of recommendations concerning experimental design, collection, pre-processing procedures and storage conditions as a practical review that can guide and serve for the standardization of protocols and reduction of undesirable variation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

2003-01-01

A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

HYDROLYSIS OF MTBE TO TBA IN GROUND WATER SAMPLES WITH HYDROCHLORIC ACID

Science.gov (United States)

Conventional sampling and analytical protocols have poor sensitivity for fuel oxygenates that are alcohols, such as tert-butyl alcohol (TBA). Because alcohols are miscible or highly soluble in water, alcohols are not efficiently transferred to the gas chromatograph for analysis....

Paper Capillary Enables Effective Sampling for Microfluidic Paper Analytical Devices.

Science.gov (United States)

Shangguan, Jin-Wen; Liu, Yu; Wang, Sha; Hou, Yun-Xuan; Xu, Bi-Yi; Xu, Jing-Juan; Chen, Hong-Yuan

2018-06-06

Paper capillary is introduced to enable effective sampling on microfluidic paper analytical devices. By coupling mac-roscale capillary force of paper capillary and microscale capillary forces of native paper, fluid transport can be flexibly tailored with proper design. Subsequently, a hybrid-fluid-mode paper capillary device was proposed, which enables fast and reliable sampling in an arrayed form, with less surface adsorption and bias for different components. The resulting device thus well supports high throughput, quantitative, and repeatable assays all by hands operation. With all these merits, multiplex analysis of ions, proteins, and microbe have all been realized on this platform, which has paved the way to level-up analysis on μPADs.

Protocol for sampling and analysis of bone specimens

International Nuclear Information System (INIS)

Aras, N.K.

2000-01-01

The iliac crest of hip bone was chosen as the most suitable sampling site for several reasons: Local variation in the elemental concentration along the iliac crest is minimal; Iliac crest biopsies are commonly taken clinically on patients; The cortical part of the sample is small (∼2 mm) and can be separated easily from the trabecular bone; The use of the trabecular part of the iliac crest for trace element analysis has the advantage of reflecting rapidly changes in the composition of bone due to external parameters, including medication. Biopsy studies, although in some ways more difficult than autopsy studies, because of the need to obtain the informed consents of the subjects, are potentially more useful than autopsy studies. Thereby many problems of postmortem migration of elements can be avoided and reliable dietary and other data can be collected simultaneously. Select the subjects among the patients undergoing orthopedic surgery due to any reason other than osteoporosis. Follow an established protocol to obtain bone biopsies. Patients undergoing synergy should fill in the 'Osteoporosis Project Questionnaire Form' including information on lifestyle variables, dietary intakes, the reason for surgery etc. If possible, measure the bone mineral density (BMD) prior to removal of the biopsy sample. However it may not possible to have BMD results on all the subjects because of difficulty of DEXA measurement after an accident

Time and temperature dependent analytical stability of dry-collected Evalyn HPV self-sampling brush for cervical cancer screening

DEFF Research Database (Denmark)

Ejegod, Ditte Møller; Pedersen, Helle; Alzua, Garazi Peña

2018-01-01

As a new initiative, HPV self-sampling to non-attenders using the dry Evalyn self-sampling brush is offered in the Capital Region of Denmark. The use of a dry brush is largely uncharted territory in terms of analytical stability. In this study we aim to provide evidence on the analytical quality...

Abstracts book of 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements

International Nuclear Information System (INIS)

1995-01-01

The 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements has been held in Poznan 27-28 April 1995. The new versions of analytical methods have been presented for quantitative determination of trace elements in biological, environmental and geological materials. Also the number of special techniques for sample preparation enables achievement the best precision of analytical results have been shown and discussed

A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water: Sample preparation, liquid chromatography, and mass spectrometry.

Science.gov (United States)

Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok; Lee, Jae-Kwan

2018-07-01

Medically important (MI) antibiotics are defined by the United States Food and Drug Administration as drugs containing certain active antimicrobial ingredients that are used for the treatment of human diseases or enteric pathogens causing food-borne diseases. The presence of MI antibiotic residues in environmental water is a major concern for both aquatic ecosystems and public health, particularly because of their potential to contribute to the development of antimicrobial-resistant microorganisms. In this article, we present a review of global trends in the sales of veterinary MI antibiotics and the analytical methodologies used for the simultaneous determination of antibiotic residues in environmental water. According to recently published government reports, sales volumes have increased steadily, despite many countries having adopted strategies for reducing the consumption of antibiotics. Global attention needs to be directed urgently at establishing new management strategies for reducing the use of MI antimicrobial products in the livestock industry. The development of standardized analytical methods for the detection of multiple residues is required to monitor and understand the fate of antibiotics in the environment. Simultaneous analyses of antibiotics have mostly been conducted using high-performance liquid chromatography-tandem mass spectrometry with a solid-phase extraction (SPE) pretreatment step. Currently, on-line SPE protocols are used for the rapid and sensitive detection of antibiotics in water samples. On-line detection protocols must be established for the monitoring and screening of unknown metabolites and transformation products of antibiotics in environmental water. Copyright © 2018 Elsevier Ltd. All rights reserved.

Agricultural Soil Spectral Response and Properties Assessment: Effects of Measurement Protocol and Data Mining Technique

Directory of Open Access Journals (Sweden)

Asa Gholizadeh

2017-10-01

Full Text Available Soil spectroscopy has shown to be a fast, cost-effective, environmentally friendly, non-destructive, reproducible and repeatable analytical technique. Soil components, as well as types of instruments, protocols, sampling methods, sample preparation, spectral acquisition techniques and analytical algorithms have a combined influence on the final performance. Therefore, it is important to characterize these differences and to introduce an effective approach in order to minimize the technical factors that alter reflectance spectra and consequent prediction. To quantify this alteration, a joint project between Czech University of Life Sciences Prague (CULS and Tel-Aviv University (TAU was conducted to estimate Cox, pH-H2O, pH-KCl and selected forms of Fe and Mn. Two different soil spectral measurement protocols and two data mining techniques were used to examine seventy-eight soil samples from five agricultural areas in different parts of the Czech Republic. Spectral measurements at both laboratories were made using different ASD spectroradiometers. The CULS protocol was based on employing a contact probe (CP spectral measurement scheme, while the TAU protocol was carried out using a CP measurement method, accompanied with the internal soil standard (ISS procedure. Two spectral datasets, acquired from different protocols, were both analyzed using partial least square regression (PLSR technique as well as the PARACUDA II®, a new data mining engine for optimizing PLSR models. The results showed that spectra based on the CULS setup (non-ISS demonstrated significantly higher albedo intensity and reflectance values relative to the TAU setup with ISS. However, the majority of statistics using the TAU protocol was not noticeably better than the CULS spectra. The paper also highlighted that under both measurement protocols, the PARACUDA II® engine proved to be a powerful tool for providing better results than PLSR. Such initiative is not only a way to

Trends in analytical methodologies for the determination of alkylphenols and bisphenol A in water samples.

Science.gov (United States)

Salgueiro-González, N; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2017-04-15

In the last decade, the impact of alkylphenols and bisphenol A in the aquatic environment has been widely evaluated because of their high use in industrial and household applications as well as their toxicological effects. These compounds are well-known endocrine disrupting compounds (EDCs) which can affect the hormonal system of humans and wildlife, even at low concentrations. Due to the fact that these pollutants enter into the environment through waters, and it is the most affected compartment, analytical methods which allow the determination of these compounds in aqueous samples at low levels are mandatory. In this review, an overview of the most significant advances in the analytical methodologies for the determination of alkylphenols and bisphenol A in waters is considered (from 2002 to the present). Sample handling and instrumental detection strategies are critically discussed, including analytical parameters related to quality assurance and quality control (QA/QC). Special attention is paid to miniaturized sample preparation methodologies and approaches proposed to reduce time- and reagents consumption according to Green Chemistry principles, which have increased in the last five years. Finally, relevant applications of these methods to the analysis of water samples are examined, being wastewater and surface water the most investigated. Copyright © 2017 Elsevier B.V. All rights reserved.

Negative dielectrophoresis spectroscopy for rare analyte quantification in biological samples

Science.gov (United States)

Kirmani, Syed Abdul Mannan; Gudagunti, Fleming Dackson; Velmanickam, Logeeshan; Nawarathna, Dharmakeerthi; Lima, Ivan T., Jr.

2017-03-01

We propose the use of negative dielectrophoresis (DEP) spectroscopy as a technique to improve the detection limit of rare analytes in biological samples. We observe a significant dependence of the negative DEP force on functionalized polystyrene beads at the edges of interdigitated electrodes with respect to the frequency of the electric field. We measured this velocity of repulsion for 0% and 0.8% conjugation of avidin with biotin functionalized polystyrene beads with our automated software through real-time image processing that monitors the Rayleigh scattering from the beads. A significant difference in the velocity of the beads was observed in the presence of as little as 80 molecules of avidin per biotin functionalized bead. This technology can be applied in the detection and quantification of rare analytes that can be useful in the diagnosis and the treatment of diseases, such as cancer and myocardial infarction, with the use of polystyrene beads functionalized with antibodies for the target biomarkers.

Review of Analytes of Concern and Sample Methods for Closure of DOE High Level Waste Storage Tanks

International Nuclear Information System (INIS)

Thomas, T.R.

2002-01-01

Sampling residual waste after tank cleaning and analysis for analytes of concern to support closure and cleaning targets of large underground tanks used for storage of legacy high level radioactive waste (HLW) at Department of Energy (DOE) sites has been underway since about 1995. The DOE Tanks Focus Area (TFA) has been working with DOE tank sites to develop new sampling plans, and sampling methods for assessment of residual waste inventories. This paper discusses regulatory analytes of concern, sampling plans, and sampling methods that support closure and cleaning target activities for large storage tanks at the Hanford Site, the Savannah River Site (SRS), the Idaho National Engineering and Environmental Laboratory (INEEL), and the West Valley Demonstration Project (WVDP)

Superhydrophobic analyte concentration utilizing colloid-pillar array SERS substrates.

Science.gov (United States)

Wallace, Ryan A; Charlton, Jennifer J; Kirchner, Teresa B; Lavrik, Nickolay V; Datskos, Panos G; Sepaniak, Michael J

2014-12-02

The ability to detect a few molecules present in a large sample is of great interest for the detection of trace components in both medicinal and environmental samples. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. The following work involves superhydrophobic surfaces that have as a framework deterministic or stochastic silicon pillar arrays formed by lithographic or metal dewetting protocols, respectively. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added to the functionalized pillar array system via soaking. Native pillars and pillars with hydrophobic modification are used. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A ≥ 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 × 10(-12) M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up uses in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

Energy Technology Data Exchange (ETDEWEB)

Herrero-Latorre, C., E-mail: carlos.herrero@usc.es; Álvarez-Méndez, J.; Barciela-García, J.; García-Martín, S.; Peña-Crecente, R.M.

2015-01-01

Highlights: • Analytical techniques for characterization of CNTs: classification, description and examples. • Determination methods for CNTs in biological and environmental samples. • Future trends and perspectives for characterization and determination of CNTs. - Abstract: In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.

Demonstration/Validation of the Snap Sampler Passive Ground Water Sampling Device

Science.gov (United States)

2011-06-01

purging and sampling protocol. Analytes that were measured at the Pease site included total and dissolved concentrations of arsenic (As), calcium ...samples remain in the original bottle in which they were collected, presumably losses of volatiles and changes in concentrations of dissolved gases or...because of excavation and removal. This has resulted in hydraulically interconnected bedrock and overburden water- bearing zones in much of this area

Improved analytical sensitivity for uranium and plutonium in environmental samples: Cavity ion source thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Ingeneri, Kristofer; Riciputi, L.

2001-01-01

Following successful field trials, environmental sampling has played a central role as a routine part of safeguards inspections since early 1996 to verify declared and to detect undeclared activity. The environmental sampling program has brought a new series of analytical challenges, and driven a need for advances in verification technology. Environmental swipe samples are often extremely low in concentration of analyte (ng level or lower), yet the need to analyze these samples accurately and precisely is vital, particularly for the detection of undeclared nuclear activities. Thermal ionization mass spectrometry (TIMS) is the standard method of determining isotope ratios of uranium and plutonium in the environmental sampling program. TIMS analysis typically employs 1-3 filaments to vaporize and ionize the sample, and the ions are mass separated and analyzed using magnetic sector instruments due to their high mass resolution and high ion transmission. However, the ionization efficiency (the ratio of material present to material actually detected) of uranium using a standard TIMS instrument is low (0.2%), even under the best conditions. Increasing ionization efficiency by even a small amount would have a dramatic impact for safeguards applications, allowing both improvements in analytical precision and a significant decrease in the amount of uranium and plutonium required for analysis, increasing the sensitivity of environmental sampling

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples.

Science.gov (United States)

Artigues, Margalida; Abellà, Jordi; Colominas, Sergi

2017-11-14

Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO₂NTAs) has been evaluated. The GOx-Chitosan/TiO₂NTAs biosensor showed a sensitivity of 5.46 μA·mM -1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95-105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx-Chitosan/TiO₂NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

Comparison of Different Sample Preparation Protocols Reveals Lysis Buffer-Specific Extraction Biases in Gram-Negative Bacteria and Human Cells.

Science.gov (United States)

Glatter, Timo; Ahrné, Erik; Schmidt, Alexander

2015-11-06

We evaluated different in-solution and FASP-based sample preparation strategies for absolute protein quantification. Label-free quantification (LFQ) was employed to compare different sample preparation strategies in the bacterium Pseudomonas aeruginosa and human embryonic kidney cells (HEK), and organismal-specific differences in general performance and enrichment of specific protein classes were noted. The original FASP protocol globally enriched for most proteins in the bacterial sample, whereas the sodium deoxycholate in-solution strategy was more efficient with HEK cells. Although detergents were found to be highly suited for global proteome analysis, higher intensities were obtained for high-abundant nucleic acid-associated protein complexes, like the ribosome and histone proteins, using guanidine hydrochloride. Importantly, we show for the first time that the observable total proteome mass of a sample strongly depends on the sample preparation protocol, with some protocols resulting in a significant underestimation of protein mass due to incomplete protein extraction of biased protein groups. Furthermore, we demonstrate that some of the observed abundance biases can be overcome by incorporating a nuclease treatment step or, alternatively, a correction factor for complementary sample preparation approaches.

The analytical calibration in (bio)imaging/mapping of the metallic elements in biological samples--definitions, nomenclature and strategies: state of the art.

Science.gov (United States)

Jurowski, Kamil; Buszewski, Bogusław; Piekoszewski, Wojciech

2015-01-01

Nowadays, studies related to the distribution of metallic elements in biological samples are one of the most important issues. There are many articles dedicated to specific analytical atomic spectrometry techniques used for mapping/(bio)imaging the metallic elements in various kinds of biological samples. However, in such literature, there is a lack of articles dedicated to reviewing calibration strategies, and their problems, nomenclature, definitions, ways and methods used to obtain quantitative distribution maps. The aim of this article was to characterize the analytical calibration in the (bio)imaging/mapping of the metallic elements in biological samples including (1) nomenclature; (2) definitions, and (3) selected and sophisticated, examples of calibration strategies with analytical calibration procedures applied in the different analytical methods currently used to study an element's distribution in biological samples/materials such as LA ICP-MS, SIMS, EDS, XRF and others. The main emphasis was placed on the procedures and methodology of the analytical calibration strategy. Additionally, the aim of this work is to systematize the nomenclature for the calibration terms: analytical calibration, analytical calibration method, analytical calibration procedure and analytical calibration strategy. The authors also want to popularize the division of calibration methods that are different than those hitherto used. This article is the first work in literature that refers to and emphasizes many different and complex aspects of analytical calibration problems in studies related to (bio)imaging/mapping metallic elements in different kinds of biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Sampling and sample handling procedures for priority pollutants in surface coal mining wastewaters. [Detailed list to be analyzed for

Energy Technology Data Exchange (ETDEWEB)

Hayden, R. S.; Johnson, D. O.; Henricks, J. D.

1979-03-01

The report describes the procedures used by Argonne National Laboratory to sample surface coal mine effluents in order to obtain field and laboratory data on 110 organic compounds or classes of compounds and 14 metals and minerals that are known as priority pollutants, plus 5-day biochemical oxygen demand (BOD/sub 5/), total organic carbon (TOC), chemical oxygen demand (COD), total dissolved solids (TDS), and total suspended solids (TSS). Included are directions for preparation of sampling containers and equipment, methods of sampling and sample preservation, and field and laboratory protocols, including chain-of-custody procedures. Actual analytical procedures are not described, but their sources are referenced.

MPLEx: a Robust and Universal Protocol for Single-Sample Integrative Proteomic, Metabolomic, and Lipidomic Analyses

Energy Technology Data Exchange (ETDEWEB)

Nakayasu, Ernesto S.; Nicora, Carrie D.; Sims, Amy C.; Burnum-Johnson, Kristin E.; Kim, Young-Mo; Kyle, Jennifer E.; Matzke, Melissa M.; Shukla, Anil K.; Chu, Rosalie K.; Schepmoes, Athena A.; Jacobs, Jon M.; Baric, Ralph S.; Webb-Robertson, Bobbie-Jo; Smith, Richard D.; Metz, Thomas O.; Chia, Nicholas

2016-05-03

Integrative multi-omics analyses can empower more effective investigation and complete understanding of complex biological systems. Despite recent advances in a range of omics analyses, multi-omic measurements of the same sample are still challenging and current methods have not been well evaluated in terms of reproducibility and broad applicability. Here we adapted a solvent-based method, widely applied for extracting lipids and metabolites, to add proteomics to mass spectrometry-based multi-omics measurements. Themetabolite,protein, andlipidextraction (MPLEx) protocol proved to be robust and applicable to a diverse set of sample types, including cell cultures, microbial communities, and tissues. To illustrate the utility of this protocol, an integrative multi-omics analysis was performed using a lung epithelial cell line infected with Middle East respiratory syndrome coronavirus, which showed the impact of this virus on the host glycolytic pathway and also suggested a role for lipids during infection. The MPLEx method is a simple, fast, and robust protocol that can be applied for integrative multi-omic measurements from diverse sample types (e.g., environmental,in vitro, and clinical).

IMPORTANCEIn systems biology studies, the integration of multiple omics measurements (i.e., genomics, transcriptomics, proteomics, metabolomics, and lipidomics) has been shown to provide a more complete and informative view of biological pathways. Thus, the prospect of extracting different types of molecules (e.g., DNAs, RNAs, proteins, and metabolites) and performing multiple omics measurements on single samples is very attractive, but such studies are challenging due to the fact that the extraction conditions differ according to the molecule type. Here, we adapted an organic solvent-based extraction method that demonstrated

EDXRF applied to the chemical element determination of small invertebrate samples

Energy Technology Data Exchange (ETDEWEB)

Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de, E-mail: marcelo_rlm@hotmail.com, E-mail: marianasantos_ufpe@hotmail.com, E-mail: rebecanuclear@gmail.com, E-mail: thomasmarques@live.com.pt, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

2015-07-01

Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E{sub n} Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Directory of Open Access Journals (Sweden)

Veridiana Martins

2008-01-01

Full Text Available Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

A review of electro analytical determinations of some important elements (Zn, Se, As) in environmental samples

International Nuclear Information System (INIS)

Lichiang; James, B.D.; Magee, R.J.

1991-01-01

This review covers electro analytical methods reported in the literature for the determination of zinc, cadmium, selenium and arsenic in environmental and biological samples. A comprehensive survey of electro analytical techniques used for the determination of four important elements, i.e. zinc, cadmium, selenium and arsenic is reported herein with 322 references up to 1990. (Orig./A.B.)

One Sample, One Shot - Evaluation of sample preparation protocols for the mass spectrometric proteome analysis of human bile fluid without extensive fractionation.

Science.gov (United States)

Megger, Dominik A; Padden, Juliet; Rosowski, Kristin; Uszkoreit, Julian; Bracht, Thilo; Eisenacher, Martin; Gerges, Christian; Neuhaus, Horst; Schumacher, Brigitte; Schlaak, Jörg F; Sitek, Barbara

2017-02-10

The proteome analysis of bile fluid represents a promising strategy to identify biomarker candidates for various diseases of the hepatobiliary system. However, to obtain substantive results in biomarker discovery studies large patient cohorts necessarily need to be analyzed. Consequently, this would lead to an unmanageable number of samples to be analyzed if sample preparation protocols with extensive fractionation methods are applied. Hence, the performance of simple workflows allowing for "one sample, one shot" experiments have been evaluated in this study. In detail, sixteen different protocols implying modifications at the stages of desalting, delipidation, deglycosylation and tryptic digestion have been examined. Each method has been individually evaluated regarding various performance criteria and comparative analyses have been conducted to uncover possible complementarities. Here, the best performance in terms of proteome coverage has been assessed for a combination of acetone precipitation with in-gel digestion. Finally, a mapping of all obtained protein identifications with putative biomarkers for hepatocellular carcinoma (HCC) and cholangiocellular carcinoma (CCC) revealed several proteins easily detectable in bile fluid. These results can build the basis for future studies with large and well-defined patient cohorts in a more disease-related context. Human bile fluid is a proximal body fluid and supposed to be a potential source of disease markers. However, due to its biochemical composition, the proteome analysis of bile fluid still represents a challenging task and is therefore mostly conducted using extensive fractionation procedures. This in turn leads to a high number of mass spectrometric measurements for one biological sample. Considering the fact that in order to overcome the biological variability a high number of biological samples needs to be analyzed in biomarker discovery studies, this leads to the dilemma of an unmanageable number of

Analytical results from salt batch 9 routine DSSHT and SEHT monthly samples

Energy Technology Data Exchange (ETDEWEB)

Peters, T. B. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2017-06-01

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 9 have been analyzed for ²³⁸Pu, ⁹⁰Sr, ¹³⁷Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Cs removal continues to be acceptable, with decontamination factors (DF) averaging 25700 (107% RSD). The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior, other than lacking the anticipated degree of dilution that is calculated to occur during Modular Caustic-Side Solvent Extraction Unit (MCU) processing.

Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 4

International Nuclear Information System (INIS)

Illy, H.

1986-09-01

The 4th supplement of a bibliographical series comprising the analytical and sampling problems of the primary coolant of PWR type reactors covers the literature from 1985 up to July 1986 (220 items). References are listed according to the following topics: boric acid; chloride, chlorine; general; hydrogen isotopes; iodine; iodide; noble gases; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. (V.N.)

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

Directory of Open Access Journals (Sweden)

Margalida Artigues

2017-11-01

Full Text Available Amperometric biosensors based on the use of glucose oxidase (GOx are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%, reproducibility (RSD = 2.5%, accuracy (95–105% recovery, and robustness (RSD = 3.3%. Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

Science.gov (United States)

2017-01-01

Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs) has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95–105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated. PMID:29135931

Development and validation of simple RP-HPLC-PDA analytical protocol for zileuton assisted with Design of Experiments for robustness determination

OpenAIRE

Saurabh B. Ganorkar; Dinesh M. Dhumal; Atul A. Shirkhedkar

2017-01-01

A simple, rapid, sensitive, robust, stability-indicating RP-HPLC-PDA analytical protocol was developed and validated for the analysis of zileuton racemate in bulk and in tablet formulation. Development of method and resolution of degradation products from forced; hydrolytic (acidic, basic, neutral), oxidative, photolytic (acidic, basic, neutral, solid state) and thermal (dry heat) degradation was achieved on a LC – GC Qualisil BDS C18 column (250 mm × 4.6 mm × 5 μm) by isocratic mode at ambie...

Intercalibration of analytical methods on marine environmental samples

International Nuclear Information System (INIS)

1988-06-01

The pollution of the seas by various chemical substances constitutes nowadays one of the principal concerns of mankind. The International Atomic Energy Agency has organized in past years several intercomparison exercises in the framework of its Analytical Quality Control Service. The present intercomparison had a double aim: first, to give laboratories participating in this intercomparison an opportunity for checking their analytical performance. Secondly, to produce on the basis of the results of this intercomparison a reference material made of fish tissue which would be accurately certified with respect to many trace elements. Such a material could be used by analytical chemists to check the validity of new analytical procedures. In total, 53 laboratories from 29 countries reported results (585 laboratory means for 48 elements). 5 refs, 52 tabs

The UK Biobank sample handling and storage protocol for the collection, processing and archiving of human blood and urine.

Science.gov (United States)

Elliott, Paul; Peakman, Tim C

2008-04-01

UK Biobank is a large prospective study in the UK to investigate the role of genetic factors, environmental exposures and lifestyle in the causes of major diseases of late and middle age. Extensive data and biological samples are being collected from 500,000 participants aged between 40 and 69 years. The biological samples that are collected and how they are processed and stored will have a major impact on the future scientific usefulness of the UK Biobank resource. The aim of the UK Biobank sample handling and storage protocol is to specify methods for the collection and storage of participant samples that give maximum scientific return within the available budget. Processing or storage methods that, as far as can be predicted, will preclude current or future assays have been avoided. The protocol was developed through a review of the literature on sample handling and processing, wide consultation within the academic community and peer review. Protocol development addressed which samples should be collected, how and when they should be processed and how the processed samples should be stored to ensure their long-term integrity. The recommended protocol was extensively tested in a series of validation studies. UK Biobank collects about 45 ml blood and 9 ml of urine with minimal local processing from each participant using the vacutainer system. A variety of preservatives, anti-coagulants and clot accelerators is used appropriate to the expected end use of the samples. Collection of other material (hair, nails, saliva and faeces) was also considered but rejected for the full cohort. Blood and urine samples from participants are transported overnight by commercial courier to a central laboratory where they are processed and aliquots of urine, plasma, serum, white cells and red cells stored in ultra-low temperature archives. Aliquots of whole blood are also stored for potential future production of immortalized cell lines. A standard panel of haematology assays is

Voltammetric technique, a panacea for analytical examination of environmental samples

International Nuclear Information System (INIS)

Zahir, E.; Mohiuddin, S.; Naqvi, I.I.

2012-01-01

Voltammetric methods for trace metal analysis in environmental samples of marine origin like mangrove, sediments and shrimps are generally recommended. Three different electro-analytical techniques i.e. polarography, anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (ADSV) have been used. Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ and Mn/sub 2/+ were determined through ASV, Cr/sub 6/+ was analyzed by ADSV and Fe/sub 2/+, Zn/sub 2/+, Ni/sub 2/+ and Co/sub 2/+ were determined through polarography. Out of which pairs of Fe/sub 2/+Zn/sub 2/+ and Ni/sub 2/+Co/sub 2/+ were determined in two separate runs while Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ were analyzed in single run of ASV. Sensitivity and speciation capabilities of voltammetric methods have been employed. Analysis conditions were optimized that includes selection of supporting electrolyte, pH, working electrodes, sweep rate etc. Stripping voltammetry was adopted for analysis at ultra trace levels. Statistical parameters for analytical method development like selectivity factor, interference, repeatability (0.0065-0.130 macro g/g), reproducibility (0.08125-1.625 macro g/g), detection limits (0.032-5.06 macro g/g), limits of quantification (0.081-12.652 macro g/g), sensitivities (5.636-2.15 nA mL macro g-1) etc. were also determined. The percentage recoveries were found in between 95-105% using certified reference materials. Real samples of complex marine environment from Karachi coastline were also analyzed. The standard addition method was employed where any matrix effect was evidenced. (author)

A review of analytical techniques for the determination of carbon-14 in environmental samples

International Nuclear Information System (INIS)

Milton, G.M.; Brown, R.M.

1993-11-01

This report contains a brief summary of analytical techniques commonly used for the determination of radiocarbon in a variety of environmental samples. Details of the applicable procedures developed and tested in the Environmental Research Branch at Chalk River Laboratories are appended

Microchip-electrochemistry route for rapid screening of hydroquinone and arbutin from miscellaneous samples: Investigation of the robustness of a simple cross-injector system

International Nuclear Information System (INIS)

Crevillen, Agustin G.; Barrigas, Ines; Blasco, Antonio Javier; Gonzalez, Maria Cristina; Escarpa, Alberto

2006-01-01

This work examines in deep the analytical performance of an example of 'first-generation' microdevices: capillary electrophoresis microchip (CE) with end-channel electrochemical detection (ED). A hydroquinone and arbutin separation strategically chosen as route involving pharmaceutical-clinical testing, public safety and food control scenes was carried out. The reproducibility of the unpinched electrokinetic protocol was carefully studied and the technical possibility of working indiscriminately and/or sequentially with both simple cross-injectors was also demonstrated using a real sample (R.S.D.'s less than 7%). The robustness of the injection protocol allowed checking the state of the microchip/detector coupling and following the extraction efficiency of the analyte from real sample. Separation variables such as pH, ionic strength and, separation voltage were also carefully assayed and optimized. Analyte screening was performed using borate buffer (pH 9, 60 mM) in less than 180 s in the samples studied improving dramatically the analysis times used for the same analytes on a conventional scale (15 min), with good precision (R.S.D.'s ranging 5-10%), accuracy (recoveries ranging 90-110%) and acceptable resolution (Rs ≥ 1.0). In addition, the excellent analytical performance of the overall analytical method indicated the quality of the whole analytical microsystem and allowed to introduce the definition of robustness for methodologies developed into the 'lab-on-a-chip' scene

Microchip-electrochemistry route for rapid screening of hydroquinone and arbutin from miscellaneous samples: Investigation of the robustness of a simple cross-injector system

Energy Technology Data Exchange (ETDEWEB)

Crevillen, Agustin G. [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Barrigas, Ines [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Blasco, Antonio Javier [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Gonzalez, Maria Cristina [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain); Escarpa, Alberto [Dpto. Quimica Analitica e Ingenieria Quimica, Universidad de Alcala, 28871 Alcala de Henares, Madrid (Spain)]. E-mail: alberto.escarpa@uah.es

2006-03-15

This work examines in deep the analytical performance of an example of 'first-generation' microdevices: capillary electrophoresis microchip (CE) with end-channel electrochemical detection (ED). A hydroquinone and arbutin separation strategically chosen as route involving pharmaceutical-clinical testing, public safety and food control scenes was carried out. The reproducibility of the unpinched electrokinetic protocol was carefully studied and the technical possibility of working indiscriminately and/or sequentially with both simple cross-injectors was also demonstrated using a real sample (R.S.D.'s less than 7%). The robustness of the injection protocol allowed checking the state of the microchip/detector coupling and following the extraction efficiency of the analyte from real sample. Separation variables such as pH, ionic strength and, separation voltage were also carefully assayed and optimized. Analyte screening was performed using borate buffer (pH 9, 60 mM) in less than 180 s in the samples studied improving dramatically the analysis times used for the same analytes on a conventional scale (15 min), with good precision (R.S.D.'s ranging 5-10%), accuracy (recoveries ranging 90-110%) and acceptable resolution (Rs {>=} 1.0). In addition, the excellent analytical performance of the overall analytical method indicated the quality of the whole analytical microsystem and allowed to introduce the definition of robustness for methodologies developed into the 'lab-on-a-chip' scene.

Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases.

Science.gov (United States)

Lluveras-Tenorio, Anna; Mazurek, Joy; Restivo, Annalaura; Colombini, Maria Perla; Bonaduce, Ilaria

2012-10-10

Saccharide materials have been used for centuries as binding media, to paint, write and illuminate manuscripts and to apply metallic leaf decorations. Although the technical literature often reports on the use of plant gums as binders, actually several other saccharide materials can be encountered in paint samples, not only as major binders, but also as additives. In the literature, there are a variety of analytical procedures that utilize GC-MS to characterize saccharide materials in paint samples, however the chromatographic profiles are often extremely different and it is impossible to compare them and reliably identify the paint binder. This paper presents a comparison between two different analytical procedures based on GC-MS for the analysis of saccharide materials in works-of-art. The research presented here evaluates the influence of the analytical procedure used, and how it impacts the sugar profiles obtained from the analysis of paint samples that contain saccharide materials. The procedures have been developed, optimised and systematically used to characterise plant gums at the Getty Conservation Institute in Los Angeles, USA (GCI) and the Department of Chemistry and Industrial Chemistry of the University of Pisa, Italy (DCCI). The main steps of the analytical procedures and their optimisation are discussed. The results presented highlight that the two methods give comparable sugar profiles, whether the samples analysed are simple raw materials, pigmented and unpigmented paint replicas, or paint samples collected from hundreds of centuries old polychrome art objects. A common database of sugar profiles of reference materials commonly found in paint samples was thus compiled. The database presents data also from those materials that only contain a minor saccharide fraction. This database highlights how many sources of saccharides can be found in a paint sample, representing an important step forward in the problem of identifying polysaccharide binders in

Optimization of analytical and pre-analytical conditions for MALDI-TOF-MS human urine protein profiles.

Science.gov (United States)

Calvano, C D; Aresta, A; Iacovone, M; De Benedetto, G E; Zambonin, C G; Battaglia, M; Ditonno, P; Rutigliano, M; Bettocchi, C

2010-03-11

Protein analysis in biological fluids, such as urine, by means of mass spectrometry (MS) still suffers for insufficient standardization in protocols for sample collection, storage and preparation. In this work, the influence of these variables on healthy donors human urine protein profiling performed by matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was studied. A screening of various urine sample pre-treatment procedures and different sample deposition approaches on the MALDI target was performed. The influence of urine samples storage time and temperature on spectral profiles was evaluated by means of principal component analysis (PCA). The whole optimized procedure was eventually applied to the MALDI-TOF-MS analysis of human urine samples taken from prostate cancer patients. The best results in terms of detected ions number and abundance in the MS spectra were obtained by using home-made microcolumns packed with hydrophilic-lipophilic balance (HLB) resin as sample pre-treatment method; this procedure was also less expensive and suitable for high throughput analyses. Afterwards, the spin coating approach for sample deposition on the MALDI target plate was optimized, obtaining homogenous and reproducible spots. Then, PCA indicated that low storage temperatures of acidified and centrifuged samples, together with short handling time, allowed to obtain reproducible profiles without artifacts contribution due to experimental conditions. Finally, interesting differences were found by comparing the MALDI-TOF-MS protein profiles of pooled urine samples of healthy donors and prostate cancer patients. The results showed that analytical and pre-analytical variables are crucial for the success of urine analysis, to obtain meaningful and reproducible data, even if the intra-patient variability is very difficult to avoid. It has been proven how pooled urine samples can be an interesting way to make easier the comparison between

Building America House Simulation Protocols

Energy Technology Data Exchange (ETDEWEB)

Hendron, Robert [National Renewable Energy Lab. (NREL), Golden, CO (United States); Engebrecht, Cheryn [National Renewable Energy Lab. (NREL), Golden, CO (United States)

2010-09-01

The House Simulation Protocol document was developed to track and manage progress toward Building America's multi-year, average whole-building energy reduction research goals for new construction and existing homes, using a consistent analytical reference point. This report summarizes the guidelines for developing and reporting these analytical results in a consistent and meaningful manner for all home energy uses using standard operating conditions.

Advanced Curation Protocols for Mars Returned Sample Handling

Science.gov (United States)

Bell, M.; Mickelson, E.; Lindstrom, D.; Allton, J.

Introduction: Johnson Space Center has over 30 years experience handling precious samples which include Lunar rocks and Antarctic meteorites. However, we recognize that future curation of samples from such missions as Genesis, Stardust, and Mars S mple Return, will require a high degree of biosafety combined witha extremely low levels of inorganic, organic, and biological contamination. To satisfy these requirements, research in the JSC Advanced Curation Lab is currently focused toward two major areas: preliminary examination techniques and cleaning and verification techniques . Preliminary Examination Techniques : In order to minimize the number of paths for contamination we are exploring the synergy between human &robotic sample handling in a controlled environment to help determine the limits of clean curation. Within the Advanced Curation Laboratory is a prototype, next-generation glovebox, which contains a robotic micromanipulator. The remotely operated manipulator has six degrees-of- freedom and can be programmed to perform repetitive sample handling tasks. Protocols are being tested and developed to perform curation tasks such as rock splitting, weighing, imaging, and storing. Techniques for sample transfer enabling more detailed remote examination without compromising the integrity of sample science are also being developed . The glovebox is equipped with a rapid transfer port through which samples can be passed without exposure. The transfer is accomplished by using a unique seal and engagement system which allows passage between containers while maintaining a first seal to the outside environment and a second seal to prevent the outside of the container cover and port door from becoming contaminated by the material being transferred. Cleaning and Verification Techniques: As part of the contamination control effort, innovative cleaning techniques are being identified and evaluated in conjunction with sensitive cleanliness verification methods. Towards this

Heparin removal by ecteola-cellulose pre-treatment enables the use of plasma samples for accurate measurement of anti-Yellow fever virus neutralizing antibodies.

Science.gov (United States)

Campi-Azevedo, Ana Carolina; Peruhype-Magalhães, Vanessa; Coelho-Dos-Reis, Jordana Grazziela; Costa-Pereira, Christiane; Yamamura, Anna Yoshida; Lima, Sheila Maria Barbosa de; Simões, Marisol; Campos, Fernanda Magalhães Freire; de Castro Zacche Tonini, Aline; Lemos, Elenice Moreira; Brum, Ricardo Cristiano; de Noronha, Tatiana Guimarães; Freire, Marcos Silva; Maia, Maria de Lourdes Sousa; Camacho, Luiz Antônio Bastos; Rios, Maria; Chancey, Caren; Romano, Alessandro; Domingues, Carla Magda; Teixeira-Carvalho, Andréa; Martins-Filho, Olindo Assis

2017-09-01

Technological innovations in vaccinology have recently contributed to bring about novel insights for the vaccine-induced immune response. While the current protocols that use peripheral blood samples may provide abundant data, a range of distinct components of whole blood samples are required and the different anticoagulant systems employed may impair some properties of the biological sample and interfere with functional assays. Although the interference of heparin in functional assays for viral neutralizing antibodies such as the functional plaque-reduction neutralization test (PRNT), considered the gold-standard method to assess and monitor the protective immunity induced by the Yellow fever virus (YFV) vaccine, has been well characterized, the development of pre-analytical treatments is still required for the establishment of optimized protocols. The present study intended to optimize and evaluate the performance of pre-analytical treatment of heparin-collected blood samples with ecteola-cellulose (ECT) to provide accurate measurement of anti-YFV neutralizing antibodies, by PRNT. The study was designed in three steps, including: I. Problem statement; II. Pre-analytical steps; III. Analytical steps. Data confirmed the interference of heparin on PRNT reactivity in a dose-responsive fashion. Distinct sets of conditions for ECT pre-treatment were tested to optimize the heparin removal. The optimized protocol was pre-validated to determine the effectiveness of heparin plasma:ECT treatment to restore the PRNT titers as compared to serum samples. The validation and comparative performance was carried out by using a large range of serum vs heparin plasma:ECT 1:2 paired samples obtained from unvaccinated and 17DD-YFV primary vaccinated subjects. Altogether, the findings support the use of heparin plasma:ECT samples for accurate measurement of anti-YFV neutralizing antibodies. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical method for the identification and assay of 12 phthalates in cosmetic products: application of the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques".

Science.gov (United States)

Gimeno, Pascal; Maggio, Annie-Françoise; Bousquet, Claudine; Quoirez, Audrey; Civade, Corinne; Bonnet, Pierre-Antoine

2012-08-31

Esters of phthalic acid, more commonly named phthalates, may be present in cosmetic products as ingredients or contaminants. Their presence as contaminant can be due to the manufacturing process, to raw materials used or to the migration of phthalates from packaging when plastic (polyvinyl chloride--PVC) is used. 8 phthalates (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP, and DiBP), classified H360 or H361, are forbidden in cosmetics according to the European regulation on cosmetics 1223/2009. A GC/MS method was developed for the assay of 12 phthalates in cosmetics, including the 8 phthalates regulated. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of phthalates is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30 m × 0.25 mm (i.d.) × 0.25 mm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard. Validation elements obtained on standard solutions, highlight a satisfactory system conformity (resolution>1.5), a common quantification limit at 0.25 ng injected, an acceptable linearity between 0.5 μg mL⁻¹ and 5.0 μg mL⁻¹ as well as a precision and an accuracy in agreement with in-house specifications. Cosmetic samples ready for analytical injection are analyzed after a dilution in ethanol whereas more complex cosmetic matrices, like milks and creams, are assayed after a liquid/liquid extraction using ter-butyl methyl ether (TBME). Depending on the type of cosmetics analyzed, the common limits of quantification for the 12 phthalates were set at 0.5 or 2.5 μg g⁻¹. All samples were assayed using the analytical approach described in the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques". This analytical protocol is particularly adapted when it is not possible to make reconstituted sample matrices. Copyright © 2012

[Sampling and measurement methods of the protocol design of the China Nine-Province Survey for blindness, visual impairment and cataract surgery].

Science.gov (United States)

Zhao, Jia-liang; Wang, Yu; Gao, Xue-cheng; Ellwein, Leon B; Liu, Hu

2011-09-01

To design the protocol of the China nine-province survey for blindness, visual impairment and cataract surgery to evaluate the prevalence and main causes of blindness and visual impairment, and the prevalence and outcomes of the cataract surgery. The protocol design was began after accepting the task for the national survey for blindness, visual impairment and cataract surgery from the Department of Medicine, Ministry of Health, China, in November, 2005. The protocol in Beijing Shunyi Eye Study in 1996 and Guangdong Doumen County Eye Study in 1997, both supported by World Health Organization, was taken as the basis for the protocol design. The relative experts were invited to discuss and prove the draft protocol. An international advisor committee was established to examine and approve the draft protocol. Finally, the survey protocol was checked and approved by the Department of Medicine, Ministry of Health, China and Prevention Program of Blindness and Deafness, WHO. The survey protocol was designed according to the characteristics and the scale of the survey. The contents of the protocol included determination of target population and survey sites, calculation of the sample size, design of the random sampling, composition and organization of the survey teams, determination of the examinee, the flowchart of the field work, survey items and methods, diagnostic criteria of blindness and moderate and sever visual impairment, the measures of the quality control, the methods of the data management. The designed protocol became the standard and practical protocol for the survey to evaluate the prevalence and main causes of blindness and visual impairment, and the prevalence and outcomes of the cataract surgery.

New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

International Nuclear Information System (INIS)

Montaser, A.

1993-01-01

In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

Analytical methodologies for the determination of benzodiazepines in biological samples.

Science.gov (United States)

Persona, Karolina; Madej, Katarzyna; Knihnicki, Paweł; Piekoszewski, Wojciech

2015-09-10

Benzodiazepine drugs belong to important and most widely used medicaments. They demonstrate such therapeutic properties as anxiolytic, sedative, somnifacient, anticonvulsant, diastolic and muscle relaxant effects. However, despite the fact that benzodiazepines possess high therapeutic index and are considered to be relatively safe, their use can be dangerous when: (1) co-administered with alcohol, (2) co-administered with other medicaments like sedatives, antidepressants, neuroleptics or morphine like substances, (3) driving under their influence, (4) using benzodiazepines non-therapeutically as drugs of abuse or in drug-facilitated crimes. For these reasons benzodiazepines are still studied and determined in a variety of biological materials. In this article, sample preparation techniques which have been applied in analysis of benzodiazepine drugs in biological samples have been reviewed and presented. The next part of the article is focused on a review of analytical methods which have been employed for pharmacological, toxicological or forensic study of this group of drugs in the biological matrices. The review was preceded by a description of the physicochemical properties of the selected benzodiazepines and two, very often coexisting in the same analyzed samples, sedative-hypnotic drugs. Copyright © 2015. Published by Elsevier B.V.

Utilizing distributional analytics and electronic records to assess timeliness of inpatient blood glucose monitoring in non-critical care wards

Directory of Open Access Journals (Sweden)

Ying Chen

2016-04-01

Full Text Available Abstract Background Regular and timely monitoring of blood glucose (BG levels in hospitalized patients with diabetes mellitus is crucial to optimizing inpatient glycaemic control. However, methods to quantify timeliness as a measurement of quality of care are lacking. We propose an analytical approach that utilizes BG measurements from electronic records to assess adherence to an inpatient BG monitoring protocol in hospital wards. Methods We applied our proposed analytical approach to electronic records obtained from 24 non-critical care wards in November and December 2013 from a tertiary care hospital in Singapore. We applied distributional analytics to evaluate daily adherence to BG monitoring timings. A one-sample Kolmogorov-Smirnov (1S-KS test was performed to test daily BG timings against non-adherence represented by the uniform distribution. This test was performed among wards with high power, determined through simulation. The 1S-KS test was coupled with visualization via the cumulative distribution function (cdf plot and a two-sample Kolmogorov-Smirnov (2S-KS test, enabling comparison of the BG timing distributions between two consecutive days. We also applied mixture modelling to identify the key features in daily BG timings. Results We found that 11 out of the 24 wards had high power. Among these wards, 1S-KS test with cdf plots indicated adherence to BG monitoring protocols. Integrating both 1S-KS and 2S-KS information within a moving window consisting of two consecutive days did not suggest frequent potential change from or towards non-adherence to protocol. From mixture modelling among wards with high power, we consistently identified four components with high concentration of BG measurements taken before mealtimes and around bedtime. This agnostic analysis provided additional evidence that the wards were adherent to BG monitoring protocols. Conclusions We demonstrated the utility of our proposed analytical approach as a monitoring

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

Science.gov (United States)

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Analytical and pre-analytical performance characteristics of a novel cartridge-type blood gas analyzer for point-of-care and laboratory testing.

Science.gov (United States)

Oyaert, Matthijs; Van Maerken, Tom; Bridts, Silke; Van Loon, Silvi; Laverge, Heleen; Stove, Veronique

2018-03-01

Point-of-care blood gas test results may benefit therapeutic decision making by their immediate impact on patient care. We evaluated the (pre-)analytical performance of a novel cartridge-type blood gas analyzer, the GEM Premier 5000 (Werfen), for the determination of pH, partial carbon dioxide pressure (pCO 2 ), partial oxygen pressure (pO 2 ), sodium (Na + ), potassium (K + ), chloride (Cl - ), ionized calcium ( i Ca 2+ ), glucose, lactate, and total hemoglobin (tHb). Total imprecision was estimated according to the CLSI EP5-A2 protocol. The estimated total error was calculated based on the mean of the range claimed by the manufacturer. Based on the CLSI EP9-A2 evaluation protocol, a method comparison with the Siemens RapidPoint 500 and Abbott i-STAT CG8+ was performed. Obtained data were compared against preset quality specifications. Interference of potential pre-analytical confounders on co-oximetry and electrolyte concentrations were studied. The analytical performance was acceptable for all parameters tested. Method comparison demonstrated good agreement to the RapidPoint 500 and i-STAT CG8+, except for some parameters (RapidPoint 500: pCO 2 , K + , lactate and tHb; i-STAT CG8+: pO 2 , Na + , i Ca 2+ and tHb) for which significant differences between analyzers were recorded. No interference of lipemia or methylene blue on CO-oximetry results was found. On the contrary, significant interference for benzalkonium and hemolysis on electrolyte measurements were found, for which the user is notified by an interferent specific flag. Identification of sample errors from pre-analytical sources, such as interferences and automatic corrective actions, along with the analytical performance, ease of use and low maintenance time of the instrument, makes the evaluated instrument a suitable blood gas analyzer for both POCT and laboratory use. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Marine anthropogenic radiotracers in the Southern Hemisphere: New sampling and analytical strategies

Science.gov (United States)

Levy, I.; Povinec, P. P.; Aoyama, M.; Hirose, K.; Sanchez-Cabeza, J. A.; Comanducci, J.-F.; Gastaud, J.; Eriksson, M.; Hamajima, Y.; Kim, C. S.; Komura, K.; Osvath, I.; Roos, P.; Yim, S. A.

2011-04-01

The Japan Agency for Marine Earth Science and Technology conducted in 2003-2004 the Blue Earth Global Expedition (BEAGLE2003) around the Southern Hemisphere Oceans, which was a rare opportunity to collect many seawater samples for anthropogenic radionuclide studies. We describe here sampling and analytical methodologies based on radiochemical separations of Cs and Pu from seawater, as well as radiometric and mass spectrometry measurements. Several laboratories took part in radionuclide analyses using different techniques. The intercomparison exercises and analyses of certified reference materials showed a reasonable agreement between the participating laboratories. The obtained data on the distribution of 137Cs and plutonium isotopes in seawater represent the most comprehensive results available for the Southern Hemisphere Oceans.

Macro elemental analysis of food samples by nuclear analytical technique

Science.gov (United States)

Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

2017-06-01

Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

Establishment of a protocol for the gene expression analysis of laser microdissected rat kidney samples with affymetrix genechips

International Nuclear Information System (INIS)

Stemmer, Kerstin; Ellinger-Ziegelbauer, Heidrun; Lotz, Kerstin; Ahr, Hans-J.; Dietrich, Daniel R.

2006-01-01

Laser microdissection in conjunction with microarray technology allows selective isolation and analysis of specific cell populations, e.g., preneoplastic renal lesions. To date, only limited information is available on sample preparation and preservation techniques that result in both optimal histomorphological preservation of sections and high-quality RNA for microarray analysis. Furthermore, amplification of minute amounts of RNA from microdissected renal samples allowing analysis with genechips has only scantily been addressed to date. The objective of this study was therefore to establish a reliable and reproducible protocol for laser microdissection in conjunction with microarray technology using kidney tissue from Eker rats p.o. treated for 7 days and 6 months with 10 and 1 mg Aristolochic acid/kg bw, respectively. Kidney tissues were preserved in RNAlater or snap frozen. Cryosections were cut and stained with either H and E or cresyl violet for subsequent morphological and RNA quality assessment and laser microdissection. RNA quality was comparable in snap frozen and RNAlater-preserved samples, however, the histomorphological preservation of renal sections was much better following cryopreservation. Moreover, the different staining techniques in combination with sample processing time at room temperature can have an influence on RNA quality. Different RNA amplification protocols were shown to have an impact on gene expression profiles as demonstrated with Affymetrix Rat Genome 230 2 .0 arrays. Considering all the parameters analyzed in this study, a protocol for RNA isolation from laser microdissected samples with subsequent Affymetrix chip hybridization was established that was also successfully applied to preneoplastic lesions laser microdissected from Aristolochic acid-treated rats

Evaluation of a reduced centrifugation time and higher centrifugal force on various general chemistry and immunochemistry analytes in plasma and serum.

Science.gov (United States)

Møller, Mette F; Søndergaard, Tove R; Kristensen, Helle T; Münster, Anna-Marie B

2017-09-01

Background Centrifugation of blood samples is an essential preanalytical step in the clinical biochemistry laboratory. Centrifugation settings are often altered to optimize sample flow and turnaround time. Few studies have addressed the effect of altering centrifugation settings on analytical quality, and almost all studies have been done using collection tubes with gel separator. Methods In this study, we compared a centrifugation time of 5 min at 3000 ×  g to a standard protocol of 10 min at 2200 ×  g. Nine selected general chemistry and immunochemistry analytes and interference indices were studied in lithium heparin plasma tubes and serum tubes without gel separator. Results were evaluated using mean bias, difference plots and coefficient of variation, compared with maximum allowable bias and coefficient of variation used in laboratory routine quality control. Results For all analytes except lactate dehydrogenase, the results were within the predefined acceptance criteria, indicating that the analytical quality was not compromised. Lactate dehydrogenase showed higher values after centrifugation for 5 min at 3000 ×  g, mean bias was 6.3 ± 2.2% and the coefficient of variation was 5%. Conclusions We found that a centrifugation protocol of 5 min at 3000 ×  g can be used for the general chemistry and immunochemistry analytes studied, with the possible exception of lactate dehydrogenase, which requires further assessment.

Analytical protocol to study the food safety of (multiple-)recycled high-density polyethylene (HDPE) and polypropylene (PP) crates: Influence of recycling on the migration and formation of degradation products

NARCIS (Netherlands)

Coulier, L.; Orbons, H.G.M.; Rijk, R.

2007-01-01

An analytical protocol was set up and successfully applied to study the food safety of recycled HDPE and PP crates. A worst-case scenario was applied that focused not only on overall migration and specific migration of accepted starting materials but also on migratable degradation products of

Building America House Simulation Protocols (Revised)

Energy Technology Data Exchange (ETDEWEB)

Hendron, R.; Engebrecht, C.

2010-10-01

The House Simulation Protocol document was developed to track and manage progress toward Building America's multi-year, average whole-building energy reduction research goals for new construction and existing homes, using a consistent analytical reference point. This report summarizes the guidelines for developing and reporting these analytical results in a consistent and meaningful manner for all home energy uses using standard operating conditions.

Sampling and Analytical Method for Alpha-Dicarbonyl Flavoring Compounds via Derivatization with o-Phenylenediamine and Analysis Using GC-NPD

Directory of Open Access Journals (Sweden)

Stephanie M. Pendergrass

2016-01-01

Full Text Available A novel methodology is described for the sampling and analysis of diacetyl, 2,3-pentanedione, 2,3-hexanedione, and 2,3-heptanedione. These analytes were collected on o-phenylenediamine-treated silica gel tubes and quantitatively recovered as the corresponding quinoxaline derivatives. After derivatization, the sorbent was desorbed in 3 mL of ethanol solvent and analyzed using gas chromatography/nitrogen-phosphorous detection (GC/NPD. The limits of detection (LOD achieved for each analyte were determined to be in the range of 5–10 nanograms/sample. Evaluation of the on-tube derivatization procedure indicated that it is unaffected by humidities ranging from 20% to 80% and that the derivatization procedure was quantitative for analyte concentrations ranging from 0.1 μg to approximately 500 μg per sample. Storage stability studies indicated that the derivatives were stable for 30 days when stored at both ambient and refrigerated temperatures. Additional studies showed that the quinoxaline derivatives were quantitatively recovered when sampling up to a total volume of 72 L at a sampling rate of 50 cc/min. This method will be important to evaluate and monitor worker exposures in the food and flavoring industry. Samples can be collected over an 8-hour shift with up to 288 L total volume collected regardless of time, sampling rate, and/or the effects of humidity.

Comparative analysis of five DNA isolation protocols and three drying methods for leaves samples of Nectandra megapotamica (Spreng. Mez

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Leonardo Severo da Costa

2016-06-01

Full Text Available The aim of the study was to establish a DNA isolation protocol Nectandra megapotamica (Spreng. Mez., able to obtain samples of high yield and quality for use in genomic analysis. A commercial kit and four classical methods of DNA extraction were tested, including three cetyltrimethylammonium bromide (CTAB-based and one sodium dodecyl sulfate (SDS-based methods. Three drying methods for leaves samples were also evaluated including drying at room temperature (RT, in an oven at 40ºC (S40, and in a microwave oven (FMO. The DNA solutions obtained from different types of leaves samples using the five protocols were assessed in terms of cost, execution time, and quality and yield of extracted DNA. The commercial kit did not extract DNA with sufficient quantity or quality for successful PCR reactions. Among the classic methods, only the protocols of Dellaporta and of Khanuja yielded DNA extractions for all three types of foliar samples that resulted in successful PCR reactions and subsequent enzyme restriction assays. Based on the evaluated variables, the most appropriate DNA extraction method for Nectandra megapotamica (Spreng. Mez. was that of Dellaporta, regardless of the method used to dry the samples. The selected method has a relatively low cost and total execution time. Moreover, the quality and quantity of DNA extracted using this method was sufficient for DNA sequence amplification using PCR reactions and to get restriction fragments.

Development of an analytical procedure for plutonium in the concentration range of femtogram/gram and its application to environmental samples

International Nuclear Information System (INIS)

Schuettelkopf, H.

1981-09-01

To study the behaviour of plutonium in the environment and to measure plutonium in the vicinity of nuclear facilities, a quick, sensitive analytical method is required which can be applied to all sample materials found in the environment. For a sediment contaminated with plutonium a boiling out method using first HNO 3 /HF and subsequently HNO 3 /Al(NO 3 ) 3 was found to be successful. The leaching solution was then extracted by TOPO and the plutonium backextracted by ascorbic acid/HCl. Some different purification steps and finally electroplating using ammonium oxalate led to an optimum sample for α- spectroscopic determination of plutonium. An analytical method was worked out for plutonium which can be applied to all materials found in the environment. The sample size is 100 g but it might also be much greater. The average chemical yield is 70 and 80%. The detection limit for soil samples is 0.1 fCi/g and for plant samples 0.5 fCi/g. One technician can perform eight analyses per working day. The analytical procedure was applied to a large number of environmental samples and the results of these analyses are indicated. (orig./RB) [de

Analytical results and sample locality map for rock, stream-sediment, and soil samples, Northern and Eastern Coloado Desert BLM Resource Area, Imperial, Riverside, and San Bernardino Counties, California

Science.gov (United States)

King, Harley D.; Chaffee, Maurice A.

2000-01-01

INTRODUCTION In 1996-1998 the U.S. Geological Survey (USGS) conducted a geochemical study of the Bureau of Land Management's (BLM) 5.5 million-acre Northern and Eastern Colorado Desert Resource Area (usually referred to as the NECD in this report), Imperial, Riverside, and San Bernardino Counties, southeastern California (figure 1). This study was done in support of the BLM's Coordinated Management Plan for the area. This report presents analytical data from this study. To provide comprehensive coverage of the NECD, we compiled and examined all available geochemical data, in digital form, from previous studies in the area, and made sample-site plots to aid in determining where sample-site coverage and analyses were sufficient, which samples should be re-analyzed, and where additional sampling was needed. Previous investigations conducted in parts of the current study area included the National Uranium Resource Evaluation (NURE) program studies of the Needles and Salton Sea 1? x 2? quadrangles; USGS studies of 12 BLM Wilderness Study Areas (WSAs) (Big Maria Mountains, Chemehuevi Mountains, Chuckwalla Mountains, Coxcomb Mountains, Mecca Hills, Orocopia Mountains, Palen-McCoy, Picacho Peak, Riverside Mountains, Sheephole Valley (also known as Sheep Hole/Cadiz), Turtle Mountains, and Whipple Mountains); and USGS studies in the Needles and El Centro 1? x 2? quadrangles done during the early 1990s as part of a project to identify the regional geochemistry of southern California. Areas where we did new sampling of rocks and stream sediments are mainly in the Chocolate Mountain Aerial Gunnery Range and in Joshua Tree National Park, which extends into the west-central part of the NECD, as shown in figure 1 and figure 2. This report contains analytical data for 132 rock samples and 1,245 stream-sediment samples collected by the USGS, and 362 stream-sediment samples and 189 soil samples collected during the NURE program. All samples are from the Northern and Eastern Colorado

Final Report on the Analytical Results for Tank Farm Samples in Support of Salt Dissolution Evaluation

International Nuclear Information System (INIS)

Hobbs, D.T.

1996-01-01

Recent processing of dilute solutions through the 2H-Evaporator system caused dissolution of salt in Tank 38H, the concentrate receipt tank. This report documents analytical results for samples taken from this evaporator system

Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 3

International Nuclear Information System (INIS)

Illy, H.

1985-03-01

The present supplement to the bibliography on analytical and sampling problems of PWR primary coolant covers the literature published in 1984 and includes some references overlooked in the previous volumes dealing with the publications of the last 10 years. References are devided into topics characterized by the following headlines: boric acid; chloride; chlorine; carbon dioxide; general; gas analysis; hydrogen isotopes; iodine; iodide; nitrogen; noble gases and radium; ammonia; ammonium; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. Under a given subject bibliographical information is listed in alphabetical order of the authors. (V.N.)

Current status of JAERI program on development of ultra-trace-analytical technology for safeguards environmental samples

International Nuclear Information System (INIS)

Adachi, T.; Usuda, S.; Watanabe, K.

2001-01-01

Full text: In order to contribute to the strengthened safeguards system based on the Program 93+2 of the IAEA, Japan Atomic Energy Research Institute (JAERI) is developing analytical technology for ultra-trace amounts of nuclear materials in environmental samples, and constructed the CLEAR facility (Clean Laboratory for Environmental Analysis and Research) for this purpose. The development of the technology is carried out, at existing laboratories for time being, in the following fields: screening, bulk analysis and particle analysis. The screening aims at estimating the amounts of nuclear materials in environmental samples to be introduced into the clean rooms, and is the first step to avoid cross-contamination among the samples and contamination of the clean rooms themselves. In addition to ordinary radiation spectrometry, Compton suppression technique was applied to low energy γ- and X-ray measurements, and sufficient reduction in background level has been demonstrated. Another technique in examination is imaging-plate method, which is a kind of autoradiography and suitable for determination of radioactive-particle distribution in the samples as well as for semiquantitative determination. As for the bulk analysis, the efforts are temporally made on uranium in swipe samples. Preliminary examination for optimization of sample pre-treatment conditions is in progress. At present, ashing by low-temperature-plasma method gives better results than high-temperature ashing or acid leaching. For the isotopic ratio measurement, instrumental performance of inductively-coupled plasma mass spectrometry (ICP-MS) are mainly examined because sample preparation for ICP-MS is simpler than that for thermal ionization mass spectrometry (TIMS). It was found by our measurement that the swipe material (TexWipe TX304, usually used by IAEA) contains un-negligible uranium blank with large deviation (2-6 ng/sheet). This would introduce significant uncertainty in the trace analysis. JAERI

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

International Nuclear Information System (INIS)

Lari, L; Dudkiewicz, A

2014-01-01

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

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

Science.gov (United States)

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.

Development of a new protocol for rapid bacterial identification and susceptibility testing directly from urine samples.

Science.gov (United States)

Zboromyrska, Y; Rubio, E; Alejo, I; Vergara, A; Mons, A; Campo, I; Bosch, J; Marco, F; Vila, J

2016-06-01

The current gold standard method for the diagnosis of urinary tract infections (UTI) is urine culture that requires 18-48 h for the identification of the causative microorganisms and an additional 24 h until the results of antimicrobial susceptibility testing (AST) are available. The aim of this study was to shorten the time of urine sample processing by a combination of flow cytometry for screening and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) for bacterial identification followed by AST directly from urine. The study was divided into two parts. During the first part, 675 urine samples were processed by a flow cytometry device and a cut-off value of bacterial count was determined to select samples for direct identification by MALDI-TOF-MS at ≥5 × 10(6) bacteria/mL. During the second part, 163 of 1029 processed samples reached the cut-off value. The sample preparation protocol for direct identification included two centrifugation and two washing steps. Direct AST was performed by the disc diffusion method if a reliable direct identification was obtained. Direct MALDI-TOF-MS identification was performed in 140 urine samples; 125 of the samples were positive by urine culture, 12 were contaminated and 3 were negative. Reliable direct identification was obtained in 108 (86.4%) of the 125 positive samples. AST was performed in 102 identified samples, and the results were fully concordant with the routine method among 83 monomicrobial infections. In conclusion, the turnaround time of the protocol described to diagnose UTI was about 1 h for microbial identification and 18-24 h for AST. Copyright © 2016 European Society of Clinical Microbiology and Infectious Diseases. Published by Elsevier Ltd. All rights reserved.

Measuring myokines with cardiovascular functions: pre-analytical variables affecting the analytical output.

Science.gov (United States)

Lombardi, Giovanni; Sansoni, Veronica; Banfi, Giuseppe

2017-08-01

In the last few years, a growing number of molecules have been associated to an endocrine function of the skeletal muscle. Circulating myokine levels, in turn, have been associated with several pathophysiological conditions including the cardiovascular ones. However, data from different studies are often not completely comparable or even discordant. This would be due, at least in part, to the whole set of situations related to the preparation of the patient prior to blood sampling, blood sampling procedure, processing and/or store. This entire process constitutes the pre-analytical phase. The importance of the pre-analytical phase is often not considered. However, in routine diagnostics, the 70% of the errors are in this phase. Moreover, errors during the pre-analytical phase are carried over in the analytical phase and affects the final output. In research, for example, when samples are collected over a long time and by different laboratories, a standardized procedure for sample collecting and the correct procedure for sample storage are acknowledged. In this review, we discuss the pre-analytical variables potentially affecting the measurement of myokines with cardiovascular functions.

A Systematic Evaluation of Blood Serum and Plasma Pre-Analytics for Metabolomics Cohort Studies

Directory of Open Access Journals (Sweden)

Elodie Jobard

2016-12-01

Full Text Available The recent thriving development of biobanks and associated high-throughput phenotyping studies requires the elaboration of large-scale approaches for monitoring biological sample quality and compliance with standard protocols. We present a metabolomic investigation of human blood samples that delineates pitfalls and guidelines for the collection, storage and handling procedures for serum and plasma. A series of eight pre-processing technical parameters is systematically investigated along variable ranges commonly encountered across clinical studies. While metabolic fingerprints, as assessed by nuclear magnetic resonance, are not significantly affected by altered centrifugation parameters or delays between sample pre-processing (blood centrifugation and storage, our metabolomic investigation highlights that both the delay and storage temperature between blood draw and centrifugation are the primary parameters impacting serum and plasma metabolic profiles. Storing the blood drawn at 4 °C is shown to be a reliable routine to confine variability associated with idle time prior to sample pre-processing. Based on their fine sensitivity to pre-analytical parameters and protocol variations, metabolic fingerprints could be exploited as valuable ways to determine compliance with standard procedures and quality assessment of blood samples within large multi-omic clinical and translational cohort studies.

Fast filtration sampling protocol for mammalian suspension cells tailored for phosphometabolome profiling by capillary ion chromatography - tandem mass spectrometry.

Science.gov (United States)

Kvitvang, Hans F N; Bruheim, Per

2015-08-15

Capillary ion chromatography (capIC) is the premium separation technology for low molecular phosphometabolites and nucleotides in biological extracts. Removal of excessive amounts of salt during sample preparation stages is a prerequisite to enable high quality capIC separation in combination with reproducible and sensitive MS detection. Existing sampling protocols for mammalian cells used for GC-MS and LC-MS metabolic profiling can therefore not be directly applied to capIC separations. Here, the development of a fast filtration sampling protocol for mammalian suspension cells tailored for quantitative profiling of the phosphometabolome on capIC-MS/MS is presented. The whole procedure from sampling the culture to transfer of filter to quenching and extraction solution takes less than 10s. To prevent leakage it is critical that a low vacuum pressure is applied, and satisfactorily reproducibility was only obtained by usage of a vacuum pressure controlling device. A vacuum of 60mbar was optimal for filtration of multiple myeloma Jjn-3 cell cultures through 5μm polyvinylidene (PVDF) filters. A quick deionized water (DI-water) rinse step prior to extraction was tested, and significantly higher metabolite yields were obtained during capIC-MS/MS analyses in this extract compared to extracts prepared by saline and reduced saline (25%) washing steps only. In addition, chromatographic performance was dramatically improved. Thus, it was verified that a quick DI-water rinse is tolerated by the cells and can be included as the final stage during filtration. Over 30 metabolites were quantitated in JJN-3 cell extracts by using the optimized sampling protocol with subsequent capIC-MS/MS analysis, and up to 2 million cells can be used in a single filtration step for the chosen filter and vacuum pressure. The technical set-up is also highly advantageous for microbial metabolome filtration protocols after optimization of vacuum pressure and washing solutions, and the reduced salt

Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase)

International Nuclear Information System (INIS)

Garcia Alonso, S.; Perez Pastor, R. M.

2013-01-01

A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

Evaluation of Extraction Protocols for Simultaneous Polar and Non-Polar Yeast Metabolite Analysis Using Multivariate Projection Methods

Directory of Open Access Journals (Sweden)

Nicolas P. Tambellini

2013-07-01

Full Text Available Metabolomic and lipidomic approaches aim to measure metabolites or lipids in the cell. Metabolite extraction is a key step in obtaining useful and reliable data for successful metabolite studies. Significant efforts have been made to identify the optimal extraction protocol for various platforms and biological systems, for both polar and non-polar metabolites. Here we report an approach utilizing chemoinformatics for systematic comparison of protocols to extract both from a single sample of the model yeast organism Saccharomyces cerevisiae. Three chloroform/methanol/water partitioning based extraction protocols found in literature were evaluated for their effectiveness at reproducibly extracting both polar and non-polar metabolites. Fatty acid methyl esters and methoxyamine/trimethylsilyl derivatized aqueous compounds were analyzed by gas chromatography mass spectrometry to evaluate non-polar or polar metabolite analysis. The comparative breadth and amount of recovered metabolites was evaluated using multivariate projection methods. This approach identified an optimal protocol consisting of 64 identified polar metabolites from 105 ion hits and 12 fatty acids recovered, and will potentially attenuate the error and variation associated with combining metabolite profiles from different samples for untargeted analysis with both polar and non-polar analytes. It also confirmed the value of using multivariate projection methods to compare established extraction protocols.

Review of robust measurement of phosphorus in river water: sampling, storage, fractionation and sensitivity

Directory of Open Access Journals (Sweden)

H. P. Jarvie

2002-01-01

Full Text Available This paper reviews current knowledge on sampling, storage and analysis of phosphorus (P in river waters. Potential sensitivity of rivers with different physical, chemical and biological characteristics (trophic status, turbidity, flow regime, matrix chemistry is examined in terms of errors associated with sampling, sample preparation, storage, contamination, interference and analytical errors. Key issues identified include: The need to tailor analytical reagents and concentrations to take into account the characteristics of the sample matrix. The effects of matrix interference on the colorimetric analysis. The influence of variable rates of phospho-molybdenum blue colour formation. The differing responses of river waters to physical and chemical conditions of storage. The higher sensitivities of samples with low P concentrations to storage and analytical errors. Given high variability of river water characteristics in space and time, no single standardised methodology for sampling, storage and analysis of P in rivers can be offered. ‘Good Practice’ guidelines are suggested, which recommend that protocols for sampling, storage and analysis of river water for P is based on thorough site-specific method testing and assessment of P stability on storage. For wider sampling programmes at the regional/national scale where intensive site-specific method and stability testing are not feasible, ‘Precautionary Practice’ guidelines are suggested. The study highlights key areas requiring further investigation for improving methodological rigour. Keywords: phosphorus, orthophosphate, soluble reactive, particulate, colorimetry, stability, sensitivity, analytical error, storage, sampling, filtration, preservative, fractionation, digestion

Evaluation of analytical results on DOE Quality Assessment Program Samples

International Nuclear Information System (INIS)

Jaquish, R.E.; Kinnison, R.R.; Mathur, S.P.; Sastry, R.

1985-01-01

Criteria were developed for evaluating the participants analytical results in the DOE Quality Assessment Program (QAP). Historical data from previous QAP studies were analyzed using descriptive statistical methods to determine the interlaboratory precision that had been attained. Performance criteria used in other similar programs were also reviewed. Using these data, precision values and control limits were recommended for each type of analysis performed in the QA program. Results of the analysis performed by the QAP participants on the November 1983 samples were statistically analyzed and evaluated. The Environmental Measurements Laboratory (EML) values were used as the known values and 3-sigma precision values were used as control limits. Results were submitted by 26 participating laboratories for 49 different radionuclide media combinations. The participants reported 419 results and of these, 350 or 84% were within control limits. Special attention was given to the data from gamma spectral analysis of air filters and water samples. both normal probability and box plots were prepared for each nuclide to help evaluate the distribution of the data. Results that were outside the expected range were identified and suggestions made that laboratories check calculations, and procedures on these results

Recovery of environmental analytes from clays and soils by supercritical fluid extracting/gas chromatography

International Nuclear Information System (INIS)

Emery, A.P.; Chesler, S.N.; MacCrehan, W.A.

1992-01-01

This paper reports on Supercritical Fluid Extraction (SFE) which promises to provide rapid extractions of organic analytes from environmental sample types without the use of hazardous solvents. In addition, SFE protocols using commercial instrumentation can be automated lowering analysis costs. Because of these benefits, we are investigating SFE as an alternative to the solvent extraction (eg. Soxhlet and sonication) techniques required in many EPA test procedures. SFE, using non-polar carbon dioxide as well as more polar supercritical fluids, was used to determine n-alkane hydrocarbons and polynuclear aromatic hydrocarbons (PAHs) in solid samples. The extraction behavior of these analyte classes from environmentally-contaminated soil matrices and model soil and clay matrices was investigated using a SFE apparatus in which the extracted analytes were collected on a solid phase trap and then selectively eluted with a solvent. The SFE conditions for quantitative recovery of n-alkane hydrocarbons in diesel fuel from a series of clays and soils were determined using materials prepared at the 0.02% level with diesel fuel oil in order to simplify analyte collection and analysis after extraction. The effect of extraction parameters including temperature, fluid flow rate and modifier addition were investigated by monitoring the amount of diesel fuel extracted as a function of time

Stability of purgeable VOCs in water samples during pre-analytical holding: Part 1, Analysis by a commercial laboratory

Energy Technology Data Exchange (ETDEWEB)

West, O.R.; Bayne, C.K.; Siegrist, R.L.; Holden, W.L.; Scarborough, S.S. [Oak Ridge National Lab., TN (United States); Bottrell, D.W. [USDOE, Washington, DC (United States)

1996-10-01

This study was undertaken to examine the hypothesis that prevalent and priority purgeable VOCs in properly preserved water samples are stable for at least 28 days. (VOCs are considered stable if concentrations do not change by more than 10%.) Surface water was spiked with 44 purgeable VOCs. Results showed that the measurement of 35 out of 44 purgeable VOCs in properly preserved water samples (4 C, 250 mg NaHSO{sub 4}, no headspace in 40 mL VOC vials with 0.010-in. Teflon-lined silicone septum caps) will not be affected by sample storage for 28 days. Larger changes (>10%) and low practical reporting times were observed for a few analytes, e.g. acrolein, CS{sub 2}, vinyl acetate, etc.; these also involve other analytical problems. Advantages of a 28-day (compared to 14-day) holding time are pointed out.

User's and reference guide to the INEL RML/analytical radiochemistry sample tracking database version 1.00

International Nuclear Information System (INIS)

Femec, D.A.

1995-09-01

This report discusses the sample tracking database in use at the Idaho National Engineering Laboratory (INEL) by the Radiation Measurements Laboratory (RML) and Analytical Radiochemistry. The database was designed in-house to meet the specific needs of the RML and Analytical Radiochemistry. The report consists of two parts, a user's guide and a reference guide. The user's guide presents some of the fundamentals needed by anyone who will be using the database via its user interface. The reference guide describes the design of both the database and the user interface. Briefly mentioned in the reference guide are the code-generating tools, CREATE-SCHEMA and BUILD-SCREEN, written to automatically generate code for the database and its user interface. The appendices contain the input files used by the these tools to create code for the sample tracking database. The output files generated by these tools are also included in the appendices

Recent bibliography on analytical and sampling problems of a PWR primary coolant Pt. 1

International Nuclear Information System (INIS)

Illy, H.

1981-12-01

The first bibliography on analytical and sampling problems of a PWR primary coolant (KFKI Report-1980-48) was published in 1980 and it covered the literature published in the previous 8-10 years. The present supplement reviews the subsequent literature up till December 1981. It also includes some references overlooked in the first volume. The serial numbers are continued from the first bibliography. (author)

INVESTIGATION OF THE TOTAL ORGANIC HALOGEN ANALYTICAL METHOD AT THE WASTE SAMPLING CHARACTERIZATION FACILITY (WSCF)

International Nuclear Information System (INIS)

DOUGLAS JG; MEZNARICH HD, PHD; OLSEN JR; ROSS GA; STAUFFER M

2008-01-01

Total organic halogen (TOX) is used as a parameter to screen groundwater samples at the Hanford Site. Trending is done for each groundwater well, and changes in TOX and other screening parameters can lead to costly changes in the monitoring protocol. The Waste Sampling and Characterization Facility (WSCF) analyzes groundwater samples for TOX using the United States Environmental Protection Agency (EPA) SW-846 method 9020B (EPA 1996a). Samples from the Soil and Groundwater Remediation Project (S and GRP) are submitted to the WSCF for analysis without information regarding the source of the sample; each sample is in essence a 'blind' sample to the laboratory. Feedback from the S and GRP indicated that some of the WSCF-generated TOX data from groundwater wells had a number of outlier values based on the historical trends (Anastos 2008a). Additionally, analysts at WSCF observed inconsistent TOX results among field sample replicates. Therefore, the WSCF lab performed an investigation of the TOX analysis to determine the cause of the outlier data points. Two causes were found that contributed to generating out-of-trend TOX data: (1) The presence of inorganic chloride in the groundwater samples: at inorganic chloride concentrations greater than about 10 parts per million (ppm), apparent TOX values increase with increasing chloride concentration. A parallel observation is the increase in apparent breakthrough of TOX from the first to the second activated-carbon adsorption tubes with increasing inorganic chloride concentration. (2) During the sample preparation step, excessive purging of the adsorption tubes with oxygen pressurization gas after sample loading may cause channeling in the activated-carbon bed. This channeling leads to poor removal of inorganic chloride during the subsequent wash step with aqueous potassium nitrate. The presence of this residual inorganic chloride then produces erroneously high TOX values. Changes in sample preparation were studied to more

INVESTIGATION OF THE TOTAL ORGANIC HALOGEN ANALYTICAL METHOD AT THE WASTE SAMPLING AND CHARACTERIZATION FACILITY

International Nuclear Information System (INIS)

Douglas, J.G.; Meznarich, H.K.; Olsen, J.R.; Ross, G.A.; Stauffer, M.

2009-01-01

Total organic halogen (TOX) is used as a parameter to screen groundwater samples at the Hanford Site. Trending is done for each groundwater well, and changes in TOX and other screening parameters can lead to costly changes in the monitoring protocol. The Waste Sampling and Characterization Facility (WSCF) analyzes groundwater samples for TOX using the United States Environmental Protection Agency (EPA) SW-S46 method 9020B (EPA 1996a). Samples from the Soil and Groundwater Remediation Project (SGRP) are submitted to the WSCF for analysis without information regarding the source of the sample; each sample is in essence a ''blind'' sample to the laboratory. Feedback from the SGRP indicated that some of the WSCF-generated TOX data from groundwater wells had a number of outlier values based on the historical trends (Anastos 200Sa). Additionally, analysts at WSCF observed inconsistent TOX results among field sample replicates. Therefore, the WSCF lab performed an investigation of the TOX analysis to determine the cause of the outlier data points. Two causes were found that contributed to generating out-of-trend TOX data: (1) The presence of inorganic chloride in the groundwater samples: at inorganic chloride concentrations greater than about 10 parts per million (ppm), apparent TOX values increase with increasing chloride concentration. A parallel observation is the increase in apparent breakthrough of TOX from the first to the second activated-carbon adsorption tubes with increasing inorganic chloride concentration. (2) During the sample preparation step, excessive purging of the adsorption tubes with oxygen pressurization gas after sample loading may cause channeling in the activated carbon bed. This channeling leads to poor removal of inorganic chloride during the subsequent wash step with aqueous potassium nitrate. The presence of this residual inorganic chloride then produces erroneously high TOX values. Changes in sample preparation were studied to more effectively

Comparative of three sampling protocols for water quality assessment using macro invertebrates; Comparacion de tres protocolos de muestreo de macroinvertebrados para determinar la calidad del agua

Energy Technology Data Exchange (ETDEWEB)

Puertolas Domenech, L.; Rieradevall Sant, M.; Prat Fornells, N.

2007-07-01

The implementation of the Water Framework directive (WFD, Directive 2000/60/CE) requires the establishment of standardized sampling protocols for the assessment of benthic fauna. In this paper, a comparative study of several sampling protocols that are used currently in Spain and Europe (AQEM, EPA and Guadalmed) has been carried out. Evaluating the three protocols with a list of 12 criteria, Guadalmed fits better to the most of them. therefore it appears as an efficient tool in the determination of Ecological Status. (Author)

Analytical validation of a reference laboratory ELISA for the detection of feline leukemia virus p27 antigen.

Science.gov (United States)

Buch, Jesse S; Clark, Genevieve H; Cahill, Roberta; Thatcher, Brendon; Smith, Peter; Chandrashekar, Ramaswamy; Leutenegger, Christian M; O'Connor, Thomas P; Beall, Melissa J

2017-09-01

Feline leukemia virus (FeLV) is an oncogenic retrovirus of cats. Immunoassays for the p27 core protein of FeLV aid in the detection of FeLV infections. Commercial microtiter-plate ELISAs have rapid protocols and visual result interpretation, limiting their usefulness in high-throughput situations. The purpose of our study was to validate the PetChek FeLV 15 ELISA, which is designed for the reference laboratory, and incorporates sequential, orthogonal screening and confirmatory protocols. A cutoff for the screening assay was established with 100% accuracy using 309 feline samples (244 negative, 65 positive) defined by the combined results of FeLV PCR and an independent reference p27 antigen ELISA. Precision of the screening assay was measured using a panel of 3 samples (negative, low-positive, and high-positive). The intra-assay coefficient of variation (CV) was 3.9-7.9%; the inter-assay CV was 6.0-8.6%. For the confirmatory assay, the intra-assay CV was 3.0-4.7%, and the inter-assay CV was 7.4-9.7%. The analytical sensitivity for p27 antigen was 3.7 ng/mL for inactivated whole FeLV and 1.2 ng/mL for purified recombinant FeLV p27. Analytical specificity was demonstrated based on the absence of cross-reactivity to related retroviruses. No interference was observed for samples containing added bilirubin, hemoglobin, or lipids. Based on these results, the new high-throughput design of the PetChek FeLV 15 ELISA makes it suitable for use in reference laboratory settings and maintains overall analytical performance.

Big data analytics : predicting traffic flow regimes from simulated connected vehicle messages using data analytics and machine learning.

Science.gov (United States)

2016-12-25

The key objectives of this study were to: 1. Develop advanced analytical techniques that make use of a dynamically configurable connected vehicle message protocol to predict traffic flow regimes in near-real time in a virtual environment and examine ...

Summarizing documentation of the laboratory automation system RADAR for the analytical services of a nuclear fuel reprocessing facility

International Nuclear Information System (INIS)

Brandenburg, G.; Brocke, W.; Brodda, B.G.; Buerger, K.; Halling, H.; Heer, H.; Puetz, K.; Schaedlich, W.; Watzlawik, K.H.

1981-12-01

The essential tasks of the system are on-line open-loop process control based on in-line measurements and automation of the off-line analytical laboratory. The in-line measurements (at 55 tanks of the chemical process area) provide density-, liquid-, level-, and temperature values. The concentration value of a single component may easily be determined, if the solution consists of no more than two phases. The automation of the off-line analytical laboratory contains laboratory organization including sample management and data organization and computer-aided sample transportation control, data acquisition and data processing at chemical and nuclear analytical devices. The computer system consists of two computer-subsystems: a front end system for sample central registration and in-line process control and a central size system for the off-line analytical tasks. The organization of the application oriented system uses a centralized data base. Similar data processing functions concerning different analytical management tasks are structured into the following subsystem: man machine interface, interrupt- and data acquisition system, data base, protocol service and data processing. The procedures for the laboratory management (organization and experiment sequences) are defined by application data bases. Following the project phases, engineering requirements-, design-, assembly-, start up- and test run phase are described. In addition figures on expenditure and experiences are given and the system concept is discussed. (orig./HP) [de

Integration of GC-MSD and ER-Calux® assay into a single protocol for determining steroid estrogens in environmental samples.

Science.gov (United States)

Avberšek, Miha; Žegura, Bojana; Filipič, Metka; Heath, Ester

2011-11-01

There are many published studies that use either chemical or biological methods to investigate steroid estrogens in the aquatic environment, but rarer are those that combine both. In this study, gas chromatography with mass selective detection (GC-MSD) and the ER-Calux(®) estrogenicity assay were integrated into a single protocol for simultaneous determination of natural (estrone--E1, 17β-estradiol--E2, estriol--E3) and synthetic (17α-ethinylestradiol--EE2) steroid estrogens concentrations and the total estrogenic potential of environmental samples. For integration purposes, several solvents were investigated and the commonly used dimethyl sulphoxide (DMSO) in the ER-Calux(®) assay was replaced by ethyl acetate, which is more compatible with gas chromatography and enables the same sample to be analysed by both GC-MSD and the ER-Calux(®) assay. The integrated protocol was initially tested using a standard mixture of estrogens. The results for pure standards showed that the estrogenicity calculated on the basis of GC-MSD and the ER-Calux(®) assay exhibited good correlation (r(2)=0.96; α=0.94). The result remained the same when spiked waste water extracts were tested (r(2)=0.92, α=1.02). When applied to real waste water influent and effluent samples the results proved (r(2)=0.93; α=0.99) the applicability of the protocol. The main advantages of this newly developed protocol are simple sample handling for both methods, and reduced material consumption and labour. In addition, it can be applied as either a complete or sequential analysis where the ER-Calux(®) assay is used as a pre-screening method prior to the chemical analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Analytical Method to Estimate the Complex Permittivity of Oil Samples

Directory of Open Access Journals (Sweden)

Lijuan Su

2018-03-01

Full Text Available In this paper, an analytical method to estimate the complex dielectric constant of liquids is presented. The method is based on the measurement of the transmission coefficient in an embedded microstrip line loaded with a complementary split ring resonator (CSRR, which is etched in the ground plane. From this response, the dielectric constant and loss tangent of the liquid under test (LUT can be extracted, provided that the CSRR is surrounded by such LUT, and the liquid level extends beyond the region where the electromagnetic fields generated by the CSRR are present. For that purpose, a liquid container acting as a pool is added to the structure. The main advantage of this method, which is validated from the measurement of the complex dielectric constant of olive and castor oil, is that reference samples for calibration are not required.

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site-Working towards a toolbox for better assessment.

Science.gov (United States)

Wroble, Julie; Frederick, Timothy; Frame, Alicia; Vallero, Daniel

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)'s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete ("grab") samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples.

Waste sampling and characterization facility (WSCF)

International Nuclear Information System (INIS)

1994-10-01

The Waste Sampling and Characterization Facility (WSCF) complex consists of the main structure (WSCF) and four support structures located in the 600 Area of the Hanford site east of the 200 West area and south of the Hanford Meterology Station. WSCF is to be used for low level sample analysis, less than 2 mRem. The Laboratory features state-of-the-art analytical and low level radiological counting equipment for gaseous, soil, and liquid sample analysis. In particular, this facility is to be used to perform Resource Conservation and Recovery Act (RCRA) of 1976 and Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) of 1980 sample analysis in accordance with U.S. Environmental Protection Agency Protocols, room air and stack monitoring sample analysis, waste water treatment process support, and contractor laboratory quality assurance checks. The samples to be analyzed contain very low concentrations of radioisotopes. The main reason that WSCF is considered a Nuclear Facility is due to the storage of samples at the facility. This maintenance Implementation Plan has been developed for maintenace functions associate with the WSCF

Addressing the need for biomarker liquid chromatography/mass spectrometry assays: a protocol for effective method development for the bioanalysis of endogenous compounds in cerebrospinal fluid.

Science.gov (United States)

Benitex, Yulia; McNaney, Colleen A; Luchetti, David; Schaeffer, Eric; Olah, Timothy V; Morgan, Daniel G; Drexler, Dieter M

2013-08-30

Research on disorders of the central nervous system (CNS) has shown that an imbalance in the levels of specific endogenous neurotransmitters may underlie certain CNS diseases. These alterations in neurotransmitter levels may provide insight into pathophysiology, but can also serve as disease and pharmacodynamic biomarkers. To measure these potential biomarkers in vivo, the relevant sample matrix is cerebrospinal fluid (CSF), which is in equilibrium with the brain's interstitial fluid and circulates through the ventricular system of the brain and spinal cord. Accurate analysis of these potential biomarkers can be challenging due to low CSF sample volume, low analyte levels, and potential interferences from other endogenous compounds. A protocol has been established for effective method development of bioanalytical assays for endogenous compounds in CSF. Database searches and standard-addition experiments are employed to qualify sample preparation and specificity of the detection thus evaluating accuracy and precision. This protocol was applied to the study of the histaminergic neurotransmitter system and the analysis of histamine and its metabolite 1-methylhistamine in rat CSF. The protocol resulted in a specific and sensitive novel method utilizing pre-column derivatization ultra high performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS), which is also capable of separating an endogenous interfering compound, identified as taurine, from the analytes of interest. Copyright © 2013 John Wiley & Sons, Ltd.

Optimisation (sampling strategies and analytical procedures) for site specific environment monitoring at the areas of uranium production legacy sites in Ukraine - 59045

International Nuclear Information System (INIS)

Voitsekhovych, Oleg V.; Lavrova, Tatiana V.; Kostezh, Alexander B.

2012-01-01

There are many sites in the world, where Environment are still under influence of the contamination related to the Uranium production carried out in past. Author's experience shows that lack of site characterization data, incomplete or unreliable environment monitoring studies can significantly limit quality of Safety Assessment procedures and Priority actions analyses needed for Remediation Planning. During recent decades the analytical laboratories of the many enterprises, currently being responsible for establishing the site specific environment monitoring program have been significantly improved their technical sampling and analytical capacities. However, lack of experience in the optimal site specific sampling strategy planning and also not enough experience in application of the required analytical techniques, such as modern alpha-beta radiometers, gamma and alpha spectrometry and liquid-scintillation analytical methods application for determination of U-Th series radionuclides in the environment, does not allow to these laboratories to develop and conduct efficiently the monitoring programs as a basis for further Safety Assessment in decision making procedures. This paper gives some conclusions, which were gained from the experience establishing monitoring programs in Ukraine and also propose some practical steps on optimization in sampling strategy planning and analytical procedures to be applied for the area required Safety assessment and justification for its potential remediation and safe management. (authors)

Sample handling in surface sensitive chemical and biological sensing: a practical review of basic fluidics and analyte transport.

Science.gov (United States)

Orgovan, Norbert; Patko, Daniel; Hos, Csaba; Kurunczi, Sándor; Szabó, Bálint; Ramsden, Jeremy J; Horvath, Robert

2014-09-01

This paper gives an overview of the advantages and associated caveats of the most common sample handling methods in surface-sensitive chemical and biological sensing. We summarize the basic theoretical and practical considerations one faces when designing and assembling the fluidic part of the sensor devices. The influence of analyte size, the use of closed and flow-through cuvettes, the importance of flow rate, tubing length and diameter, bubble traps, pressure-driven pumping, cuvette dead volumes, and sample injection systems are all discussed. Typical application areas of particular arrangements are also highlighted, such as the monitoring of cellular adhesion, biomolecule adsorption-desorption and ligand-receptor affinity binding. Our work is a practical review in the sense that for every sample handling arrangement considered we present our own experimental data and critically review our experience with the given arrangement. In the experimental part we focus on sample handling in optical waveguide lightmode spectroscopy (OWLS) measurements, but the present study is equally applicable for other biosensing technologies in which an analyte in solution is captured at a surface and its presence is monitored. Explicit attention is given to features that are expected to play an increasingly decisive role in determining the reliability of (bio)chemical sensing measurements, such as analyte transport to the sensor surface; the distorting influence of dead volumes in the fluidic system; and the appropriate sample handling of cell suspensions (e.g. their quasi-simultaneous deposition). At the appropriate places, biological aspects closely related to fluidics (e.g. cellular mechanotransduction, competitive adsorption, blood flow in veins) are also discussed, particularly with regard to their models used in biosensing. Copyright © 2014 Elsevier B.V. All rights reserved.

Connectivity-Based Reliable Multicast MAC Protocol for IEEE 802.11 Wireless LANs

Directory of Open Access Journals (Sweden)

Woo-Yong Choi

2009-01-01

Full Text Available We propose the efficient reliable multicast MAC protocol based on the connectivity information among the recipients. Enhancing the BMMM (Batch Mode Multicast MAC protocol, the reliable multicast MAC protocol significantly reduces the RAK (Request for ACK frame transmissions in a reasonable computational time and enhances the MAC performance. By the analytical performance analysis, the throughputs of the BMMM protocol and our proposed MAC protocol are derived. Numerical examples show that our proposed MAC protocol increases the reliable multicast MAC performance for IEEE 802.11 wireless LANs.

A 'smart' tube holder enables real-time sample monitoring in a standard lab centrifuge.

Science.gov (United States)

Hoang, Tony; Moskwa, Nicholas; Halvorsen, Ken

2018-01-01

The centrifuge is among the oldest and most widely used pieces of laboratory equipment, with significant applications that include clinical diagnostics and biomedical research. A major limitation of laboratory centrifuges is their "black box" nature, limiting sample observation to before and after centrifugation. Thus, optimized protocols require significant trial and error, while unoptimized protocols waste time by centrifuging longer than necessary or material due to incomplete sedimentation. Here, we developed an instrumented centrifuge tube receptacle compatible with several commercial benchtop centrifuges that can provide real-time sample analysis during centrifugation. We demonstrated the system by monitoring cell separations during centrifugation for different spin speeds, concentrations, buffers, cell types, and temperatures. We show that the collected data are valuable for analytical purposes (e.g. quality control), or as feedback to the user or the instrument. For the latter, we verified an adaptation where complete sedimentation turned off the centrifuge and notified the user by a text message. Our system adds new functionality to existing laboratory centrifuges, saving users time and providing useful feedback. This add-on potentially enables new analytical applications for an instrument that has remained largely unchanged for decades.

A Standardized and Reproducible Urine Preparation Protocol for Cancer Biomarkers Discovery

Directory of Open Access Journals (Sweden)

Julia Beretov

2014-01-01

Full Text Available A suitable and standardized protein purification technique is essential to maintain consistency and to allow data comparison between proteomic studies for urine biomarker discovery. Ultimately, efforts should be made to standardize urine preparation protocols. The aim of this study was to develop an optimal analytical protocol to achieve maximal protein yield and to ensure that this method was applicable to examine urine protein patterns that distinguish disease and disease-free states. In this pilot study, we compared seven different urine sample preparation methods to remove salts, and to precipitate and isolate urinary proteins. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE profiles showed that the sequential preparation of urinary proteins by combining acetone and trichloroacetic acid (TCA alongside high speed centrifugation (HSC provided the best separation, and retained the most urinary proteins. Therefore, this approach is the preferred method for all further urine protein analysis.

Toxoplasma gondii and pre-treatment protocols for polymerase chain reaction analysis of milk samples: a field trial in sheep from Southern Italy

Directory of Open Access Journals (Sweden)

Alice Vismarra

2017-02-01

Full Text Available Toxoplasmosis is a zoonotic disease caused by the protozoan Toxoplasma gondii. Ingestion of raw milk has been suggested as a risk for transmission to humans. Here the authors evaluated pre-treatment protocols for DNA extraction on T. gondii tachyzoite-spiked sheep milk with the aim of identifying the method that resulted in the most rapid and reliable polymerase chain reaction (PCR positivity. This protocol was then used to analyse milk samples from sheep of three different farms in Southern Italy, including real time PCR for DNA quantification and PCR-restriction fragment length polymorphism for genotyping. The pre-treatment protocol using ethylenediaminetetraacetic acid and Tris-HCl to remove casein gave the best results in the least amount of time compared to the others on spiked milk samples. One sample of 21 collected from sheep farms was positive on one-step PCR, real time PCR and resulted in a Type I genotype at one locus (SAG3. Milk usually contains a low number of tachyzoites and this could be a limiting factor for molecular identification. Our preliminary data has evaluated a rapid, cost-effective and sensitive protocol to treat milk before DNA extraction. The results of the present study also confirm the possibility of T. gondii transmission through consumption of raw milk and its unpasteurised derivatives.

Collaborative Visual Analytics: A Health Analytics Approach to Injury Prevention

Directory of Open Access Journals (Sweden)

Samar Al-Hajj

2017-09-01

Full Text Available Background: Accurate understanding of complex health data is critical in order to deal with wicked health problems and make timely decisions. Wicked problems refer to ill-structured and dynamic problems that combine multidimensional elements, which often preclude the conventional problem solving approach. This pilot study introduces visual analytics (VA methods to multi-stakeholder decision-making sessions about child injury prevention; Methods: Inspired by the Delphi method, we introduced a novel methodology—group analytics (GA. GA was pilot-tested to evaluate the impact of collaborative visual analytics on facilitating problem solving and supporting decision-making. We conducted two GA sessions. Collected data included stakeholders’ observations, audio and video recordings, questionnaires, and follow up interviews. The GA sessions were analyzed using the Joint Activity Theory protocol analysis methods; Results: The GA methodology triggered the emergence of ‘common ground’ among stakeholders. This common ground evolved throughout the sessions to enhance stakeholders’ verbal and non-verbal communication, as well as coordination of joint activities and ultimately collaboration on problem solving and decision-making; Conclusions: Understanding complex health data is necessary for informed decisions. Equally important, in this case, is the use of the group analytics methodology to achieve ‘common ground’ among diverse stakeholders about health data and their implications.

Collaborative Visual Analytics: A Health Analytics Approach to Injury Prevention.

Science.gov (United States)

Al-Hajj, Samar; Fisher, Brian; Smith, Jennifer; Pike, Ian

2017-09-12

Background : Accurate understanding of complex health data is critical in order to deal with wicked health problems and make timely decisions. Wicked problems refer to ill-structured and dynamic problems that combine multidimensional elements, which often preclude the conventional problem solving approach. This pilot study introduces visual analytics (VA) methods to multi-stakeholder decision-making sessions about child injury prevention; Methods : Inspired by the Delphi method, we introduced a novel methodology-group analytics (GA). GA was pilot-tested to evaluate the impact of collaborative visual analytics on facilitating problem solving and supporting decision-making. We conducted two GA sessions. Collected data included stakeholders' observations, audio and video recordings, questionnaires, and follow up interviews. The GA sessions were analyzed using the Joint Activity Theory protocol analysis methods; Results : The GA methodology triggered the emergence of ' common g round ' among stakeholders. This common ground evolved throughout the sessions to enhance stakeholders' verbal and non-verbal communication, as well as coordination of joint activities and ultimately collaboration on problem solving and decision-making; Conclusion s : Understanding complex health data is necessary for informed decisions. Equally important, in this case, is the use of the group analytics methodology to achieve ' common ground' among diverse stakeholders about health data and their implications.

Inter-comparison of NIOSH and IMPROVE protocols for OC and EC determination: implications for inter-protocol data conversion

Science.gov (United States)

Wu, Cheng; Huang, X. H. Hilda; Ng, Wai Man; Griffith, Stephen M.; Zhen Yu, Jian

2016-09-01

Organic carbon (OC) and elemental carbon (EC) are operationally defined by analytical methods. As a result, OC and EC measurements are protocol dependent, leading to uncertainties in their quantification. In this study, more than 1300 Hong Kong samples were analyzed using both National Institute for Occupational Safety and Health (NIOSH) thermal optical transmittance (TOT) and Interagency Monitoring of Protected Visual Environment (IMPROVE) thermal optical reflectance (TOR) protocols to explore the cause of EC disagreement between the two protocols. EC discrepancy mainly (83 %) arises from a difference in peak inert mode temperature, which determines the allocation of OC4NSH, while the rest (17 %) is attributed to a difference in the optical method (transmittance vs. reflectance) applied for the charring correction. Evidence shows that the magnitude of the EC discrepancy is positively correlated with the intensity of the biomass burning signal, whereby biomass burning increases the fraction of OC4NSH and widens the disagreement in the inter-protocol EC determination. It is also found that the EC discrepancy is positively correlated with the abundance of metal oxide in the samples. Two approaches (M1 and M2) that translate NIOSH TOT OC and EC data into IMPROVE TOR OC and EC data are proposed. M1 uses direct relationship between ECNSH_TOT and ECIMP_TOR for reconstruction: M1 : ECIMP_TOR = a × ECNSH_TOT + b; while M2 deconstructs ECIMP_TOR into several terms based on analysis principles and applies regression only on the unknown terms: M2 : ECIMP_TOR = AECNSH + OC4NSH - (a × PCNSH_TOR + b), where AECNSH, apparent EC by the NIOSH protocol, is the carbon that evolves in the He-O2 analysis stage, OC4NSH is the carbon that evolves at the fourth temperature step of the pure helium analysis stage of NIOSH, and PCNSH_TOR is the pyrolyzed carbon as determined by the NIOSH protocol. The implementation of M1 to all urban site data (without considering seasonal specificity

Pre-analytical and analytical factors influencing Alzheimer's disease cerebrospinal fluid biomarker variability.

Science.gov (United States)

Fourier, Anthony; Portelius, Erik; Zetterberg, Henrik; Blennow, Kaj; Quadrio, Isabelle; Perret-Liaudet, Armand

2015-09-20

A panel of cerebrospinal fluid (CSF) biomarkers including total Tau (t-Tau), phosphorylated Tau protein at residue 181 (p-Tau) and β-amyloid peptides (Aβ42 and Aβ40), is frequently used as an aid in Alzheimer's disease (AD) diagnosis for young patients with cognitive impairment, for predicting prodromal AD in mild cognitive impairment (MCI) subjects, for AD discrimination in atypical clinical phenotypes and for inclusion/exclusion and stratification of patients in clinical trials. Due to variability in absolute levels between laboratories, there is no consensus on medical cut-off value for the CSF AD signature. Thus, for full implementation of this core AD biomarker panel in clinical routine, this issue has to be solved. Variability can be explained both by pre-analytical and analytical factors. For example, the plastic tubes used for CSF collection and storage, the lack of reference material and the variability of the analytical protocols were identified as important sources of variability. The aim of this review is to highlight these pre-analytical and analytical factors and describe efforts done to counteract them in order to establish cut-off values for core CSF AD biomarkers. This review will give the current state of recommendations. Copyright © 2015. Published by Elsevier B.V.

Analytical and between-subject variation of thrombin generation measured by calibrated automated thrombography on plasma samples.

Science.gov (United States)

Kristensen, Anne F; Kristensen, Søren R; Falkmer, Ursula; Münster, Anna-Marie B; Pedersen, Shona

2018-05-01

The Calibrated Automated Thrombography (CAT) is an in vitro thrombin generation (TG) assay that holds promise as a valuable tool within clinical diagnostics. However, the technique has a considerable analytical variation, and we therefore, investigated the analytical and between-subject variation of CAT systematically. Moreover, we assess the application of an internal standard for normalization to diminish variation. 20 healthy volunteers donated one blood sample which was subsequently centrifuged, aliquoted and stored at -80 °C prior to analysis. The analytical variation was determined on eight runs, where plasma from the same seven volunteers was processed in triplicates, and for the between-subject variation, TG analysis was performed on plasma from all 20 volunteers. The trigger reagents used for the TG assays included both PPP reagent containing 5 pM tissue factor (TF) and PPPlow with 1 pM TF. Plasma, drawn from a single donor, was applied to all plates as an internal standard for each TG analysis, which subsequently was used for normalization. The total analytical variation for TG analysis performed with PPPlow reagent is 3-14% and 9-13% for PPP reagent. This variation can be minimally reduced by using an internal standard but mainly for ETP (endogenous thrombin potential). The between-subject variation is higher when using PPPlow than PPP and this variation is considerable higher than the analytical variation. TG has a rather high inherent analytical variation but considerable lower than the between-subject variation when using PPPlow as reagent.

Sample preparation combined with electroanalysis to improve simultaneous determination of antibiotics in animal derived food samples.

Science.gov (United States)

da Silva, Wesley Pereira; de Oliveira, Luiz Henrique; Santos, André Luiz Dos; Ferreira, Valdir Souza; Trindade, Magno Aparecido Gonçalves

2018-06-01

A procedure based on liquid-liquid extraction (LLE) and phase separation using magnetically stirred salt-induced high-temperature liquid-liquid extraction (PS-MSSI-HT-LLE) was developed to extract and pre-concentrate ciprofloxacin (CIPRO) and enrofloxacin (ENRO) from animal food samples before electroanalysis. Firstly, simple LLE was used to extract the fluoroquinolones (FQs) from animal food samples, in which dilution was performed to reduce interference effects to below a tolerable threshold. Then, adapted PS-MSSI-HT-LLE protocols allowed re-extraction and further pre-concentration of target analytes in the diluted acid samples for simultaneous electrochemical quantification at low concentration levels. To improve the peak separation, in simultaneous detection, a baseline-corrected second-order derivative approach was processed. These approaches allowed quantification of target FQs from animal food samples spiked at levels of 0.80 to 2.00 µmol L -1 in chicken meat, with recovery values always higher than 80.5%, as well as in milk samples spiked at 4.00 µmol L -1 , with recovery values close to 70.0%. Copyright © 2018 Elsevier Ltd. All rights reserved.

Interlaboratory test comparison among Environmental Radioactivity Laboratories using the ISO/IUPAC/AOAC Protocol

International Nuclear Information System (INIS)

Romero, L.; Ramos, L.; Salas, R.

1998-01-01

World-wide acceptance of results from radiochemical analyses requires reliable, traceable and comparable measurements to SI units, particularly when data sets generated by laboratories are to contribute to evaluation of data from environmental pollution research and monitoring programmes. The Spanish Nuclear Safety Council (CSN) organizes in collaboration with CIEMAT periodical interlaboratory test comparisons for environmental radioactivity laboratories aiming to provide them with the necessary means to asses the quality of their results. This paper presents data from the most recent exercise which, for the first time, was evaluated following the procedure recommended in the ISO/IUPAC/AOAC Harmonized Protocol for the proficiency testing of analytical laboratories (1). The test sample was a Reference Material provided by the IAEA-AQCS, a lake sediment containing the following radionuclides: k-40, Ra-226, Ac-228, Cs-137, Sr-90, Pu-(239+240). The results of the proficiency test were computed for the 28 participating laboratories using the z-score approach, the evaluation of the exercises is presented in the paper. The use of a z-score classification has demonstrated to provide laboratories with a more objective means of assessing and demonstrating the reliability of the data they are producing. Analytical proficiency of the participating laboratories has been found to be satisfactory in 57 to 100 percent of cases. (1)- The International harmonized protocol for the proficiency testing of (chemical) analytical laboratories. Pure and Appl. Chem. Vol. 65, n 9, pp. 2123-2144, 1993 IUPAC. GB (Author) 3 refs

Analytical results for 544 water samples collected in the Attean Quartz Monzonite in the vicinity of Jackman, Maine

Science.gov (United States)

Ficklin, W.H.; Nowlan, G.A.; Preston, D.J.

1983-01-01

Water samples were collected in the vicinity of Jackman, Maine as a part of the study of the relationship of dissolved constituents in water to the sediments subjacent to the water. Each sample was analyzed for specific conductance, alkalinity, acidity, pH, fluoride, chloride, sulfate, phosphate, nitrate, sodium, potassium, calcium, magnesium, and silica. Trace elements determined were copper, zinc, molybdenum, lead, iron, manganese, arsenic, cobalt, nickel, and strontium. The longitude and latitude of each sample location and a sample site map are included in the report as well as a table of the analytical results.

Security of Semi-Device-Independent Random Number Expansion Protocols.

Science.gov (United States)

Li, Dan-Dan; Wen, Qiao-Yan; Wang, Yu-Kun; Zhou, Yu-Qian; Gao, Fei

2015-10-27

Semi-device-independent random number expansion (SDI-RNE) protocols require some truly random numbers to generate fresh ones, with making no assumptions on the internal working of quantum devices except for the dimension of the Hilbert space. The generated randomness is certified by non-classical correlation in the prepare-and-measure test. Until now, the analytical relations between the amount of the generated randomness and the degree of non-classical correlation, which are crucial for evaluating the security of SDI-RNE protocols, are not clear under both the ideal condition and the practical one. In the paper, first, we give the analytical relation between the above two factors under the ideal condition. As well, we derive the analytical relation under the practical conditions, where devices' behavior is not independent and identical in each round and there exists deviation in estimating the non-classical behavior of devices. Furthermore, we choose a different randomness extractor (i.e., two-universal random function) and give the security proof.

A ‘smart’ tube holder enables real-time sample monitoring in a standard lab centrifuge

Science.gov (United States)

Hoang, Tony; Moskwa, Nicholas

2018-01-01

The centrifuge is among the oldest and most widely used pieces of laboratory equipment, with significant applications that include clinical diagnostics and biomedical research. A major limitation of laboratory centrifuges is their “black box” nature, limiting sample observation to before and after centrifugation. Thus, optimized protocols require significant trial and error, while unoptimized protocols waste time by centrifuging longer than necessary or material due to incomplete sedimentation. Here, we developed an instrumented centrifuge tube receptacle compatible with several commercial benchtop centrifuges that can provide real-time sample analysis during centrifugation. We demonstrated the system by monitoring cell separations during centrifugation for different spin speeds, concentrations, buffers, cell types, and temperatures. We show that the collected data are valuable for analytical purposes (e.g. quality control), or as feedback to the user or the instrument. For the latter, we verified an adaptation where complete sedimentation turned off the centrifuge and notified the user by a text message. Our system adds new functionality to existing laboratory centrifuges, saving users time and providing useful feedback. This add-on potentially enables new analytical applications for an instrument that has remained largely unchanged for decades. PMID:29659624

A Protocol Layer Trust-Based Intrusion Detection Scheme for Wireless Sensor Networks

Directory of Open Access Journals (Sweden)

Jian Wang

2017-05-01

Full Text Available This article proposes a protocol layer trust-based intrusion detection scheme for wireless sensor networks. Unlike existing work, the trust value of a sensor node is evaluated according to the deviations of key parameters at each protocol layer considering the attacks initiated at different protocol layers will inevitably have impacts on the parameters of the corresponding protocol layers. For simplicity, the paper mainly considers three aspects of trustworthiness, namely physical layer trust, media access control layer trust and network layer trust. The per-layer trust metrics are then combined to determine the overall trust metric of a sensor node. The performance of the proposed intrusion detection mechanism is then analyzed using the t-distribution to derive analytical results of false positive and false negative probabilities. Numerical analytical results, validated by simulation results, are presented in different attack scenarios. It is shown that the proposed protocol layer trust-based intrusion detection scheme outperforms a state-of-the-art scheme in terms of detection probability and false probability, demonstrating its usefulness for detecting cross-layer attacks.

Analytical Chemistry Laboratory (ACL) procedure compendium

International Nuclear Information System (INIS)

1992-06-01

Covered are: analytical laboratory operations (ALO) sample receipt and control, ALO data report/package preparation review and control, single shell tank (PST) project sample tracking system, sample receiving, analytical balances, duties and responsibilities of sample custodian, sample refrigerator temperature monitoring, security, assignment of staff responsibilities, sample storage, data reporting, and general requirements for glassware

Improved online δ18O measurements of nitrogen- and sulfur-bearing organic materials and a proposed analytical protocol

Science.gov (United States)

Qi, H.; Coplen, T.B.; Wassenaar, L.I.

2011-01-01

It is well known that N2 in the ion source of a mass spectrometer interferes with the CO background during the δ18O measurement of carbon monoxide. A similar problem arises with the high-temperature conversion (HTC) analysis of nitrogenous O-bearing samples (e.g. nitrates and keratins) to CO for δ18O measurement, where the sample introduces a significant N2 peak before the CO peak, making determination of accurate oxygen isotope ratios difficult. Although using a gas chromatography (GC) column longer than that commonly provided by manufacturers (0.6 m) can improve the efficiency of separation of CO and N2 and using a valve to divert nitrogen and prevent it from entering the ion source of a mass spectrometer improved measurement results, biased δ18O values could still be obtained. A careful evaluation of the performance of the GC separation column was carried out. With optimal GC columns, the δ18O reproducibility of human hair keratins and other keratin materials was better than ±0.15 ‰ (n = 5; for the internal analytical reproducibility), and better than ±0.10 ‰ (n = 4; for the external analytical reproducibility).

Automated Ground-Water Sampling and Analysis of Hexavalent Chromium using a “Universal” Sampling/Analytical System

Directory of Open Access Journals (Sweden)

Richard J. Venedam

2005-02-01

Full Text Available The capabilities of a “universal platform” for the deployment of analyticalsensors in the field for long-term monitoring of environmental contaminants were expandedin this investigation. The platform was previously used to monitor trichloroethene inmonitoring wells and at groundwater treatment systems (1,2. The platform was interfacedwith chromium (VI and conductivity analytical systems to monitor shallow wells installedadjacent to the Columbia River at the 100-D Area of the Hanford Site, Washington. Agroundwater plume of hexavalent chromium is discharging into the Columbia River throughthe gravels beds used by spawning salmon. The sampling/analytical platform was deployedfor the purpose of collecting data on subsurface hexavalent chromium concentrations atmore frequent intervals than was possible with the previous sampling and analysis methodsemployed a the Site.

Next Generation Offline Approaches to Trace Gas-Phase Organic Compound Speciation: Sample Collection and Analysis

Science.gov (United States)

Sheu, R.; Marcotte, A.; Khare, P.; Ditto, J.; Charan, S.; Gentner, D. R.

2017-12-01

Intermediate-volatility and semi-volatile organic compounds (I/SVOCs) are major precursors to secondary organic aerosol, and contribute to tropospheric ozone formation. Their wide volatility range, chemical complexity, behavior in analytical systems, and trace concentrations present numerous hurdles to characterization. We present an integrated sampling-to-analysis system for the collection and offline analysis of trace gas-phase organic compounds with the goal of preserving and recovering analytes throughout sample collection, transport, storage, and thermal desorption for accurate analysis. Custom multi-bed adsorbent tubes are used to collect samples for offline analysis by advanced analytical detectors. The analytical instrumentation comprises an automated thermal desorption system that introduces analytes from the adsorbent tubes into a gas chromatograph, which is coupled with an electron ionization mass spectrometer (GC-EIMS) and other detectors. In order to optimize the collection and recovery for a wide range of analyte volatility and functionalization, we evaluated a variety of commercially-available materials, including Res-Sil beads, quartz wool, glass beads, Tenax TA, and silica gel. Key properties for optimization include inertness, versatile chemical capture, minimal affinity for water, and minimal artifacts or degradation byproducts; these properties were assessed with a diverse mix of traditionally-measured and functionalized analytes. Along with a focus on material selection, we provide recommendations spanning the entire sampling-and-analysis process to improve the accuracy of future comprehensive I/SVOC measurements, including oxygenated and other functionalized I/SVOCs. We demonstrate the performance of our system by providing results on speciated VOCs-SVOCs from indoor, outdoor, and chamber studies that establish the utility of our protocols and pave the way for precise laboratory characterization via a mix of detection methods.

Thermal/optical methods for elemental carbon quantification in soils and urban dusts: equivalence of different analysis protocols.

Directory of Open Access Journals (Sweden)

Yongming Han

Full Text Available Quantifying elemental carbon (EC content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT. A high-temperature method with extended heating times (STN120 showed the highest ECT/ECR ratio (0.86 while a low-temperature protocol (IMPROVE-550, with heating time adjusted for sample loading, showed the lowest (0.53. STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average than in soils (5.2 on average, most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method.

Thermal/optical methods for elemental carbon quantification in soils and urban dusts: equivalence of different analysis protocols.

Science.gov (United States)

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method.

Asymptotic performance modelling of DCF protocol with prioritized channel access

Science.gov (United States)

Choi, Woo-Yong

2017-11-01

Recently, the modification of the DCF (Distributed Coordination Function) protocol by the prioritized channel access was proposed to resolve the problem that the DCF performance worsens exponentially as more nodes exist in IEEE 802.11 wireless LANs. In this paper, an asymptotic analytical performance model is presented to analyze the MAC performance of the DCF protocol with the prioritized channel access.

Entanglement distillation protocols and number theory

International Nuclear Information System (INIS)

Bombin, H.; Martin-Delgado, M.A.

2005-01-01

We show that the analysis of entanglement distillation protocols for qudits of arbitrary dimension D benefits from applying basic concepts from number theory, since the set Z D n associated with Bell diagonal states is a module rather than a vector space. We find that a partition of Z D n into divisor classes characterizes the invariant properties of mixed Bell diagonal states under local permutations. We construct a very general class of recursion protocols by means of unitary operations implementing these local permutations. We study these distillation protocols depending on whether we use twirling operations in the intermediate steps or not, and we study them both analytically and numerically with Monte Carlo methods. In the absence of twirling operations, we construct extensions of the quantum privacy algorithms valid for secure communications with qudits of any dimension D. When D is a prime number, we show that distillation protocols are optimal both qualitatively and quantitatively

Possibilities for decreasing detection limits of analytical methods for determination of transformation products of unsymmetrical dimethylhydrazine in environmental samples

Directory of Open Access Journals (Sweden)

Bulat Kenessov

2015-12-01

Full Text Available Most rockets of middle and heavy class launched from Kazakhstan, Russia, China and other countries still use highly toxic unsymmetrical dimethylhydrazine (UDMH as a liquid propellant. Study of migration, distribution and accumulation of UDMH transformation products in environment and human health impact assessment of space rocket activity are currently complicated due to the absence of analytical methods allowing detection of trace concentrations of these compounds in analyzed samples. This paper reviews methods and approaches, which can be applied for development of such methods. Detection limits at a part-per-trillion (ppt level may be achieved using most selective and sensitive methods based on gas or liquid chromatography in combination of tandem or high-resolution mass spectrometry. In addition, 1000-fold concentration of samples or integrated sample preparation methods, e.g., dynamic headspace extraction, are required. Special attention during development and application of such methods must be paid to purity of laboratory air, reagents, glassware and analytical instruments.

Development of Characterization Protocol for Mixed Liquid Radioactive Waste Classification

International Nuclear Information System (INIS)

Norasalwa Zakaria; Syed Asraf Wafa; Wo, Y.M.; Sarimah Mahat; Mohamad Annuar Assadat Husain

2017-01-01

Mixed organic liquid waste generated from health-care and research activities containing tritium, carbon-14, and other radionuclide posed specific challenges in its management. Often, this waste becomes legacy waste in many nuclear facilities and being considered as 'problematic' waste. One of the most important recommendations made by IAEA is to perform multistage processes aiming at declassification of the waste. At this moment, approximately 3000 bottles of mixed liquid waste, with estimated volume of 6000 litres are currently stored at the National Radioactive Waste Management Centre, Malaysia and some have been stored for more than 25 years. The aim of this study is to develop a characterization protocol towards reclassification of these wastes. The characterization protocol entails waste identification, waste screening and segregation, and analytical radionuclides profiling using analytical procedures involving gross alpha beta, and gamma spectrometry. The results obtained from the characterization protocol are used to establish criteria for speedy classification of the waste. (author)

Development of characterization protocol for mixed liquid radioactive waste classification

Energy Technology Data Exchange (ETDEWEB)

Zakaria, Norasalwa, E-mail: norasalwa@nuclearmalaysia.gov.my [Waste Technology Development Centre, Malaysian Nuclear Agency, 43000 Kajang, Selangor (Malaysia); Wafa, Syed Asraf [Radioisotop Technology and Innovation, Malaysian Nuclear Agency, 43000 Kajang, Selangor (Malaysia); Wo, Yii Mei [Radiochemistry and Environment, Malaysian Nuclear Agency, 43000 Kajang, Selangor (Malaysia); Mahat, Sarimah [Material Technology Group, Malaysian Nuclear Agency, 43000 Kajang, Selangor (Malaysia)

2015-04-29

Mixed liquid organic waste generated from health-care and research activities containing tritium, carbon-14, and other radionuclides posed specific challenges in its management. Often, these wastes become legacy waste in many nuclear facilities and being considered as ‘problematic’ waste. One of the most important recommendations made by IAEA is to perform multistage processes aiming at declassification of the waste. At this moment, approximately 3000 bottles of mixed liquid waste, with estimated volume of 6000 litres are currently stored at the National Radioactive Waste Management Centre, Malaysia and some have been stored for more than 25 years. The aim of this study is to develop a characterization protocol towards reclassification of these wastes. The characterization protocol entails waste identification, waste screening and segregation, and analytical radionuclides profiling using various analytical procedures including gross alpha/ gross beta, gamma spectrometry, and LSC method. The results obtained from the characterization protocol are used to establish criteria for speedy classification of the waste.

Determination of hydrazine in drinking water: Development and multivariate optimization of a rapid and simple solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry protocol.

Science.gov (United States)

Gionfriddo, Emanuela; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

2014-07-04

In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GC-QqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simple derivatization reaction with propyl chloroformate and pyridine carried out directly in water samples, followed by automated SPME analysis in the same vial without further sample handling. The affinity of the different derivatized compounds obtained towards five commercially available SPME coatings was evaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GC-QqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed the achievement of high specificity by selecting appropriate precursor-product ion couples improving the capability in analyte identification. The multivariate approach of experimental design was crucial in order to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters. Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L(-1), provided satisfactory values (114.2%, 83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%, 7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L(-1) were obtained. The reliable application of the proposed protocol to real drinking water samples confirmed its capability to be used as analytical tool for routine analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of analytical techniques for water and environmental samples (2)

Energy Technology Data Exchange (ETDEWEB)

Eum, Chul Hun; Jeon, Chi Wan; Jung, Kang Sup; Song, Kyung Sun; Kim, Sang Yeon [Korea Institute of Geology Mining and Materials, Taejon (Korea)

1998-12-01

The purpose of this study is to develop new analytical methods with good detection limit for toxic inorganic and organic compounds. The analyses of CN, organic acids, particulate materials in environmental samples have been done using several methods such as Ion Chromatography, SPE, SPME, GC/MS, GC/FID, SPLITT (split-flow thin cell fractionation) during the second year of this project. Advantage and disadvantage of several distillation method (by KS, JIS, EPA) for CN analysis in wastewater were investigated. As the results, we proposed new distillation apparatus for CN analysis, which was proved to be simpler, faster and to get better recovery than conventional apparatus. And ion chromatograph/pulsed amperometric detector (IC/PAD) system instead of colorimetry for CN detection was setup to solve matrix interference. And SPE(solid phase extraction) and SPME (solid phase micro extraction) as liquid-solid extraction technique were applied to the analysis of phenols in wastewater. Optimum experimental conditions and factors influencing analytical results were determined. From these results, It could be concluded that C{sub 18} cartridge and polystyrene-divinylbenzene disk in SPE method, polyacrylate fiber in SPME were proper solid phase adsorbent for phenol. Optimum conditions to analyze phenol derivatives simultaneously were established. Also, Continuous SPLITT (Split-flow thin cell) Fractionation (CSF) is a new preparative separation technique that is useful for fractionation of particulate and macromolecular materials. CSF is carried out in a thin ribbon-like channel equipped with two splitters at both inlet and outlet of the channel. In this work, we set up a new CSF system, and tested using polystyrene latex standard particles. And then we fractionated particles contained in air and underground water based on their sedimentation coefficients using CSF. (author). 27 refs., 13 tabs., 31 figs.

Effects of fecal sampling on preanalytical and analytical phases in quantitative fecal immunochemical tests for hemoglobin.

Science.gov (United States)

Rapi, Stefano; Berardi, Margherita; Cellai, Filippo; Ciattini, Samuele; Chelazzi, Laura; Ognibene, Agostino; Rubeca, Tiziana

2017-07-24

Information on preanalytical variability is mandatory to bring laboratories up to ISO 15189 requirements. Fecal sampling is greatly affected by lack of harmonization in laboratory medicine. The aims of this study were to obtain information on the devices used for fecal sampling and to explore the effect of different amounts of feces on the results from the fecal immunochemical test for hemoglobin (FIT-Hb). Four commercial sample collection devices for quantitative FIT-Hb measurements were investigated. The volume of interest (VOI) of the probes was measured from diameter and geometry. Quantitative measurements of the mass of feces were carried out by gravimetry. The effects of an increased amount of feces on the analytical environment were investigated measuring the Hb values with a single analytical method. VOI was 8.22, 7.1 and 9.44 mm3 for probes that collected a target of 10 mg of feces, and 3.08 mm3 for one probe that targeted 2 mg of feces. The ratio between recovered and target amounts of devices ranged from 56% to 121%. Different changes in the measured Hb values were observed, in adding increasing amounts of feces in commercial buffers. The amounts of collected materials are related to the design of probes. Three out 4 manufacturers declare the same target amount using different sampling volumes and obtaining different amounts of collected materials. The introduction of a standard probes to reduce preanalytical variability could be an useful step for fecal test harmonization and to fulfill the ISO 15189 requirements.

Evaluation of the analytic performance of laboratories: inter-laboratorial study of the spectroscopy of atomic absorption

International Nuclear Information System (INIS)

Wong Wong, S. M.

1996-01-01

The author made an inter-laboratorial study, with the participation of 18 national laboratories, that have spectrophotometer of atomic absorption. To evaluate the methods of analysis of lead, sodium, potasium, calcium, magnesium, zinc, copper, manganese, and iron, in the ambit of mg/l. The samples, distributed in four rounds to the laboratories, were prepared from primary patterns, deionized and distilled water. The study evaluated the homogeneity and stability, and verified its concentration, using as a reference method, the spectrometry method of Inductively Coupled Plasma emission (1CP). To obtain the characteristics of analytic performance, it applied the norm ASTM E 691. To evaluated the analytic performance, it used harmonized protocol of the International Union of Pure and applied chemistry (IUPAC). The study obtained the 29% of the laboratories had a satisfactory analytic performance, 9% had a questionable performance and 62% made an unsatisfactory analytic performance, according to the IUPAC norm. The results of the values of the characteristic performance method, show that there is no intercomparability between the laboratories, which is attributed to the different methodologies of analysis. (S. Grainger)

Evaluation of analytical performance of a new high-sensitivity immunoassay for cardiac troponin I.

Science.gov (United States)

Masotti, Silvia; Prontera, Concetta; Musetti, Veronica; Storti, Simona; Ndreu, Rudina; Zucchelli, Gian Carlo; Passino, Claudio; Clerico, Aldo

2018-02-23

The study aim was to evaluate and compare the analytical performance of the new chemiluminescent immunoassay for cardiac troponin I (cTnI), called Access hs-TnI using DxI platform, with those of Access AccuTnI+3 method, and high-sensitivity (hs) cTnI method for ARCHITECT platform. The limits of blank (LoB), detection (LoD) and quantitation (LoQ) at 10% and 20% CV were evaluated according to international standardized protocols. For the evaluation of analytical performance and comparison of cTnI results, both heparinized plasma samples, collected from healthy subjects and patients with cardiac diseases, and quality control samples distributed in external quality assessment programs were used. LoB, LoD and LoQ at 20% and 10% CV values of the Access hs-cTnI method were 0.6, 1.3, 2.1 and 5.3 ng/L, respectively. Access hs-cTnI method showed analytical performance significantly better than that of Access AccuTnI+3 method and similar results to those of hs ARCHITECT cTnI method. Moreover, the cTnI concentrations measured with Access hs-cTnI method showed close linear regressions with both Access AccuTnI+3 and ARCHITECT hs-cTnI methods, although there were systematic differences between these methods. There was no difference between cTnI values measured by Access hs-cTnI in heparinized plasma and serum samples, whereas there was a significant difference between cTnI values, respectively measured in EDTA and heparin plasma samples. Access hs-cTnI has analytical sensitivity parameters significantly improved compared to Access AccuTnI+3 method and is similar to those of the high-sensitivity method using ARCHITECT platform.

Bioinspired Security Analysis of Wireless Protocols

DEFF Research Database (Denmark)

Petrocchi, Marinella; Spognardi, Angelo; Santi, Paolo

2016-01-01

work, this paper investigates feasibility of adopting fraglets as model for specifying security protocols and analysing their properties. In particular, we give concrete sample analyses over a secure RFID protocol, showing evolution of the protocol run as chemical dynamics and simulating an adversary...

Chapter 12. Sampling and analytical methods

International Nuclear Information System (INIS)

Busenberg, E.; Plummer, L.N.; Cook, P.G.; Solomon, D.K.; Han, L.F.; Groening, M.; Oster, H.

2006-01-01

When water samples are taken for the analysis of CFCs, regardless of the sampling method used, contamination of samples by contact with atmospheric air (with its 'high' CFC concentrations) is a major concern. This is because groundwaters usually have lower CFC concentrations than those waters which have been exposed to the modern air. Some groundwaters might not contain CFCs and, therefore, are most sensitive to trace contamination by atmospheric air. Thus, extreme precautions are needed to obtain uncontaminated samples when groundwaters, particularly those with older ages, are sampled. It is recommended at the start of any CFC investigation that samples from a CFC-free source be collected and analysed, as a check upon the sampling equipment and methodology. The CFC-free source might be a deep monitoring well or, alternatively, CFC-free water could be carefully prepared in the laboratory. It is especially important that all tubing, pumps and connection that will be used in the sampling campaign be checked in this manner

Urine sample preparation for proteomic analysis.

Science.gov (United States)

Olszowy, Pawel; Buszewski, Boguslaw

2014-10-01

Sample preparation for both environmental and more importantly biological matrices is a bottleneck of all kinds of analytical processes. In the case of proteomic analysis this element is even more important due to the amount of cross-reactions that should be taken into consideration. The incorporation of new post-translational modifications, protein hydrolysis, or even its degradation is possible as side effects of proteins sample processing. If protocols are evaluated appropriately, then identification of such proteins does not bring difficulties. However, if structural changes are provided without sufficient attention then protein sequence coverage will be reduced or even identification of such proteins could be impossible. This review summarizes obstacles and achievements in protein sample preparation of urine for proteome analysis using different tools for mass spectrometry analysis. The main aim is to present comprehensively the idea of urine application as a valuable matrix. This article is dedicated to sample preparation and application of urine mainly in novel cancer biomarkers discovery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of a lateral flow-based technology card for blood typing using a simplified protocol in a model of extreme blood sampling conditions.

Science.gov (United States)

Clavier, Benoît; Pouget, Thomas; Sailliol, Anne

2018-02-01

Life-threatening situations requiring blood transfusion under extreme conditions or in remote and austere locations, such as the battlefield or in traffic accidents, would benefit from reliable blood typing practices that are easily understood by a nonscientist or nonlaboratory technician and provide quick results. A simplified protocol was developed for the lateral flow-based device MDmulticard ABO-D-Rh subgroups-K. Its performance was compared to a reference method (PK7300, Beckman Coulter) in native blood samples from donors. The method was tested on blood samples stressed in vitro as a model of hemorrhage cases (through hemodilution using physiologic serum) and dehydration (through hemoconcentration by removing an aliquot of plasma after centrifugation), respectively. A total of 146 tests were performed on 52 samples; 126 in the hemodilution group (42 for each native, diluted 1/2, and diluted 1/4 samples) and 20 in the hemoconcentration group (10 for each native and 10% concentrated samples). Hematocrit in the tested samples ranged from 9.8% to 57.6% while hemoglobin levels ranged from 3.2 to 20.1 g/dL. The phenotype profile detected with the MDmulticard using the simplified protocol resulted in 22 A, seven B, 20 O, and three AB, of which nine were D- and five were Kell positive. No discrepancies were found with respect to the results obtained with the reference method. The simplified protocol for MDmulticard use could be considered a reliable method for blood typing in extreme environment or emergency situations, worsened by red blood cell dilution or concentration. © 2017 AABB.

SPIDIA-DNA: An External Quality Assessment for the pre-analytical phase of blood samples used for DNA-based analyses

Czech Academy of Sciences Publication Activity Database

Malentacchi, F.; Pazzagli, M.; Simi, L.; Orlando, C.; Wyrich, R.; Hartmann, C.C.; Verderio, P.; Pizzamiglio, S.; Ciniselli, C.M.; Tichopád, Aleš; Kubista, Mikael; Gelmini, S.

-, č. 424 (2013), s. 274-286 ISSN 0009-8981 Institutional research plan: CEZ:AV0Z50520701 Keywords : Pre-analytical phase * DNA quality * Blood samples Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.764, year: 2013

Data validation report for the 100-HR-3 Operable Unit first quarter 1994 groundwater sampling data

Energy Technology Data Exchange (ETDEWEB)

Biggerstaff, R.L.

1994-06-24

Westinghouse-Hanford has requested that a minimum of 20% of the total number of Sample Delivery Groups be validated for the 100-HR-3 Operable Unit First Quarter 1994 Groundwater Sampling Investigation. Therefore, the data from the chemical analysis of twenty-four samples from this sampling event and their related quality assurance samples were reviewed and validated to verify that reported sample results were of sufficient quality to support decisions regarding remedial actions performed at this site. The samples were analyzed by Thermo-Analytic Laboratories (TMA) and Roy F. Weston Laboratories (WESTON) using US Environmental Protection Agency (EPA) CLP protocols. Sample analyses included: inorganics; and general chemical parameters. Forty-two samples were validated for radiochemical parameters by TMA and Teledyne.

Data validation report for the 100-HR-3 Operable Unit first quarter 1994 groundwater sampling data

International Nuclear Information System (INIS)

Biggerstaff, R.L.

1994-01-01

Westinghouse-Hanford has requested that a minimum of 20% of the total number of Sample Delivery Groups be validated for the 100-HR-3 Operable Unit First Quarter 1994 Groundwater Sampling Investigation. Therefore, the data from the chemical analysis of twenty-four samples from this sampling event and their related quality assurance samples were reviewed and validated to verify that reported sample results were of sufficient quality to support decisions regarding remedial actions performed at this site. The samples were analyzed by Thermo-Analytic Laboratories (TMA) and Roy F. Weston Laboratories (WESTON) using US Environmental Protection Agency (EPA) CLP protocols. Sample analyses included: inorganics; and general chemical parameters. Forty-two samples were validated for radiochemical parameters by TMA and Teledyne

Dry sample storage system for an analytical laboratory supporting plutonium processing

International Nuclear Information System (INIS)

Treibs, H.A.; Hartenstein, S.D.; Griebenow, B.L.; Wade, M.A.

1990-01-01

The Special Isotope Separation (SIS) plant is designed to provide removal of undesirable isotopes in fuel grade plutonium by the atomic vapor laser isotope separation (AVLIS) process. The AVLIS process involves evaporation of plutonium metal, and passage of an intense beam of light from a laser through the plutonium vapor. The laser beam consists of several discrete wavelengths, tuned to the precise wavelength required to ionize the undesired isotopes. These ions are attracted to charged plates, leaving the bulk of the plutonium vapor enriched in the desired isotopes to be collected on a cold plate. Major portions of the process consist of pyrochemical processes, including direct reduction of the plutonium oxide feed material with calcium metal, and aqueous processes for purification of plutonium in residues. The analytical laboratory for the plant is called the Material and Process Control Laboratory (MPCL), and provides for the analysis of solid and liquid process samples

Application of X-ray fluorescence analytical techniques in phytoremediation and plant biology studies

International Nuclear Information System (INIS)

Necemer, Marijan; Kump, Peter; Scancar, Janez; Jacimovic, Radojko; Simcic, Jurij; Pelicon, Primoz; Budnar, Milos; Jeran, Zvonka; Pongrac, Paula; Regvar, Marjana; Vogel-Mikus, Katarina

2008-01-01

Phytoremediation is an emerging technology that employs the use of higher plants for the clean-up of contaminated environments. Progress in the field is however handicapped by limited knowledge of the biological processes involved in plant metal uptake, translocation, tolerance and plant-microbe-soil interactions; therefore a better understanding of the basic biological mechanisms involved in plant/microbe/soil/contaminant interactions would allow further optimization of phytoremediation technologies. In view of the needs of global environmental protection, it is important that in phytoremediation and plant biology studies the analytical procedures for elemental determination in plant tissues and soil should be fast and cheap, with simple sample preparation, and of adequate accuracy and reproducibility. The aim of this study was therefore to present the main characteristics, sample preparation protocols and applications of X-ray fluorescence-based analytical techniques (energy dispersive X-ray fluorescence spectrometry-EDXRF, total reflection X-ray fluorescence spectrometry-TXRF and micro-proton induced X-ray emission-micro-PIXE). Element concentrations in plant leaves from metal polluted and non-polluted sites, as well as standard reference materials, were analyzed by the mentioned techniques, and additionally by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). The results were compared and critically evaluated in order to assess the performance and capability of X-ray fluorescence-based techniques in phytoremediation and plant biology studies. It is the EDXRF, which is recommended as suitable to be used in the analyses of a large number of samples, because it is multi-elemental, requires only simple preparation of sample material, and it is analytically comparable to the most frequently used instrumental chemical techniques. The TXRF is compatible to FAAS in sample preparation, but relative to AAS it is fast, sensitive and

Development of the Diabetes Technology Society Blood Glucose Monitor System Surveillance Protocol.

Science.gov (United States)

Klonoff, David C; Lias, Courtney; Beck, Stayce; Parkes, Joan Lee; Kovatchev, Boris; Vigersky, Robert A; Arreaza-Rubin, Guillermo; Burk, Robert D; Kowalski, Aaron; Little, Randie; Nichols, James; Petersen, Matt; Rawlings, Kelly; Sacks, David B; Sampson, Eric; Scott, Steve; Seley, Jane Jeffrie; Slingerland, Robbert; Vesper, Hubert W

2016-05-01

Inaccurate blood glucsoe monitoring systems (BGMSs) can lead to adverse health effects. The Diabetes Technology Society (DTS) Surveillance Program for cleared BGMSs is intended to protect people with diabetes from inaccurate, unreliable BGMS products that are currently on the market in the United States. The Surveillance Program will provide an independent assessment of the analytical performance of cleared BGMSs. The DTS BGMS Surveillance Program Steering Committee included experts in glucose monitoring, surveillance testing, and regulatory science. Over one year, the committee engaged in meetings and teleconferences aiming to describe how to conduct BGMS surveillance studies in a scientifically sound manner that is in compliance with good clinical practice and all relevant regulations. A clinical surveillance protocol was created that contains performance targets and analytical accuracy-testing studies with marketed BGMS products conducted by qualified clinical and laboratory sites. This protocol entitled "Protocol for the Diabetes Technology Society Blood Glucose Monitor System Surveillance Program" is attached as supplementary material. This program is needed because currently once a BGMS product has been cleared for use by the FDA, no systematic postmarket Surveillance Program exists that can monitor analytical performance and detect potential problems. This protocol will allow identification of inaccurate and unreliable BGMSs currently available on the US market. The DTS Surveillance Program will provide BGMS manufacturers a benchmark to understand the postmarket analytical performance of their products. Furthermore, patients, health care professionals, payers, and regulatory agencies will be able to use the results of the study to make informed decisions to, respectively, select, prescribe, finance, and regulate BGMSs on the market. © 2015 Diabetes Technology Society.

Development of the Diabetes Technology Society Blood Glucose Monitor System Surveillance Protocol

Science.gov (United States)

Klonoff, David C.; Lias, Courtney; Beck, Stayce; Parkes, Joan Lee; Kovatchev, Boris; Vigersky, Robert A.; Arreaza-Rubin, Guillermo; Burk, Robert D.; Kowalski, Aaron; Little, Randie; Nichols, James; Petersen, Matt; Rawlings, Kelly; Sacks, David B.; Sampson, Eric; Scott, Steve; Seley, Jane Jeffrie; Slingerland, Robbert; Vesper, Hubert W.

2015-01-01

Background: Inaccurate blood glucsoe monitoring systems (BGMSs) can lead to adverse health effects. The Diabetes Technology Society (DTS) Surveillance Program for cleared BGMSs is intended to protect people with diabetes from inaccurate, unreliable BGMS products that are currently on the market in the United States. The Surveillance Program will provide an independent assessment of the analytical performance of cleared BGMSs. Methods: The DTS BGMS Surveillance Program Steering Committee included experts in glucose monitoring, surveillance testing, and regulatory science. Over one year, the committee engaged in meetings and teleconferences aiming to describe how to conduct BGMS surveillance studies in a scientifically sound manner that is in compliance with good clinical practice and all relevant regulations. Results: A clinical surveillance protocol was created that contains performance targets and analytical accuracy-testing studies with marketed BGMS products conducted by qualified clinical and laboratory sites. This protocol entitled “Protocol for the Diabetes Technology Society Blood Glucose Monitor System Surveillance Program” is attached as supplementary material. Conclusion: This program is needed because currently once a BGMS product has been cleared for use by the FDA, no systematic postmarket Surveillance Program exists that can monitor analytical performance and detect potential problems. This protocol will allow identification of inaccurate and unreliable BGMSs currently available on the US market. The DTS Surveillance Program will provide BGMS manufacturers a benchmark to understand the postmarket analytical performance of their products. Furthermore, patients, health care professionals, payers, and regulatory agencies will be able to use the results of the study to make informed decisions to, respectively, select, prescribe, finance, and regulate BGMSs on the market. PMID:26481642

Development of analytical methods for the separation of plutonium, americium, curium and neptunium from environmental samples

Energy Technology Data Exchange (ETDEWEB)

Salminen, S.

2009-07-01

In this work, separation methods have been developed for the analysis of anthropogenic transuranium elements plutonium, americium, curium and neptunium from environmental samples contaminated by global nuclear weapons testing and the Chernobyl accident. The analytical methods utilized in this study are based on extraction chromatography. Highly varying atmospheric plutonium isotope concentrations and activity ratios were found at both Kurchatov (Kazakhstan), near the former Semipalatinsk test site, and Sodankylae (Finland). The origin of plutonium is almost impossible to identify at Kurchatov, since hundreds of nuclear tests were performed at the Semipalatinsk test site. In Sodankylae, plutonium in the surface air originated from nuclear weapons testing, conducted mostly by USSR and USA before the sampling year 1963. The variation in americium, curium and neptunium concentrations was great as well in peat samples collected in southern and central Finland in 1986 immediately after the Chernobyl accident. The main source of transuranium contamination in peats was from global nuclear test fallout, although there are wide regional differences in the fraction of Chernobyl-originated activity (of the total activity) for americium, curium and neptunium. The separation methods developed in this study yielded good chemical recovery for the elements investigated and adequately pure fractions for radiometric activity determination. The extraction chromatographic methods were faster compared to older methods based on ion exchange chromatography. In addition, extraction chromatography is a more environmentally friendly separation method than ion exchange, because less acidic waste solutions are produced during the analytical procedures. (orig.)

IFSA: a microfluidic chip-platform for frit-based immunoassay protocols

Science.gov (United States)

Hlawatsch, Nadine; Bangert, Michael; Miethe, Peter; Becker, Holger; Gärtner, Claudia

2013-03-01

Point-of-care diagnostics (POC) is one of the key application fields for lab-on-a-chip devices. While in recent years much of the work has concentrated on integrating complex molecular diagnostic assays onto a microfluidic device, there is a need to also put comparatively simple immunoassay-type protocols on a microfluidic platform. In this paper, we present the development of a microfluidic cartridge using an immunofiltration approach. In this method, the sandwich immunoassay takes place in a porous frit on which the antibodies have immobilized. The device is designed to be able to handle three samples in parallel and up to four analytical targets per sample. In order to meet the critical cost targets for the diagnostic market, the microfluidic chip has been designed and manufactured using high-volume manufacturing technologies in mind. Validation experiments show comparable sensitivities in comparison with conventional immunofiltration kits.

Collection of biological samples in forensic toxicology.

Science.gov (United States)

Dinis-Oliveira, R J; Carvalho, F; Duarte, J A; Remião, F; Marques, A; Santos, A; Magalhães, T

2010-09-01

Forensic toxicology is the study and practice of the application of toxicology to the purposes of the law. The relevance of any finding is determined, in the first instance, by the nature and integrity of the specimen(s) submitted for analysis. This means that there are several specific challenges to select and collect specimens for ante-mortem and post-mortem toxicology investigation. Post-mortem specimens may be numerous and can endow some special difficulties compared to clinical specimens, namely those resulting from autolytic and putrefactive changes. Storage stability is also an important issue to be considered during the pre-analytic phase, since its consideration should facilitate the assessment of sample quality and the analytical result obtained from that sample. The knowledge on degradation mechanisms and methods to increase storage stability may enable the forensic toxicologist to circumvent possible difficulties. Therefore, advantages and limitations of specimen preservation procedures are thoroughfully discussed in this review. Presently, harmonized protocols for sampling in suspected intoxications would have obvious utility. In the present article an overview is given on sampling procedures for routinely collected specimens as well as on alternative specimens that may provide additional information on the route and timing of exposure to a specific xenobiotic. Last, but not least, a discussion on possible bias that can influence the interpretation of toxicological results is provided. This comprehensive review article is intented as a significant help for forensic toxicologists to accomplish their frequently overwhelming mission.

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

Science.gov (United States)

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

SPIDIA-RNA: First external quality assessment for the pre-analytical phase of blood samples used for RNA based analyses

Czech Academy of Sciences Publication Activity Database

Pazzagli, M.; Malentacchi, F.; Simi, L.; Wyrich, R.; Guenther, K.; Hartmann, C.; Verderio, P.; Pizzamiglio, S.; Ciniselli, C.M.; Tichopád, Aleš; Kubista, Mikael; Gelmini, S.

2013-01-01

Roč. 59, č. 1 (2013), s. 20-31 ISSN 1046-2023 Institutional research plan: CEZ:AV0Z50520701 Keywords : Pre-analytical phase * RNA quality * Blood samples Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 3.221, year: 2013

Ball assisted device for analytical surface sampling

Science.gov (United States)

ElNaggar, Mariam S; Van Berkel, Gary J; Covey, Thomas R

2015-11-03

A system for sampling a surface includes a sampling probe having a housing and a socket, and a rolling sampling sphere within the socket. The housing has a sampling fluid supply conduit and a sampling fluid exhaust conduit. The sampling fluid supply conduit supplies sampling fluid to the sampling sphere. The sampling fluid exhaust conduit has an inlet opening for receiving sampling fluid carried from the surface by the sampling sphere. A surface sampling probe and a method for sampling a surface are also disclosed.

A slotted access control protocol for metropolitan WDM ring networks

Science.gov (United States)

Baziana, P. A.; Pountourakis, I. E.

2009-03-01

In this study we focus on the serious scalability problems that many access protocols for WDM ring networks introduce due to the use of a dedicated wavelength per access node for either transmission or reception. We propose an efficient slotted MAC protocol suitable for WDM ring metropolitan area networks. The proposed network architecture employs a separate wavelength for control information exchange prior to the data packet transmission. Each access node is equipped with a pair of tunable transceivers for data communication and a pair of fixed tuned transceivers for control information exchange. Also, each access node includes a set of fixed delay lines for synchronization reasons; to keep the data packets, while the control information is processed. An efficient access algorithm is applied to avoid both the data wavelengths and the receiver collisions. In our protocol, each access node is capable of transmitting and receiving over any of the data wavelengths, facing the scalability issues. Two different slot reuse schemes are assumed: the source and the destination stripping schemes. For both schemes, performance measures evaluation is provided via an analytic model. The analytical results are validated by a discrete event simulation model that uses Poisson traffic sources. Simulation results show that the proposed protocol manages efficient bandwidth utilization, especially under high load. Also, comparative simulation results prove that our protocol achieves significant performance improvement as compared with other WDMA protocols which restrict transmission over a dedicated data wavelength. Finally, performance measures evaluation is explored for diverse numbers of buffer size, access nodes and data wavelengths.

Analytical methodologies for aluminium speciation in environmental and biological samples--a review.

Science.gov (United States)

Bi, S P; Yang, X D; Zhang, F P; Wang, X L; Zou, G W

2001-08-01

It is recognized that aluminium (Al) is a potential environmental hazard. Acidic deposition has been linked to increased Al concentrations in natural waters. Elevated levels of Al might have serious consequences for biological communities. Of particular interest is the speciation of Al in aquatic environments, because Al toxicity depends on its forms and concentrations. In this paper, advances in analytical methodologies for Al speciation in environmental and biological samples during the past five years are reviewed. Concerns about the specific problems of Al speciation and highlights of some important methods are elucidated in sections devoted to hybrid techniques (HPLC or FPLC coupled with ET-AAS, ICP-AES, or ICP-MS), flow-injection analysis (FIA), nuclear magnetic resonance (27Al NMR), electrochemical analysis, and computer simulation. More than 130 references are cited.

Sampling and analytical methodologies for instrumental neutron activation analysis of airborne particulate matter

International Nuclear Information System (INIS)

1992-01-01

The IAEA supports a number of projects having to do with the analysis of airborne particulate matter by nuclear techniques. Most of this work involves the use of activation analysis in its various forms, particularly instrumental neutron activation analysis (INAA). This technique has been widely used in many different countries for the analysis of airborne particulate matter, and there are already many publications in scientific journals, books and reports describing such work. The present document represents an attempt to summarize the most important features of INAA as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of INAA to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability, although they are presented here in a way that takes account of the particular requirements arising from the use of INAA as the analytical technique. The analytical part of the document, however, is presented in a form that is applicable only to INAA. (Subsequent publications in this series are expected to deal specifically with other nuclear related techniques such as energy dispersive X ray fluorescence (ED-XRF) and particle induced X ray emission (PIXE) analysis). Although the methods and procedures described here have been found through experience to yield acceptable results, they should not be considered mandatory. Any other procedure used should, however, be chosen to be capable of yielding results at least of equal quality to those described

Sampling and analytical methodologies for instrumental neutron activation analysis of airborne particulate matter

Energy Technology Data Exchange (ETDEWEB)

NONE

1992-12-01

The IAEA supports a number of projects having to do with the analysis of airborne particulate matter by nuclear techniques. Most of this work involves the use of activation analysis in its various forms, particularly instrumental neutron activation analysis (INAA). This technique has been widely used in many different countries for the analysis of airborne particulate matter, and there are already many publications in scientific journals, books and reports describing such work. The present document represents an attempt to summarize the most important features of INAA as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of INAA to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability, although they are presented here in a way that takes account of the particular requirements arising from the use of INAA as the analytical technique. The analytical part of the document, however, is presented in a form that is applicable only to INAA. (Subsequent publications in this series are expected to deal specifically with other nuclear related techniques such as energy dispersive X ray fluorescence (ED-XRF) and particle induced X ray emission (PIXE) analysis). Although the methods and procedures described here have been found through experience to yield acceptable results, they should not be considered mandatory. Any other procedure used should, however, be chosen to be capable of yielding results at least of equal quality to those described.

Impact of sample processing on the measurement of circulating microparticles: storage and centrifugation parameters.

Science.gov (United States)

Vila-Liante, Virtudes; Sánchez-López, Verónica; Martínez-Sales, Vicenta; Ramón-Nuñez, Luis A; Arellano-Orden, Elena; Cano-Ruiz, Alejandra; Rodríguez-Martorell, Francisco J; Gao, Lin; Otero-Candelera, Remedios

2016-11-01

Microparticles (MPs) have been shown to be markers of cellular activation and interactions. Pre-analytical conditions such as the centrifugation protocol and sample storage conditions represent an important source of variability in determining MPs values. The objectives of this study were to evaluate the influence of sample storage conditions and centrifugation speed and temperature on the determination of MPs in plasma. Citrate-anticoagulated blood samples obtained from 21 healthy subjects were centrifuged under four different protocols involving different speeds (2500 g or 1500 g) and temperatures (4 °C or 20 °C) to isolate platelet-poor plasma (PPP). The number of MPs in fresh and frozen-thawed PPP were analyzed by flow cytometry, and MPs-mediated procoagulant activity was determined by a thrombin generation test and phospholipid-dependent procoagulant tests. The number of MPs and their procoagulant activity were affected by freeze-thaw cycling and centrifugation speed but not by centrifugation temperature. Sample freezing increased MPs number (six-fold) and thrombin generation (four-fold), and decreased clotting time (two-fold). Low centrifugation speed caused an increase in MPs number and a parallel increase in MP-mediated procoagulant activity. Sample storage conditions and centrifugation speed are important processing conditions affecting MPs number and activity. Before any study, the protocol for MPs isolation should be optimized to ensure a reliable characterization of MPs, which could provide important information for diagnostic purposes and for understanding the pathogenesis of diseases.

Data validation summary report for the 100-BC-5 Operable Unit Round 9 Groundwater Sampling. Revision 0

International Nuclear Information System (INIS)

Kearney, A.T.

1996-03-01

The information provided in this validation summary report includes chemical analyses of samples from 100-BC-5 Operable Unit Round 9 Groundwater sampling data. Data from this sampling event and their related quality assurance (QA) samples were reviewed and validated in accordance with Westinghouse Hanford Company (WHC) guidelines at the requested level. Sample analyses included metals, general chemistry, and radiochemistry. Sixty metals samples were analyzed by Quanterra Environmental Services (QES) and Lockheed Analytical Services (LAS). The metals samples were validated using WHC protocols specified in Data Validation Procedures for Chemical Analyses. All qualifiers assigned to the metals data were based on this guidance. The Table 1.1 lists the metals sample delivery group (SDG) that were validated for this sampling event

Micro-Crater Laser Induced Breakdown Spectroscopy--an Analytical approach in metals samples

Energy Technology Data Exchange (ETDEWEB)

Piscitelli, Vincent [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela); Lawrence Berkeley National laboratory, Berkeley, US (United States); Gonzalez, Jhanis; Xianglei, Mao; Russo, Richard [Lawrence Berkeley National laboratory, Berkeley, US (United States); Fernandez, Alberto [UCV- Laboratorio de Espectroscopia Laser, Caracas (Venezuela)

2008-04-15

The laser ablation has been increasing its popularity like as technique of chemical analysis. This is due to its great potentiality in the analysis of solid samples. On the way to contributing to the development of the technique, we in this work studied the laser induced breakdown spectroscopy (LIBS) in conditions of micro ablation for future studies of coverings and micro crates analysis. Craters between 2 and 7 micrometers of diameter were made using an Nd-YAG nanosecond laser in their fundamental emission of 1064 nm. In order to create these craters we use an objective lens of long distance work and 0.45 of numerical aperture. The atomic emission versus the energy of the laser and its effect on the size of craters was study. We found that below 3 micrometers although there was evidence of material removal by the formation of a crater, it was no detectable atomic emission for our instruments. In order to try to understand this, curves of size of crater versus plasma temperature using the Boltzmann distribution graphs taking the Copper emission lines in the visible region were made. In addition calibration curves for Copper and aluminum were made in two different matrices; one of it was a Cu/Zn alloy and the other a Zinc Matrix. The atomic lines Cu I (521.78 nm) and Al I (396.15 nm) was used. From the Calibration curve the analytical limit of detection and other analytical parameters were obtained.

Analytical evaluation of BEA zeolite for the pre-concentration of polycyclic aromatic hydrocarbons and their subsequent chromatographic analysis in water samples.

Science.gov (United States)

Wilson, Walter B; Costa, Andréia A; Wang, Huiyong; Dias, José A; Dias, Sílvia C L; Campiglia, Andres D

2012-07-06

The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 μL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated. Copyright © 2012 Elsevier B.V. All rights reserved.

Technical Protocol. Transformation of biocides in liquid manures

Energy Technology Data Exchange (ETDEWEB)

Kreuzig, Robert; Schlag, Patrick; Teigeler, Jennifer; Hartmann, Constanze; Cvetkovi, Benjamin [Technische Univ. Braunschweig (Germany). Inst. fuer Oekologische Chemie und Abfallanalytik

2010-07-15

The Reference Manure Concept, already developed for laboratory tests on fate and behavior of veterinary medicinal products in liquid manures and manured soils, was successfully applied for biocides used for disinfection purposes and control of insects in animal houses. Since the representative and reproducible sampling of manures from high-volume tanks has been considered impossible, excrement samples of cattle and pigs individually kept at an experimental animal house were taken. These samples were thoroughly matrix characterized. Then, tap water was added to prepare reference manures of definite dry substance contents. Subsequently, the long-term transformation of the biocides imazalil and cyanamide applied as {sup 14}C-labeled radiotracers was investigated in these manure samples. On the basis of the transformation tests, test manures with 7-day aged biocide residues were prepared and applied in laboratory tests on transformation and sorption in manured soil. By means of this experimental approach, the impacts of aging processes during manure storage and of the manure matrix on the fate of biocides in soils can be assessed already under laboratory conditions. These laboratory tests have been directed as closely as possible to agricultural practice as well as to analytical practicability and quality assurance. Finally, the methodological aspects have been compiled in a Technical Protocol (Draft version). (orig.)

Sampling and sample processing in pesticide residue analysis.

Science.gov (United States)

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Pre-Analytical Considerations for Successful Next-Generation Sequencing (NGS: Challenges and Opportunities for Formalin-Fixed and Paraffin-Embedded Tumor Tissue (FFPE Samples

Directory of Open Access Journals (Sweden)

Gladys Arreaza

2016-09-01

Full Text Available In cancer drug discovery, it is important to investigate the genetic determinants of response or resistance to cancer therapy as well as factors that contribute to adverse events in the course of clinical trials. Despite the emergence of new technologies and the ability to measure more diverse analytes (e.g., circulating tumor cell (CTC, circulating tumor DNA (ctDNA, etc., tumor tissue is still the most common and reliable source for biomarker investigation. Because of its worldwide use and ability to preserve samples for many decades at ambient temperature, formalin-fixed, paraffin-embedded tumor tissue (FFPE is likely to be the preferred choice for tissue preservation in clinical practice for the foreseeable future. Multiple analyses are routinely performed on the same FFPE samples (such as Immunohistochemistry (IHC, in situ hybridization, RNAseq, DNAseq, TILseq, Methyl-Seq, etc.. Thus, specimen prioritization and optimization of the isolation of analytes is critical to ensure successful completion of each assay. FFPE is notorious for producing suboptimal DNA quality and low DNA yield. However, commercial vendors tend to request higher DNA sample mass than what is actually required for downstream assays, which restricts the breadth of biomarker work that can be performed. We evaluated multiple genomics service laboratories to assess the current state of NGS pre-analytical processing of FFPE. Significant differences in pre-analytical capabilities were observed. Key aspects are highlighted and recommendations are made to improve the current practice in translational research.

Sampling and analytical methodologies for energy dispersive X-ray fluorescence analysis of airborne particulate matter

International Nuclear Information System (INIS)

1993-01-01

The present document represents an attempt to summarize the most important features of the different forms of ED-XFR as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of ED-XRF to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability. Emphasis is also placed on the sources of errors affecting the sampling of airborne particulate matter. The analytical part of the document describes the different forms of ED-XRF and their potential applications. Spectrum evaluation, a key step in X-ray spectrometry, is covered in depth, including discussion on several calibration and peak fitting techniques and computer programs especially designed for this purpose. 148 refs, 25 figs, 13 tabs

Pre-analytical and analytical variation of drug determination in segmented hair using ultra-performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Nielsen, Marie Katrine Klose; Johansen, Sys Stybe; Linnet, Kristian

2014-01-01

Assessment of total uncertainty of analytical methods for the measurements of drugs in human hair has mainly been derived from the analytical variation. However, in hair analysis several other sources of uncertainty will contribute to the total uncertainty. Particularly, in segmental hair analysis pre-analytical variations associated with the sampling and segmentation may be significant factors in the assessment of the total uncertainty budget. The aim of this study was to develop and validate a method for the analysis of 31 common drugs in hair using ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with focus on the assessment of both the analytical and pre-analytical sampling variations. The validated method was specific, accurate (80-120%), and precise (CV≤20%) across a wide linear concentration range from 0.025-25 ng/mg for most compounds. The analytical variation was estimated to be less than 15% for almost all compounds. The method was successfully applied to 25 segmented hair specimens from deceased drug addicts showing a broad pattern of poly-drug use. The pre-analytical sampling variation was estimated from the genuine duplicate measurements of two bundles of hair collected from each subject after subtraction of the analytical component. For the most frequently detected analytes, the pre-analytical variation was estimated to be 26-69%. Thus, the pre-analytical variation was 3-7 folds larger than the analytical variation (7-13%) and hence the dominant component in the total variation (29-70%). The present study demonstrated the importance of including the pre-analytical variation in the assessment of the total uncertainty budget and in the setting of the 95%-uncertainty interval (±2CVT). Excluding the pre-analytical sampling variation could significantly affect the interpretation of results from segmental hair analysis. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Laser sampling

International Nuclear Information System (INIS)

Gorbatenko, A A; Revina, E I

2015-01-01

The review is devoted to the major advances in laser sampling. The advantages and drawbacks of the technique are considered. Specific features of combinations of laser sampling with various instrumental analytical methods, primarily inductively coupled plasma mass spectrometry, are discussed. Examples of practical implementation of hybrid methods involving laser sampling as well as corresponding analytical characteristics are presented. The bibliography includes 78 references

Pierre Gy's sampling theory and sampling practice heterogeneity, sampling correctness, and statistical process control

CERN Document Server

Pitard, Francis F

1993-01-01

Pierre Gy's Sampling Theory and Sampling Practice, Second Edition is a concise, step-by-step guide for process variability management and methods. Updated and expanded, this new edition provides a comprehensive study of heterogeneity, covering the basic principles of sampling theory and its various applications. It presents many practical examples to allow readers to select appropriate sampling protocols and assess the validity of sampling protocols from others. The variability of dynamic process streams using variography is discussed to help bridge sampling theory with statistical process control. Many descriptions of good sampling devices, as well as descriptions of poor ones, are featured to educate readers on what to look for when purchasing sampling systems. The book uses its accessible, tutorial style to focus on professional selection and use of methods. The book will be a valuable guide for mineral processing engineers; metallurgists; geologists; miners; chemists; environmental scientists; and practit...

Establishing a protocol for element determination in human nail clippings by neutron activation analysis

International Nuclear Information System (INIS)

Sanches, Thalita Pinheiro; Saiki, Mitiko

2011-01-01

Human nail samples have been analyzed to evaluate occupational exposure, nutritional status and to diagnose certain diseases. However, sampling and washing protocols for nail analyses vary from study to study not allowing comparisons between studies. One of the difficulties in analyzing nail samples is to eliminate only surface contamination without removing elements of interest in this tissue. In the present study, a protocol was defined in order to obtain reliable results of element concentrations in human nail clippings. Nail clippings collected from all 10 fingers or toes were previously pre cleaned using an ethyl alcohol solution to eliminate microbes. Then, the clippings were cut in small pieces and submitted to different reagents for washing by shaking. Neutron activation analysis (NAA) was applied for nail samples analysis which consisted of irradiating aliquots of samples together with synthetic elemental standards in the IEA-R1 nuclear research reactor followed by gamma ray spectrometry. Comparisons made between the results obtained for nails submitted to different reagents for cleaning indicated that the procedure using acetone and Triton X100 solution is more effective than that of nitric acid solution. Analyses in triplicates of a nail sample indicated results with relative standard deviations lower than 15% for most of elements, showing the homogeneity of the prepared sample. Qualitative analyses of different nail polishes showed that the presence of elements determined in the present study is negligible in these products. Quality control of the analytical results indicated that the applied NAA procedure is adequate for human nail analysis. (author)

Throughput and Fairness of Collision Avoidance Protocols in Ad Hoc Networks

National Research Council Canada - National Science Library

Garcia-Luna-Aceves, J. J; Wang, Yu

2004-01-01

.... In Section 1, The authors present an analytical modeling to derive the saturation throughput of these sender-initiated collision avoidance protocols in multi-hop ad hoc networks with nodes randomly...

Investigations of the post-IR IRSL protocol applied to single K-feldspar grains from fluvial sediment samples

International Nuclear Information System (INIS)

Nian, Xiaomei; Bailey, Richard M.; Zhou, Liping

2012-01-01

The post-IR IRSL protocol with single K-feldspar grains was applied to three samples taken from a fluvial sedimentary sequence at the archaeological site of the Dali Man, Shaanxi Province, China. K-feldspar coarse grains were extracted for measurement. Approximately 30–40% of the grains were sufficiently bright to measure, and after application of rejection criteria based on signal strength, recuperation, recycling ratio and saturation dose, ∼10–15% of the grains were used for D e calculation. The relationship of signal decay rate and form of D e (t) with the recovery dose were investigated. The dose recovery ratios of the samples after initial bleaching with the four different light sources were within uncertainties of unity. No anomalous fading was observed. The over-dispersion of the recovered dose and D e values were similar, suggesting neither incomplete resetting of the post-IR IRSL signals nor spatially heterogeneous dose rates significantly affected the natural dose estimates. The values of D e obtained with the single K-feldspar grain post-IR IRSL protocol were in the range ∼400–490 Gy. Combining all of the measured single-grain signals for each of the individual samples (into a ‘synthetic single aliquot’) increased the D e estimates to the range ∼700–900 Gy, suggesting that the grains screened-out by the rejection criteria may have the potential to cause palaeodose over-estimation, although this finding requires a more extensive investigation. Thermally transferred signals were found in the single K-feldspar grains post-IR IRSL protocol, and the proportion of thermally transferred signal to test-dose OSL signal (stimulation at 290 °C) from the natural dose was higher than from regenerative doses, and the proportion was grain- and dose-dependent. As such, TT-post-IR IRSL signals at 290 °C have the potential to cause dose underestimation, although this may be reduced by using larger test-dose irradiations. Our study demonstrates

Analytical chemistry

Energy Technology Data Exchange (ETDEWEB)

Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

1989-02-15

This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

Analytical chemistry

International Nuclear Information System (INIS)

Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

1989-02-01

This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

Design Protocols and Analytical Strategies that Incorporate Structural Reliability Models

Science.gov (United States)

Duffy, Stephen F.

1997-01-01

Ceramic matrix composites (CMC) and intermetallic materials (e.g., single crystal nickel aluminide) are high performance materials that exhibit attractive mechanical, thermal and chemical properties. These materials are critically important in advancing certain performance aspects of gas turbine engines. From an aerospace engineer's perspective the new generation of ceramic composites and intermetallics offers a significant potential for raising the thrust/weight ratio and reducing NO(x) emissions of gas turbine engines. These aspects have increased interest in utilizing these materials in the hot sections of turbine engines. However, as these materials evolve and their performance characteristics improve a persistent need exists for state-of-the-art analytical methods that predict the response of components fabricated from CMC and intermetallic material systems. This need provided the motivation for the technology developed under this research effort. Continuous ceramic fiber composites exhibit an increase in work of fracture, which allows for "graceful" rather than catastrophic failure. When loaded in the fiber direction, these composites retain substantial strength capacity beyond the initiation of transverse matrix cracking despite the fact that neither of its constituents would exhibit such behavior if tested alone. As additional load is applied beyond first matrix cracking, the matrix tends to break in a series of cracks bridged by the ceramic fibers. Any additional load is born increasingly by the fibers until the ultimate strength of the composite is reached. Thus modeling efforts supported under this research effort have focused on predicting this sort of behavior. For single crystal intermetallics the issues that motivated the technology development involved questions relating to material behavior and component design. Thus the research effort supported by this grant had to determine the statistical nature and source of fracture in a high strength, Ni

Studies on application of neutron activation analysis -Applied research on air pollution monitoring and development of analytical method of environmental samples

International Nuclear Information System (INIS)

Chung, Yong Sam; Moon, Jong Hwa; Chung, Young Ju; Jeong, Eui Sik; Lee, Sang Mi; Kang, Sang Hun; Cho, Seung Yeon; Kwon, Young Sik; Chung, Sang Wuk; Lee, Kyu Sung; Chun, Ki Hong; Kim, Nak Bae; Lee, Kil Yong; Yoon, Yoon Yeol; Chun, Sang Ki.

1997-09-01

This research report is written for results of applied research on air pollution monitoring using instrumental neutron activation analysis. For identification and standardization of analytical method, 24 environmental samples are analyzed quantitatively, and accuracy and precision of this method are measured. Using airborne particulate matter and biomonitor chosen as environmental indicators, trace elemental concentrations of sample collected at urban and rural site monthly are determined ant then the calculation of statistics and the factor analysis are carried out for investigation of emission source. Facilities for NAA are installed in a new HANARO reactor, functional test is performed for routine operation. In addition, unified software code for NAA is developed to improve accuracy, precision and abilities of analytical processes. (author). 103 refs., 61 tabs., 19 figs

Comparison of protocols and RNA carriers for plasma miRNA isolation. Unraveling RNA carrier influence on miRNA isolation

Science.gov (United States)

Martos, Laura; Fernández-Pardo, Álvaro; Oto, Julia; Medina, Pilar; España, Francisco; Navarro, Silvia

2017-01-01

microRNAs are promising biomarkers in biological fluids in several diseases. Different plasma RNA isolation protocols and carriers are available, but their efficiencies have been scarcely compared. Plasma microRNAs were isolated using a phenol and column-based procedure and a column-based procedure, in the presence or absence of two RNA carriers (yeast RNA and MS2 RNA). We evaluated the presence of PCR inhibitors and the relative abundance of certain microRNAs by qRT-PCR. Furthermore, we analyzed the association between different isolation protocols, the relative abundance of the miRNAs in the sample, the GC content and the free energy of microRNAs. In all microRNAs analyzed, the addition of yeast RNA as a carrier in the different isolation protocols used gave lower raw Cq values, indicating higher microRNA recovery. Moreover, this increase in microRNAs recovery was dependent on their own relative abundance in the sample, their GC content and the free-energy of their own most stable secondary structure. Furthermore, the normalization of microRNA levels by an endogenous microRNA is more reliable than the normalization by plasma volume, as it reduced the difference in microRNA fold abundance between the different isolation protocols evaluated. Our thorough study indicates that a standardization of pre- and analytical conditions is necessary to obtain reproducible inter-laboratory results in plasma microRNA studies. PMID:29077772

Network protocols and sockets

OpenAIRE

BALEJ, Marek

2010-01-01

My work will deal with network protocols and sockets and their use in programming language C#. It will therefore deal programming network applications on the platform .NET from Microsoft and instruments, which C# provides to us. There will describe the tools and methods for programming network applications, and shows a description and sample applications that work with sockets and application protocols.

Pre-Analytical Parameters Affecting Vascular Endothelial Growth Factor Measurement in Plasma: Identifying Confounders.

Science.gov (United States)

Walz, Johanna M; Boehringer, Daniel; Deissler, Heidrun L; Faerber, Lothar; Goepfert, Jens C; Heiduschka, Peter; Kleeberger, Susannah M; Klettner, Alexa; Krohne, Tim U; Schneiderhan-Marra, Nicole; Ziemssen, Focke; Stahl, Andreas

2016-01-01

Vascular endothelial growth factor-A (VEGF-A) is intensively investigated in various medical fields. However, comparing VEGF-A measurements is difficult because sample acquisition and pre-analytic procedures differ between studies. We therefore investigated which variables act as confounders of VEGF-A measurements. Following a standardized protocol, blood was taken at three clinical sites from six healthy participants (one male and one female participant at each center) twice one week apart. The following pre-analytical parameters were varied in order to analyze their impact on VEGF-A measurements: analyzing center, anticoagulant (EDTA vs. PECT / CTAD), cannula (butterfly vs. neonatal), type of centrifuge (swing-out vs. fixed-angle), time before and after centrifugation, filling level (completely filled vs. half-filled tubes) and analyzing method (ELISA vs. multiplex bead array). Additionally, intrapersonal variations over time and sex differences were explored. Statistical analysis was performed using a linear regression model. The following parameters were identified as statistically significant independent confounders of VEGF-A measurements: analyzing center, anticoagulant, centrifuge, analyzing method and sex of the proband. The following parameters were no significant confounders in our data set: intrapersonal variation over one week, cannula, time before and after centrifugation and filling level of collection tubes. VEGF-A measurement results can be affected significantly by the identified pre-analytical parameters. We recommend the use of CTAD anticoagulant, a standardized type of centrifuge and one central laboratory using the same analyzing method for all samples.

Pre-Analytical Parameters Affecting Vascular Endothelial Growth Factor Measurement in Plasma: Identifying Confounders.

Directory of Open Access Journals (Sweden)

Johanna M Walz

Full Text Available Vascular endothelial growth factor-A (VEGF-A is intensively investigated in various medical fields. However, comparing VEGF-A measurements is difficult because sample acquisition and pre-analytic procedures differ between studies. We therefore investigated which variables act as confounders of VEGF-A measurements.Following a standardized protocol, blood was taken at three clinical sites from six healthy participants (one male and one female participant at each center twice one week apart. The following pre-analytical parameters were varied in order to analyze their impact on VEGF-A measurements: analyzing center, anticoagulant (EDTA vs. PECT / CTAD, cannula (butterfly vs. neonatal, type of centrifuge (swing-out vs. fixed-angle, time before and after centrifugation, filling level (completely filled vs. half-filled tubes and analyzing method (ELISA vs. multiplex bead array. Additionally, intrapersonal variations over time and sex differences were explored. Statistical analysis was performed using a linear regression model.The following parameters were identified as statistically significant independent confounders of VEGF-A measurements: analyzing center, anticoagulant, centrifuge, analyzing method and sex of the proband. The following parameters were no significant confounders in our data set: intrapersonal variation over one week, cannula, time before and after centrifugation and filling level of collection tubes.VEGF-A measurement results can be affected significantly by the identified pre-analytical parameters. We recommend the use of CTAD anticoagulant, a standardized type of centrifuge and one central laboratory using the same analyzing method for all samples.

Is a pre-analytical process for urinalysis required?

Science.gov (United States)

Petit, Morgane; Beaudeux, Jean-Louis; Majoux, Sandrine; Hennequin, Carole

2017-10-01

For the reliable urinary measurement of calcium, phosphate and uric acid, a pre-analytical process by adding acid or base to urine samples at laboratory is recommended in order to dissolve precipitated solutes. Several studies on different kind of samples and analysers have previously shown that a such pre-analytical treatment is useless. The objective was to study the necessity of pre-analytical treatment of urine on samples collected using the V-Monovette ® (Sarstedt) system and measured on the analyser Architect C16000 (Abbott Diagnostics). Sixty urinary samples of hospitalized patients were selected (n=30 for calcium and phosphate, and n=30 for uric acid). After acidification of urine samples for measurement of calcium and phosphate, and alkalinisation for measurement of uric acid respectively, differences between results before and after the pre-analytical treatment were compared to acceptable limits recommended by the French society of clinical biology (SFBC). No difference in concentration between before and after pre-analytical treatment of urine samples exceeded acceptable limits from SFBC for measurement of calcium and uric acid. For phosphate, only one sample exceeded these acceptable limits, showing a result paradoxically lower after acidification. In conclusion, in agreement with previous study, our results show that acidification or alkalinisation of urine samples from 24 h urines or from urination is not a pre-analytical necessity for measurement of calcium, phosphate and uric acid.

Optimization and validation of the protocol used to analyze the taste of traditional Chinese medicines using an electronic tongue.

Science.gov (United States)

Li, Xuelin; Gao, Xiaojie; Liu, Ruixin; Wang, Junming; Wu, Zidan; Zhang, Lu; Li, Huiling; Gui, Xinjing; Kang, Bingya; Shi, Junhan

2016-11-01

Tools to define the active ingredients and flavors of Traditional Chinese Medicines (TCMs) are limited by long analysis times, complex sample preparation and a lack of multiplexed analysis. The aim of the present study was to optimize and validate an electronic tongue (E-tongue) methodology to analyze the bitterness of TCMs. To test the protocol, 35 different TCM concoctions were measured using an E-tongue, and seven replicate measurements of each sample were taken to evaluate reproducibility and precision. E-tongue sensor information was identified and classified using analysis approaches including least squares support vector machine (LS-SVM), support vector machine (SVM), discriminant analysis (DA) and partial least squares (PLS). A benefit of this analytical protocol was that the analysis of a single sample took <15 min for all seven sensors. The results identified that the LS-SVM approach provided the best bitterness classification accuracy (binary classification accuracy, 100%; ternary classification accuracy, 89.66%). The E-tongue protocol developed showed good reproducibility and high precision within a 6 h measurement cycle. To the best of our knowledge, this is the first study of an E-tongue being applied to assay the bitterness of TCMs. This approach could be applied in the classification of the taste of TCMs, and serve important roles in other fields, including foods and beverages.

A clean laboratory for ultratrace analysis: the ultratrace analytical facility (UTAF)

International Nuclear Information System (INIS)

Jadhav, S.G.; Sounderajan, Suvarna; Kumar, Sanjukta A.; Udas, A.C.; Ramanathan, M.; Palrecha, M.M.; Sudersanan, M.

2003-06-01

Thare has been an increasing demand for the quantification of various elements at extremely low concentrations in a variety of samples such as high purity materials, environmental and biological samples. The need for a controlled environment to obtain reliable and reproducible data necessitates the use of strategies and practices to minimize contamination during the analytical procedure. This report describes the protocol observed in our clean laboratory to eliminate contamination and ensure low laboratory blanks and some of the methodologies developed to carry out the analysis. The analysis is carried out by Graphite Furnace Atomic Absorption Spectrometry and electrochemical techniques such as Anodic/ Cathodic / Adsorptive Stripping Voltammetry. Characterisation of 5N (total impurities 10 ppm) arsenic is routinely carried out. Al in serum of patients suffering from end stage renal failure are also analyzed. Pine leaves, spinach, carrot puree and milk powder have been characterized for Al and Hg content and bovine serum has been characterized for Cu, Zn, Na, K in samples as part of intercomparison exercises. (author)

Reducing the cost of semi-automated in-gel tryptic digestion and GeLC sample preparation for high-throughput proteomics.

Science.gov (United States)

Ruelcke, Jayde E; Loo, Dorothy; Hill, Michelle M

2016-10-21

Peptide generation by trypsin digestion is typically the first step in mass spectrometry-based proteomics experiments, including 'bottom-up' discovery and targeted proteomics using multiple reaction monitoring. Manual tryptic digest and the subsequent clean-up steps can add variability even before the sample reaches the analytical platform. While specialized filter plates and tips have been designed for automated sample processing, the specialty reagents required may not be accessible or feasible due to their high cost. Here, we report a lower-cost semi-automated protocol for in-gel digestion and GeLC using standard 96-well microplates. Further cost savings were realized by re-using reagent tips with optimized sample ordering. To evaluate the methodology, we compared a simple mixture of 7 proteins and a complex cell-lysate sample. The results across three replicates showed that our semi-automated protocol had performance equal to or better than a manual in-gel digestion with respect to replicate variability and level of contamination. In this paper, we also provide the Agilent Bravo method file, which can be adapted to other liquid handlers. The simplicity, reproducibility, and cost-effectiveness of our semi-automated protocol make it ideal for routine in-gel and GeLC sample preparations, as well as high throughput processing of large clinical sample cohorts. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample Preparation Strategies for the Effective Quantitation of Hydrophilic Metabolites in Serum by Multi-Targeted HILIC-MS/MS

Directory of Open Access Journals (Sweden)

Elisavet Tsakelidou

2017-03-01

Full Text Available The effect of endogenous interferences of serum in multi-targeted metabolite profiling HILIC-MS/MS analysis was investigated by studying different sample preparation procedures. A modified QuEChERS dispersive SPE protocol, a HybridSPE protocol, and a combination of liquid extraction with protein precipitation were compared to a simple protein precipitation. Evaluation of extraction efficiency and sample clean-up was performed for all methods. SPE sorbent materials tested were found to retain hydrophilic analytes together with endogenous interferences, thus additional elution steps were needed. Liquid extraction was not shown to minimise matrix effects. In general, it was observed that a balance should be reached in terms of recovery, efficient clean-up, and sample treatment time when a wide range of metabolites are analysed. A quick step for removing phospholipids prior to the determination of hydrophilic endogenous metabolites is required, however, based on the results from the applied methods, further studies are needed to achieve high recoveries for all metabolites.

A Business Evaluation Of The Next Generation Ipv6 Protocol In Fixed And Mobile Communication Services

NARCIS (Netherlands)

L-F. Pau (Louis-François)

2002-01-01

textabstractThis paper gives an analytical business model of the Internet IPv4 and IPv6 protocols ,focussing on the business implications of intrinsic technical properties of these protocols .The technical properties modeled in business terms are : address space, payload, autoconfiguration, IP

[Protocol for the study of bone tumours and standardization of pathology reports].

Science.gov (United States)

Machado, Isidro; Pozo, José Juan; Marcilla, David; Cruz, Julia; Tardío, Juan C; Astudillo, Aurora; Bagué, Sílvia

Primary bone neoplasms represent a rare and heterogeneous group of mesenchymal tumours. The prevalence of benign and malignant tumours varies; the latter (sarcomas) account for less than 0.2% of all malignant tumours. Primary bone neoplasms are usually diagnosed and classified according to the criteria established and published by the World Health Organization (WHO 2013). These criteria are a result of advances in molecular pathology, which complements the histopathological diagnosis. Bone tumours should be diagnosed and treated in referral centers by a multidisciplinary team including pathologists, radiologists, orthopedic surgeons and oncologists. We analyzed different national and international protocols in order to provide a guide of recommendations for the improvement of pathological evaluation and management of bone tumours. We include specific recommendations for the pre-analytical, analytical, and post-analytical phases, as well as protocols for gross and microscopic pathology. Copyright © 2016 Sociedad Española de Anatomía Patológica. Publicado por Elsevier España, S.L.U. All rights reserved.

Use of CTX-I and PINP as bone turnover markers: National Bone Health Alliance recommendations to standardize sample handling and patient preparation to reduce pre-analytical variability.

Science.gov (United States)

Szulc, P; Naylor, K; Hoyle, N R; Eastell, R; Leary, E T

2017-09-01

The National Bone Health Alliance (NBHA) recommends standardized sample handling and patient preparation for C-terminal telopeptide of type I collagen (CTX-I) and N-terminal propeptide of type I procollagen (PINP) measurements to reduce pre-analytical variability. Controllable and uncontrollable patient-related factors are reviewed to facilitate interpretation and minimize pre-analytical variability. The IOF and the International Federation of Clinical Chemistry (IFCC) Bone Marker Standards Working Group have identified PINP and CTX-I in blood to be the reference markers of bone turnover for the fracture risk prediction and monitoring of osteoporosis treatment. Although used in clinical research for many years, bone turnover markers (BTM) have not been widely adopted in clinical practice primarily due to their poor within-subject and between-lab reproducibility. The NBHA Bone Turnover Marker Project team aim to reduce pre-analytical variability of CTX-I and PINP measurements through standardized sample handling and patient preparation. Recommendations for sample handling and patient preparations were made based on review of available publications and pragmatic considerations to reduce pre-analytical variability. Controllable and un-controllable patient-related factors were reviewed to facilitate interpretation and sample collection. Samples for CTX-I must be collected consistently in the morning hours in the fasted state. EDTA plasma is preferred for CTX-I for its greater sample stability. Sample collection conditions for PINP are less critical as PINP has minimal circadian variability and is not affected by food intake. Sample stability limits should be observed. The uncontrollable aspects (age, sex, pregnancy, immobility, recent fracture, co-morbidities, anti-osteoporotic drugs, other medications) should be considered in BTM interpretation. Adopting standardized sample handling and patient preparation procedures will significantly reduce controllable pre-analytical

Evaluation protocol for amusia: Portuguese sample.

Science.gov (United States)

Peixoto, Maria Conceição; Martins, Jorge; Teixeira, Pedro; Alves, Marisa; Bastos, José; Ribeiro, Carlos

2012-12-01

Amusia is a disorder that affects the processing of music. Part of this processing happens in the primary auditory cortex. The study of this condition allows us to evaluate the central auditory pathways. To explore the diagnostic evaluation tests of amusia. The authors propose an evaluation protocol for patients with suspected amusia (after brain injury or complaints of poor musical perception), in parallel with the assessment of central auditory processing, already implemented in the department. The Montreal Evaluation of Battery of amusia was the basis for the selection of the tests. From this comprehensive battery of tests we selected some of the musical examples to evaluate different musical aspects, including memory and perception of music, ability concerning musical recognition and discrimination. In terms of memory there is a test for assessing delayed memory, adapted to the Portuguese culture. Prospective study. Although still experimental, with the possibility of adjustments in the assessment, we believe that this assessment, combined with the study of central auditory processing, will allow us to understand some central lesions, congenital or acquired hearing perception limitations.

A two-hypothesis approach to establishing a life detection/biohazard protocol for planetary samples

Science.gov (United States)

Conley, Catharine; Steele, Andrew

2016-07-01

The COSPAR policy on performing a biohazard assessment on samples brought from Mars to Earth is framed in the context of a concern for false-positive results. However, as noted during the 2012 Workshop for Life Detection in Samples from Mars (ref. Kminek et al., 2014), a more significant concern for planetary samples brought to Earth is false-negative results, because an undetected biohazard could increase risk to the Earth. This is the reason that stringent contamination control must be a high priority for all Category V Restricted Earth Return missions. A useful conceptual framework for addressing these concerns involves two complementary 'null' hypotheses: testing both of them, together, would allow statistical and community confidence to be developed regarding one or the other conclusion. As noted above, false negatives are of primary concern for safety of the Earth, so the 'Earth Safety null hypothesis' -- that must be disproved to assure low risk to the Earth from samples introduced by Category V Restricted Earth Return missions -- is 'There is native life in these samples.' False positives are of primary concern for Astrobiology, so the 'Astrobiology null hypothesis' -- that must be disproved in order to demonstrate the existence of extraterrestrial life is 'There is no life in these samples.' The presence of Earth contamination would render both of these hypotheses more difficult to disprove. Both these hypotheses can be tested following a strict science protocol; analyse, interprete, test the hypotheses and repeat. The science measurements undertaken are then done in an iterative fashion that responds to discovery with both hypotheses testable from interpretation of the scientific data. This is a robust, community involved activity that ensures maximum science return with minimal sample use.

Multi-site study of additive genetic effects on fractional anisotropy of cerebral white matter: comparing meta and mega analytical approaches for data pooling

Science.gov (United States)

Kochunov, Peter; Jahanshad, Neda; Sprooten, Emma; Nichols, Thomas E.; Mandl, René C.; Almasy, Laura; Booth, Tom; Brouwer, Rachel M.; Curran, Joanne E.; de Zubicaray, Greig I.; Dimitrova, Rali; Duggirala, Ravi; Fox, Peter T.; Hong, L. Elliot; Landman, Bennett A.; Lemaitre, Hervé; Lopez, Lorna; Martin, Nicholas G.; McMahon, Katie L.; Mitchell, Braxton D.; Olvera, Rene L.; Peterson, Charles P.; Starr, John M.; Sussmann, Jessika E.; Toga, Arthur W.; Wardlaw, Joanna M.; Wright, Margaret J.; Wright, Susan N.; Bastin, Mark E.; McIntosh, Andrew M.; Boomsma, Dorret I.; Kahn, René S.; den Braber, Anouk; de Geus, Eco JC; Deary, Ian J.; Hulshoff Pol, Hilleke E.; Williamson, Douglas E.; Blangero, John; van ’t Ent, Dennis; Thompson, Paul M.; Glahn, David C.

2014-01-01

Combining datasets across independent studies can boost statistical power by increasing the numbers of observations and can achieve more accurate estimates of effect sizes. This is especially important for genetic studies where a large number of observations are required to obtain sufficient power to detect and replicate genetic effects. There is a need to develop and evaluate methods for joint-analytical analyses of rich datasets collected in imaging genetics studies. The ENIGMA-DTI consortium is developing and evaluating approaches for obtaining pooled estimates of heritability through meta-and mega-genetic analytical approaches, to estimate the general additive genetic contributions to the intersubject variance in fractional anisotropy (FA) measured from diffusion tensor imaging (DTI). We used the ENIGMA-DTI data harmonization protocol for uniform processing of DTI data from multiple sites. We evaluated this protocol in five family-based cohorts providing data from a total of 2248 children and adults (ages: 9–85) collected with various imaging protocols. We used the imaging genetics analysis tool, SOLAR-Eclipse, to combine twin and family data from Dutch, Australian and Mexican-American cohorts into one large “mega-family”. We showed that heritability estimates may vary from one cohort to another. We used two meta-analytical (the sample-size and standard-error weighted) approaches and a mega-genetic analysis to calculate heritability estimates across-population. We performed leave-one-out analysis of the joint estimates of heritability, removing a different cohort each time to understand the estimate variability. Overall, meta- and mega-genetic analyses of heritability produced robust estimates of heritability. PMID:24657781

Quality assurance procedures for the analysis of TRU waste samples

International Nuclear Information System (INIS)

Glasgow, D.C. Giaquinto, J.M.; Robinson, L.

1995-01-01

The Waste Isolation Pilot Plant (WIPP) project was undertaken in response to the growing need for a national repository for transuranic (TRU) waste. Guidelines for WIPP specify that any waste item to be interred must be fully characterized and analyzed to determine the presence of chemical compounds designated hazardous and certain toxic elements. The Transuranic Waste Characterization Program (TWCP) was launched to develop analysis and quality guidelines, certify laboratories, and to oversee the actual waste characterizations at the laboratories. ORNL is participating in the waste characterization phase and brings to bear a variety of analytical techniques including ICP-AES, cold vapor atomic absorption, and instrumental neutron activation analysis (INAA) to collective determine arsenic, cadmium, barium, chromium, mercury, selenium, silver, and other elements. All of the analytical techniques involved participate in a cooperative effort to meet the project objectives. One important component of any good quality assurance program is determining when an alternate method is more suitable for a given analytical problem. By bringing to bear a whole arsenal of analytical techniques working toward common objectives, few analytical problems prove to be insurmountable. INAA and ICP-AES form a powerful pair when functioning in this cooperative manner. This paper will provide details of the quality assurance protocols, typical results from quality control samples for both INAA and ICP-AES, and detail method cooperation schemes used

Matrix effects break the LC behavior rule for analytes in LC-MS/MS analysis of biological samples.

Science.gov (United States)

Fang, Nianbai; Yu, Shanggong; Ronis, Martin Jj; Badger, Thomas M

2015-04-01

High-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) are generally accepted as the preferred techniques for detecting and quantitating analytes of interest in biological matrices on the basis of the rule that one chemical compound yields one LC-peak with reliable retention time (Rt.). However, in the current study, we have found that under the same LC-MS conditions, the Rt. and shape of LC-peaks of bile acids in urine samples from animals fed dissimilar diets differed significantly among each other. To verify this matrix effect, 17 authentic bile acid standards were dissolved in pure methanol or in methanol containing extracts of urine from pigs consuming either breast milk or infant formula and analyzed by LC-MS/MS. The matrix components in urine from piglets fed formula significantly reduced the LC-peak Rt. and areas of bile acids. This is the first characterization of this matrix effect on Rt. in the literature. Moreover, the matrix effect resulted in an unexpected LC behavior: one single compound yielded two LC-peaks, which broke the rule of one LC-peak for one compound. The three bile acid standards which exhibited this unconventional LC behavior were chenodeoxycholic acid, deoxycholic acid, and glycocholic acid. One possible explanation for this effect is that some matrix components may have loosely bonded to analytes, which changed the time analytes were retained on a chromatography column and interfered with the ionization of analytes in the MS ion source to alter the peak area. This study indicates that a comprehensive understanding of matrix effects is needed towards improving the use of HPLC and LC-MS/MS techniques for qualitative and quantitative analyses of analytes in pharmacokinetics, proteomics/metabolomics, drug development, and sports drug testing, especially when LC-MS/MS data are analyzed by automation software where identification of an analyte is based on its exact molecular weight and Rt

Analysis of water and soil from the wetlands of Upper Three Runs Creek. Volume 2A, Analytical data packages September--October 1991 sampling

Energy Technology Data Exchange (ETDEWEB)

Haselow, L.A.; Rogers, V.A. [Westinghouse Savannah River Co., Aiken, SC (United States); Riordan, C.J. [Metcalf and Eddy, Inc. (United States); Eidson, G.W.; Herring, M.K. [Normandeau Associates, Inc. (United States)

1992-08-01

Shallow water and soils along Upper Three Runs Creek (UTRC) and associated wetlands between SRS Road F and Cato Road were sampled for nonradioactive and radioactive constituents. The sampling program is associated with risk evaluations being performed for various regulatory documents in these areas of the Savannah River Site (SRS). WSRC selected fifty sampling sites bordering the Mixed Waste Management Facility (MWMF), F- and H-Area Seepage Basins (FHSB), and the Sanitary Landfill (SL). The analytical results from this study provided information on the water and soil quality in UTRC and its associated wetlands. The analytical results from this investigation indicated that the primary constituents and radiological indicators detected in the shallow water and soils were tritium, gross alpha, radium 226, total radium and strontium 90. This investigation involved the collection of shallow water samples during the Fall of 1991 and the Spring of 1992 at fifty (50) sampling locations. Sampling was performed during these periods to incorporate high and low water table periods. Samples were collected from three sections along UTRC denoted as Phase I (MWMF), Phase II (FHSB) and Phase III (SL). One vibracored soil sample was also collected in each phase during the Fall of 1991. This document is compiled solely of experimental data obtained from the sampling procedures.

Analysis of water and soil from the wetlands of Upper Three Runs Creek. Volume 2B: Analytical data packages, January--February 1992 sampling

Energy Technology Data Exchange (ETDEWEB)

Haselow, L.A.; Rogers, V.A. [Westinghouse Savannah River Co., Aiken, SC (United States); Riordan, C.J. [Metcalf and Eddy (United States); Eidson, G.W.; Herring, M.K. [Normandeau Associates, Inc., Aiken, SC (United States)

1992-08-01

Shallow water and soils along Upper Three Runs Creek (UTRC) and associated wetlands between SRS Road F and Cato Road were sampled for nonradioactive and radioactive constituents. The sampling program is associated with risk evaluations being performed for various regulatory documents in these areas of the Savannah River Site (SRS). WSRC selected fifty sampling sites bordering the Mixed Waste Management Facility (MWMF), F- and H-Area Seepage Basins (FHSB), and the Sanitary Landfill (SL). The analytical results from this study provided information on the water and soil quality in UTRC and its associated wetlands. The analytical results from this investigation indicated that the primary constituents and radiological indicators detected in the shallow water and soils were tritium, gross alpha, radium 226, total radium and strontium 90. This investigation involved the collection of shallow water samples during the Fall of 1991 and the Spring of 1992 at fifty (50) sampling locations. Sampling was performed during these periods to incorporate high and low water table periods. Samples were collected from three sections along UTRC denoted as Phase I (MWMF), Phase II (FHSB) and Phase III (SL). One vibracored soil sample was also collected in each phase during the Fall of 1991. This document is compiled of experimental data obtained from the sampling procedures.

Analytical Validation of a New Enzymatic and Automatable Method for d-Xylose Measurement in Human Urine Samples

Directory of Open Access Journals (Sweden)

Israel Sánchez-Moreno

2017-01-01

Full Text Available Hypolactasia, or intestinal lactase deficiency, affects more than half of the world population. Currently, xylose quantification in urine after gaxilose oral administration for the noninvasive diagnosis of hypolactasia is performed with the hand-operated nonautomatable phloroglucinol reaction. This work demonstrates that a new enzymatic xylose quantification method, based on the activity of xylose dehydrogenase from Caulobacter crescentus, represents an excellent alternative to the manual phloroglucinol reaction. The new method is automatable and facilitates the use of the gaxilose test for hypolactasia diagnosis in the clinical practice. The analytical validation of the new technique was performed in three different autoanalyzers, using buffer or urine samples spiked with different xylose concentrations. For the comparison between the phloroglucinol and the enzymatic assays, 224 urine samples of patients to whom the gaxilose test had been prescribed were assayed by both methods. A mean bias of −16.08 mg of xylose was observed when comparing the results obtained by both techniques. After adjusting the cut-off of the enzymatic method to 19.18 mg of xylose, the Kappa coefficient was found to be 0.9531, indicating an excellent level of agreement between both analytical procedures. This new assay represents the first automatable enzymatic technique validated for xylose quantification in urine.

Integrated sampling and analysis plan for samples measuring >10 mrem/hour

International Nuclear Information System (INIS)

Haller, C.S.

1992-03-01

This integrated sampling and analysis plan was prepared to assist in planning and scheduling of Hanford Site sampling and analytical activities for all waste characterization samples that measure greater than 10 mrem/hour. This report also satisfies the requirements of the renegotiated Interim Milestone M-10-05 of the Hanford Federal Facility Agreement and Consent Order (the Tri-Party Agreement). For purposes of comparing the various analytical needs with the Hanford Site laboratory capabilities, the analytical requirements of the various programs were normalized by converting required laboratory effort for each type of sample to a common unit of work, the standard analytical equivalency unit (AEU). The AEU approximates the amount of laboratory resources required to perform an extensive suite of analyses on five core segments individually plus one additional suite of analyses on a composite sample derived from a mixture of the five core segments and prepare a validated RCRA-type data package

Double-contained receiver tank 244-TX, grab samples, 244TX-97-1 through 244TX-97-3 analytical results for the final report

International Nuclear Information System (INIS)

Esch, R.A.

1997-01-01

This document is the final report for the double-contained receiver tank (DCRT) 244-TX grab samples. Three grabs samples were collected from riser 8 on May 29, 1997. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DQO). The analytical results are presented in a table

XPS Protocol for the Characterization of Pristine and Functionalized Single Wall Carbon Nanotubes

Science.gov (United States)

Sosa, E. D.; Allada, R.; Huffman, C. B.; Arepalli, S.

2009-01-01

Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

Analytical method for heavy metal determination in algae and turtle eggs from Guanahacabibes Protected Sea Park

Directory of Open Access Journals (Sweden)

Abel I. Balbín Tamayo

2014-12-01

Full Text Available A standard digestion method coupled to electrochemical detection for the monitoring of heavy metals in biological samples has been used for the simultaneous analysis of the target analytes. Square wave anodic stripping voltammetry (SWASV coupled to disposable screen-printed electrodes (SPEs was employed as a fast and sensitive electroanalytical method for the detection of heavy metals. The aim of our study was to determine Cd, Pb and Cu by SWASV in brown algae (Sargasum natan and green turtle eggs (Chelonia mydas using screen-printed electrodes. The method proved useful for the simultaneous analysis of these metals by comparison between two different procedures for preparing the samples. Two different approaches in digestion protocols were assessed. The study was focused on Guanahacabibes brown algae and green turtle eggs because the metal concentrations recorded in this area may be used for intraspecific comparison within the Guanahacabibes Protected Sea Park area, a body of water for which information is still very scarce. The best results were obtained by digesting biological samples with the EPA 3050B method. This treatment allowed the fast and quantitative extraction from brown algae and green turtle eggs of the target analytes, with high sensitivity and avoiding organic residues, eventually affecting electrochemical measurements.

Aflatoxin B1-lysine adduct in dried blood spot samples of animals and humans.

Science.gov (United States)

Xue, Kathy S; Cai, Wenjie; Tang, Lili; Wang, Jia-Sheng

2016-12-01

Dried blood spots (DBS) were proposed as potentially viable method for exposure assessment of environmental toxicants in infant and young children. For this study, we validated an experimental protocol to quantify AFB 1 -lysine adduct in DBS samples of AFB 1 -treated F344 rats, as well as samples from human field study. Significant dose-response relationships in AFB 1 -lysine adduct formation were found in DBS samples of rats treated with single- and repeated-dose AFB 1 . AFB 1 -lysine levels in DBS samples were highly correlated with corresponding serum sample levels. The Person coefficients were 0.997 for the single-dose exposure, and 0.996 for the repeated-dose exposure. Levels of AFB 1 -lysine adduct had also good agreement between DBS and serum samples as shown by Bland-Altman plot analysis. For human field study samples (n = 36), a Pearson correlation coefficient of 0.784 was found between AFB 1 -lysine adduct levels of DBS and corresponding serum samples. Bland-Altman plots showed the distribution of the log differences between DBS and serum AFB 1 -lysine levels are within 95% confidence intervals. These results showed AFB 1 -lysine adduct levels in DBS cards and serum samples from animals and human samples are comparable, and the DBS technique and analytical protocol is a good means to assess AFB 1 exposure in infant and children populations. Copyright © 2016 Elsevier Ltd. All rights reserved.

Recent analytical applications of magnetic nanoparticles

Directory of Open Access Journals (Sweden)

Mohammad Faraji

2016-07-01

Full Text Available Analytical chemistry has experienced, as well as other areas of science, a big change due to the needs and opportunities provided by analytical nanoscience and nanotechnology. Now, nanotechnology is increasingly proving to be a powerful ally of analytical chemistry to achieve its objectives, and to simplify analytical processes. Moreover, the information needs arising from the growing nanotechnological activity are opening an exciting new field of action for analytical chemists. Magnetic nanoparticles have been used in various fields owing to their unique properties including large specific surface area and simple separation with magnetic fields. For Analytical applications, they have been used mainly for sample preparation techniques (magnetic solid phase extraction with different advanced functional groups (layered double hydroxide, β-cyclodextrin, carbon nanotube, graphen, polymer, octadecylsilane and automation of it, microextraction techniques enantioseparation and chemosensors. This review summarizes the basic principles and achievements of magnetic nanoparticles in sample preparation techniques, enantioseparation and chemosensors. Also, some selected articles recently published (2010-2016 have been reviewed and discussed.

Analytical challenges in sports drug testing.

Science.gov (United States)

Thevis, Mario; Krug, Oliver; Geyer, Hans; Walpurgis, Katja; Baume, Norbert; Thomas, Andreas

2018-03-01

Analytical chemistry represents a central aspect of doping controls. Routine sports drug testing approaches are primarily designed to address the question whether a prohibited substance is present in a doping control sample and whether prohibited methods (for example, blood transfusion or sample manipulation) have been conducted by an athlete. As some athletes have availed themselves of the substantial breadth of research and development in the pharmaceutical arena, proactive and preventive measures are required such as the early implementation of new drug candidates and corresponding metabolites into routine doping control assays, even though these drug candidates are to date not approved for human use. Beyond this, analytical data are also cornerstones of investigations into atypical or adverse analytical findings, where the overall picture provides ample reason for follow-up studies. Such studies have been of most diverse nature, and tailored approaches have been required to probe hypotheses and scenarios reported by the involved parties concerning the plausibility and consistency of statements and (analytical) facts. In order to outline the variety of challenges that doping control laboratories are facing besides providing optimal detection capabilities and analytical comprehensiveness, selected case vignettes involving the follow-up of unconventional adverse analytical findings, urine sample manipulation, drug/food contamination issues, and unexpected biotransformation reactions are thematized.

Recent advances in hopanoids analysis: Quantification protocols overview, main research targets and selected problems of complex data exploration.

Science.gov (United States)

Zarzycki, Paweł K; Portka, Joanna K

2015-09-01

Pentacyclic triterpenoids, particularly hopanoids, are organism-specific compounds and are generally considered as useful biomarkers that allow fingerprinting and classification of biological, environmental and geological samples. Simultaneous quantification of various hopanoids together with battery of related non-polar and low-molecular mass compounds may provide principal information for geochemical and environmental research focusing on both modern and ancient investigations. Target compounds can be derived from microbial biomass, water columns, sediments, coals, crude fossils or rocks. This create number of analytical problems due to different composition of the analytical matrix and interfering compounds and therefore, proper optimization of quantification protocols for such biomarkers is still the challenge. In this work we summarizing typical analytical protocols that were recently applied for quantification of hopanoids like compounds from different samples. Main steps including components of interest extraction, pre-purification, fractionation, derivatization and quantification involving gas (1D and 2D) as well as liquid separation techniques (liquid-liquid extraction, solid-phase extraction, planar and low resolution column chromatography, high-performance liquid chromatography) are described and discussed from practical point of view, mainly based on the experimental papers that were published within last two years, where significant increase in hopanoids research was noticed. The second aim of this review is to describe the latest research trends concerning determination of hopanoids and related low-molecular mass lipids analyzed in various samples including sediments, rocks, coals, crude oils and plant fossils as well as stromatolites and microbial biomass cultivated under different conditions. It has been found that majority of the most recent papers are based on uni- or bivariate approach for complex data analysis. Data interpretation involves

Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 1, Administrative

Energy Technology Data Exchange (ETDEWEB)

1992-06-01

Covered are: analytical laboratory operations (ALO) sample receipt and control, ALO data report/package preparation review and control, single shell tank (PST) project sample tracking system, sample receiving, analytical balances, duties and responsibilities of sample custodian, sample refrigerator temperature monitoring, security, assignment of staff responsibilities, sample storage, data reporting, and general requirements for glassware.

A new analytical application of nylon-induced room-temperature phosphorescence: Determination of thiabendazole in water samples

Energy Technology Data Exchange (ETDEWEB)

Correa, R.A. [Departamento de Quimica Analitica, Facultad de Ciencias Bioquimicas y Farmaceuticas, Universidad Nacional de Rosario, Suipacha 531 (2000) Rosario (Argentina); Escandar, G.M. [Departamento de Quimica Analitica, Facultad de Ciencias Bioquimicas y Farmaceuticas, Universidad Nacional de Rosario, Suipacha 531 (2000) Rosario (Argentina)]. E-mail: gescanda@fbioyf.unr.edu.ar

2006-06-30

This paper discusses the first analytical determination of the widely used fungicide thiabendazole by nylon-induced phosphorimetry. Nylon was investigated as a novel solid-matrix for inducing room-temperature phosphorescence of thiabendazole, which was enhanced under the effect of external heavy-atom salts. Among the investigated salts, lead(II) acetate was the most effective in yielding a high phosphorescence signal. An additional enhancement of the phosphorescence emission was attained when the measurements were carried out under a nitrogen atmosphere. There was only a moderate increase in the presence of cyclodextrins. The room-temperature phosphorescence lifetimes of the adsorbed thiabendazole were measured under different working conditions and, in all cases, two decaying components were detected. On the basis of the obtained results, a very simple and sensitive phosphorimetric method for the determination of thiabendazole was established. The analytical figures of merit obtained under the best experimental conditions were: linear calibration range from 0.031 to 0.26 {mu}g ml{sup -1} (the lowest value corresponds to the quantitation limit), relative standard deviation, 2.4% (n = 5) at a level of 0.096 {mu}g ml{sup -1}, and limit of detection calculated according to 1995 IUPAC Recommendations equal to 0.010 {mu}g ml{sup -1} (0.03 ng/spot). The potential interference from common agrochemicals was also studied. The feasibility of determining thiabendazole in real samples was successfully evaluated through the analysis of spiked river, tap and mineral water samples.

Efficiency of analytical and sampling-based uncertainty propagation in intensity-modulated proton therapy

Science.gov (United States)

Wahl, N.; Hennig, P.; Wieser, H. P.; Bangert, M.

2017-07-01

The sensitivity of intensity-modulated proton therapy (IMPT) treatment plans to uncertainties can be quantified and mitigated with robust/min-max and stochastic/probabilistic treatment analysis and optimization techniques. Those methods usually rely on sparse random, importance, or worst-case sampling. Inevitably, this imposes a trade-off between computational speed and accuracy of the uncertainty propagation. Here, we investigate analytical probabilistic modeling (APM) as an alternative for uncertainty propagation and minimization in IMPT that does not rely on scenario sampling. APM propagates probability distributions over range and setup uncertainties via a Gaussian pencil-beam approximation into moments of the probability distributions over the resulting dose in closed form. It supports arbitrary correlation models and allows for efficient incorporation of fractionation effects regarding random and systematic errors. We evaluate the trade-off between run-time and accuracy of APM uncertainty computations on three patient datasets. Results are compared against reference computations facilitating importance and random sampling. Two approximation techniques to accelerate uncertainty propagation and minimization based on probabilistic treatment plan optimization are presented. Runtimes are measured on CPU and GPU platforms, dosimetric accuracy is quantified in comparison to a sampling-based benchmark (5000 random samples). APM accurately propagates range and setup uncertainties into dose uncertainties at competitive run-times (GPU ≤slant {5} min). The resulting standard deviation (expectation value) of dose show average global γ{3% / {3}~mm} pass rates between 94.2% and 99.9% (98.4% and 100.0%). All investigated importance sampling strategies provided less accuracy at higher run-times considering only a single fraction. Considering fractionation, APM uncertainty propagation and treatment plan optimization was proven to be possible at constant time complexity

Radon in large buildings: The development of a protocol

International Nuclear Information System (INIS)

Wilson, D.L.; Dudney, C.S.; Gammage, R.B.

1993-01-01

Over the past several years, considerable research has been devoted by the US Environmental Protection Agency (USEPA) and others to develop radon sampling protocols for single family residences and schools. However, very little research has been performed on measuring radon in the work place. To evaluate possible sampling protocols, 833 buildings throughout the United States were selected for extensive radon testing. The buildings tested (warehouses, production plants and office buildings) were representative of commercial buildings across the country both in design, size and use. Based on the results, preliminary radon sampling protocols for the work place have been developed

Active SAmpling Protocol (ASAP) to Optimize Individual Neurocognitive Hypothesis Testing: A BCI-Inspired Dynamic Experimental Design.

Science.gov (United States)

Sanchez, Gaëtan; Lecaignard, Françoise; Otman, Anatole; Maby, Emmanuel; Mattout, Jérémie

2016-01-01

The relatively young field of Brain-Computer Interfaces has promoted the use of electrophysiology and neuroimaging in real-time. In the meantime, cognitive neuroscience studies, which make extensive use of functional exploration techniques, have evolved toward model-based experiments and fine hypothesis testing protocols. Although these two developments are mostly unrelated, we argue that, brought together, they may trigger an important shift in the way experimental paradigms are being designed, which should prove fruitful to both endeavors. This change simply consists in using real-time neuroimaging in order to optimize advanced neurocognitive hypothesis testing. We refer to this new approach as the instantiation of an Active SAmpling Protocol (ASAP). As opposed to classical (static) experimental protocols, ASAP implements online model comparison, enabling the optimization of design parameters (e.g., stimuli) during the course of data acquisition. This follows the well-known principle of sequential hypothesis testing. What is radically new, however, is our ability to perform online processing of the huge amount of complex data that brain imaging techniques provide. This is all the more relevant at a time when physiological and psychological processes are beginning to be approached using more realistic, generative models which may be difficult to tease apart empirically. Based upon Bayesian inference, ASAP proposes a generic and principled way to optimize experimental design adaptively. In this perspective paper, we summarize the main steps in ASAP. Using synthetic data we illustrate its superiority in selecting the right perceptual model compared to a classical design. Finally, we briefly discuss its future potential for basic and clinical neuroscience as well as some remaining challenges.

Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

Science.gov (United States)

Cantrell, John H., Jr.; Cantrell, Sean A.

2008-01-01

A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

Two analytical models for evaluating performance of Gigabit Ethernet Hosts

International Nuclear Information System (INIS)

Salah, K.

2006-01-01

Two analytical models are developed to study the impact of interrupt overhead on operating system performance of network hosts when subjected to Gigabit network traffic. Under heavy network traffic, the system performance will be negatively affected due to interrupt overhead caused by incoming traffic. In particular, excessive latency and significant degradation in system throughput can be experienced. Also user application may livelock as the CPU power is mostly consumed by interrupt handling and protocol processing. In this paper we present and compare two analytical models that capture host behavior and evaluate its performance. The first model is based Markov processes and queuing theory, while the second, which is more accurate but more complex is a pure Markov process. For the most part both models give mathematically-equivalent closed-form solutions for a number of important system performance metrics. These metrics include throughput, latency and stability condition, CPU utilization of interrupt handling and protocol processing and CPU availability for user applications. The analysis yields insight into understanding and predicting the impact of system and network choices on the performance of interrupt-driven systems when subjected to light and heavy network loads. More, importantly, our analytical work can also be valuable in improving host performance. The paper gives guidelines and recommendations to address design and implementation issues. Simulation and reported experimental results show that our analytical models are valid and give a good approximation. (author)

Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

Science.gov (United States)

Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

2017-02-01

Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

Capillary Electrophoresis Analysis of Organic Amines and Amino Acids in Saline and Acidic Samples Using the Mars Organic Analyzer

Science.gov (United States)

Stockton, Amanda M.; Chiesl, Thomas N.; Lowenstein, Tim K.; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A.

2009-11-01

The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pKa values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

[Pre-analytical stability before centrifugation of 7 biochemical analytes in whole blood].

Science.gov (United States)

Perrier-Cornet, Andreas; Moineau, Marie-Pierre; Narbonne, Valérie; Plee-Gautier, Emmanuelle; Le Saos, Fabienne; Carre, Jean-Luc

2015-01-01

The pre-analytical stability of 7 biochemical parameters (parathyroid hormone -PTH-, vitamins A, C E and D, 1,25-dihydroxyvitamin D and insulin) at +4 °C, was studied on whole blood samples before centrifugation. The impact of freezing at -20°C was also analyzed/performed for PTH and vitamin D. The differences in the results of assays for whole blood samples, being kept for different times between sampling time and analysis, from 9 healthy adults, were compaired by using a Student t test. The 7 analytes investigated remained stable up to 4 hours at +4°C in whole blood. This study showed that it is possible to accept uncentrifuged whole blood specimens kept at +4°C before analysis. PTH is affected by freezing whereas vitamin D is not.

Determination of 7BE in soil sample by gamma spectrometry for erosion researchs

International Nuclear Information System (INIS)

Esquivel, Alexander D.; Kastner, Geraldo F.; Amaral, Angela M.; Monteiro, Roberto Pellacani G.; Moreira, Rubens M.

2015-01-01

Cosmogenic 7 Be is a natural radiotracer produced in the stratosphere and troposphere and reached to the Earth surface via wet and dry fallout and hence its measurement for research of erosion in soils is very significant. The 7 Be radio analyse based on gamma spectrometry technique has been a routine methodology for decades and although is the reference procedure is not free of analytical interference. 7 Be is a β-γ emitting radionuclide (Eγ = 477.59 keV, T½ = 53.12d) and depending on the chemical profile of the soil its determination is susceptible to 228 Ac (E γ = 478.40 keV, T½ = 6.15h) interference. The aim of this work was to establish an analytical protocol for the 7 Be determination in soil samples from Juatuba-Mg region in different sampling periods of dry and rainy seasons for erosion studies and to establish some methodologies for evaluating and correcting the interference level of 228 Ac in the 7 Be activity measurements by gamma spectrometry. (author)

Electrophoretic extraction of low molecular weight cationic analytes from sodium dodecyl sulfate containing sample matrices for their direct electrospray ionization mass spectrometry.

Science.gov (United States)

Kinde, Tristan F; Lopez, Thomas D; Dutta, Debashis

2015-03-03

While the use of sodium dodecyl sulfate (SDS) in separation buffers allows efficient analysis of complex mixtures, its presence in the sample matrix is known to severely interfere with the mass-spectrometric characterization of analyte molecules. In this article, we report a microfluidic device that addresses this analytical challenge by enabling inline electrospray ionization mass spectrometry (ESI-MS) of low molecular weight cationic samples prepared in SDS containing matrices. The functionality of this device relies on the continuous extraction of analyte molecules into an SDS-free solvent stream based on the free-flow zone electrophoresis (FFZE) technique prior to their ESI-MS analysis. The reported extraction was accomplished in our current work in a glass channel with microelectrodes fabricated along its sidewalls to realize the desired electric field. Our experiments show that a key challenge to successfully operating such a device is to suppress the electroosmotically driven fluid circulations generated in its extraction channel that otherwise tend to vigorously mix the liquid streams flowing through this duct. A new coating medium, N-(2-triethoxysilylpropyl) formamide, recently demonstrated by our laboratory to nearly eliminate electroosmotic flow in glass microchannels was employed to address this issue. Applying this surface modifier, we were able to efficiently extract two different peptides, human angiotensin I and MRFA, individually from an SDS containing matrix using the FFZE method and detect them at concentrations down to 3.7 and 6.3 μg/mL, respectively, in samples containing as much as 10 mM SDS. Notice that in addition to greatly reducing the amount of SDS entering the MS instrument, the reported approach allows rapid solvent exchange for facilitating efficient analyte ionization desired in ESI-MS analysis.

Tissue Sampling Guides for Porcine Biomedical Models.

Science.gov (United States)

Albl, Barbara; Haesner, Serena; Braun-Reichhart, Christina; Streckel, Elisabeth; Renner, Simone; Seeliger, Frank; Wolf, Eckhard; Wanke, Rüdiger; Blutke, Andreas

2016-04-01

This article provides guidelines for organ and tissue sampling adapted to porcine animal models in translational medical research. Detailed protocols for the determination of sampling locations and numbers as well as recommendations on the orientation, size, and trimming direction of samples from ∼50 different porcine organs and tissues are provided in the Supplementary Material. The proposed sampling protocols include the generation of samples suitable for subsequent qualitative and quantitative analyses, including cryohistology, paraffin, and plastic histology; immunohistochemistry;in situhybridization; electron microscopy; and quantitative stereology as well as molecular analyses of DNA, RNA, proteins, metabolites, and electrolytes. With regard to the planned extent of sampling efforts, time, and personnel expenses, and dependent upon the scheduled analyses, different protocols are provided. These protocols are adjusted for (I) routine screenings, as used in general toxicity studies or in analyses of gene expression patterns or histopathological organ alterations, (II) advanced analyses of single organs/tissues, and (III) large-scale sampling procedures to be applied in biobank projects. Providing a robust reference for studies of porcine models, the described protocols will ensure the efficiency of sampling, the systematic recovery of high-quality samples representing the entire organ or tissue as well as the intra-/interstudy comparability and reproducibility of results. © The Author(s) 2016.

Pre-analytical and analytical validations and clinical applications of a miniaturized, simple and cost-effective solid phase extraction combined with LC-MS/MS for the simultaneous determination of catecholamines and metanephrines in spot urine samples.

Science.gov (United States)

Li, Xiaoguang Sunny; Li, Shu; Kellermann, Gottfried

2016-10-01

It remains a challenge to simultaneously quantify catecholamines and metanephrines in a simple, sensitive and cost-effective manner due to pre-analytical and analytical constraints. Herein, we describe such a method consisting of a miniaturized sample preparation and selective LC-MS/MS detection by the use of second morning spot urine samples. Ten microliters of second morning urine sample were subjected to solid phase extraction on an Oasis HLB microplate upon complexation with phenylboronic acid. The analytes were well-resolved on a Luna PFP column followed by tandem mass spectrometric detection. Full validation and suitability of spot urine sampling and biological variation were investigated. The extraction recovery and matrix effect are 74.1-97.3% and 84.1-119.0%, respectively. The linearity range is 2.5-500, 0.5-500, 2.5-1250, 2.5-1250 and 0.5-1250ng/mL for norepinephrine, epinephrine, dopamine, normetanephrine and metanephrine, respectively. The intra- and inter-assay imprecisions are ≤9.4% for spiked quality control samples, and the respective recoveries are 97.2-112.5% and 95.9-104.0%. The Deming regression slope is 0.90-1.08, and the mean Bland-Altman percentage difference is from -3.29 to 11.85 between a published and proposed method (n=50). A correlation observed for the spot and 24h urine collections is significant (n=20, p<0.0001, r: 0.84-0.95, slope: 0.61-0.98). No statistical differences are found in day-to-day biological variability (n=20). Reference intervals are established for an apparently healthy population (n=88). The developed method, being practical, sensitive, reliable and cost-effective, is expected to set a new stage for routine testing, basic research and clinical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Irregular analytical errors in diagnostic testing - a novel concept.

Science.gov (United States)

Vogeser, Michael; Seger, Christoph

2018-02-23

In laboratory medicine, routine periodic analyses for internal and external quality control measurements interpreted by statistical methods are mandatory for batch clearance. Data analysis of these process-oriented measurements allows for insight into random analytical variation and systematic calibration bias over time. However, in such a setting, any individual sample is not under individual quality control. The quality control measurements act only at the batch level. Quantitative or qualitative data derived for many effects and interferences associated with an individual diagnostic sample can compromise any analyte. It is obvious that a process for a quality-control-sample-based approach of quality assurance is not sensitive to such errors. To address the potential causes and nature of such analytical interference in individual samples more systematically, we suggest the introduction of a new term called the irregular (individual) analytical error. Practically, this term can be applied in any analytical assay that is traceable to a reference measurement system. For an individual sample an irregular analytical error is defined as an inaccuracy (which is the deviation from a reference measurement procedure result) of a test result that is so high it cannot be explained by measurement uncertainty of the utilized routine assay operating within the accepted limitations of the associated process quality control measurements. The deviation can be defined as the linear combination of the process measurement uncertainty and the method bias for the reference measurement system. Such errors should be coined irregular analytical errors of the individual sample. The measurement result is compromised either by an irregular effect associated with the individual composition (matrix) of the sample or an individual single sample associated processing error in the analytical process. Currently, the availability of reference measurement procedures is still highly limited, but LC

On Equivalence between Critical Probabilities of Dynamic Gossip Protocol and Static Site Percolation

Science.gov (United States)

Ishikawa, Tetsuya; Hayakawa, Tomohisa

The relationship between the critical probability of gossip protocol on the square lattice and the critical probability of site percolation on the square lattice is discussed. Specifically, these two critical probabilities are analytically shown to be equal to each other. Furthermore, we present a way of evaluating the critical probability of site percolation by approximating the saturation of gossip protocol. Finally, we provide numerical results which support the theoretical analysis.

Forensic analysis of high explosives residues in post-blast water samples employing solid phase extraction for analyte pro-concentration

International Nuclear Information System (INIS)

Umi Kalsom Ahmad; Rajendran, Sumathy; Ling, Lee Woan

2008-01-01

Nitro aromatic, nitramine and nitrate ester compounds are a major group of high order explosive or better known as military explosives. Octahydro-1,3,5,7-tetrazocine (HMX), 1,3,5-hexahydro-1,3,5-trinitro triazine (RDX), 2,4,6-trinitro-toluene (TNT), pentaerythritol tetranitrate (PETN) and 2,4-dinitrotoluene (2,4-DNT) are secondary high explosives classified as most commonly used explosives components. There is an increasing demand for pre-concentration of these compounds in water samples as the sensitivity achieved by instrumental analytical methods for these high explosives residues are the main drawback in the application at trace levels for forensic analysis. Hence, a simple cartridge solid phase extraction (SPE) procedure was optimized as the off-line extraction and pre-concentration method to enhance the detection limit of high explosive residues using micellar electrokinetic chromatography (MEKC) and gas chromatography with electron-capture detection (GC-ECD) methods. The SPE cartridges utilized LiChrolut EN as the SPE adsorbent. By emplying pre-concentration using SPE, the detection limits of the target analytes in water sample were lowered by more than 1000 times with good percentage recovery (>87%) for MEKC method and lowered by 120 times with more than 2 % percentage recovery for GC-ECD methods. In order to test the feasibility of the developed method to real cases, post-blast water samples were analyzed. The post-blast water samples which were collected from Baling Bom training range, Ulu Kinta, Perak contained RDX and PETN in the range of 0.05 - 0.17 ppm and 0.0124 - 0.0390 ppm respectively. (author)

Hopping control channel MAC protocol for opportunistic spectrum access networks

Institute of Scientific and Technical Information of China (English)

FU Jing-tuan; JI Hong; MAO Xu

2010-01-01

Opportunistic spectrum access （OSA） is considered as a promising approach to mitigate spectrum scarcity by allowing unlicensed users to exploit spectrum opportunities in licensed frequency bands. Derived from the existing channel-hopping multiple access （CHMA） protocol,we introduce a hopping control channel medium access control （MAC） protocol in the context of OSA networks. In our proposed protocol,all nodes in the network follow a common channel-hopping sequence; every frequency channel can be used as control channel and data channel. Considering primary users＇ occupancy of the channel,we use a primary user （PU） detection model to calculate the channel availability for unlicensed users＇ access. Then,a discrete Markov chain analytical model is applied to describe the channel states and deduce the system throughput. Through simulation,we present numerical results to demonstrate the throughput performance of our protocol and thus validate our work.

First Total Reflection X-Ray Fluorescence round-robin test of water samples: Preliminary results

Energy Technology Data Exchange (ETDEWEB)

Borgese, Laura; Bilo, Fabjola [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy); Tsuji, Kouichi [Graduate School of Engineering, Osaka City University, Osaka (Japan); Fernández-Ruiz, Ramón [Servicio Interdepartamental de Investigación (SIdI), Laboratorio de TXRF, Universidad Autónoma de Madrid, Madrid (Spain); Margui, Eva [Department of Chemistry, University of Girona, Girona (Spain); Streli, Christina [TU Wien, Atominstitut,Radiation Physics, Vienna (Austria); Pepponi, Giancarlo [Fondazione Bruno Kessler, Povo, Trento (Italy); Stosnach, Hagen [Bruker Nano GmbH, Berlin (Germany); Yamada, Takashi [Rigaku Corporation, Takatsuki, Osaka (Japan); Vandenabeele, Peter [Department of Archaeology, Ghent University, Ghent (Belgium); Maina, David M.; Gatari, Michael [Institute of Nuclear Science and Technology, University of Nairobi, Nairobi (Kenya); Shepherd, Keith D.; Towett, Erick K. [World Agroforestry Centre (ICRAF), Nairobi (Kenya); Bennun, Leonardo [Laboratorio de Física Aplicada, Departamento de Física, Universidad de Concepción (Chile); Custo, Graciela; Vasquez, Cristina [Gerencia Química, Laboratorio B025, Centro Atómico Constituyentes, San Martín (Argentina); Depero, Laura E., E-mail: laura.depero@unibs.it [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy)

2014-11-01

Total Reflection X-Ray Fluorescence (TXRF) is a mature technique to evaluate quantitatively the elemental composition of liquid samples deposited on clean and well polished reflectors. In this paper the results of the first worldwide TXRF round-robin test of water samples, involving 18 laboratories in 10 countries are presented and discussed. The test was performed within the framework of the VAMAS project, interlaboratory comparison of TXRF spectroscopy for environmental analysis, whose aim is to develop guidelines and a standard methodology for biological and environmental analysis by means of the TXRF analytical technique. - Highlights: • The discussion of the first worldwide TXRF round-robin test of water samples (18 laboratories of 10 countries) is reported. • Drinking, waste, and desalinated water samples were tested. • Data dispersion sources were identified: sample concentration, preparation, fitting procedure, and quantification. • The protocol for TXRF analysis of drinking water is proposed.

An analytical model for the performance of geographical multi-hop broadcast

NARCIS (Netherlands)

Klein Wolterink, W.; Heijenk, G.; Berg, J.L. van den

2012-01-01

In this paper we present an analytical model accurately describing the behaviour of a multi-hop broadcast protocol. Our model covers the scenario in which a message is forwarded over a straight road and inter-node distances are distributed exponentially. Intermediate forwarders draw a small random

Microfluidic devices for sample clean-up and screening of biological samples

NARCIS (Netherlands)

Tetala, K.K.R.

2009-01-01

Analytical chemistry plays an important role in the separation and identification of analytes from raw samples (e.g. plant extracts, blood), but the whole analytical process is tedious, difficult to automate and time consuming. To overcome these drawbacks, the concept of μTAS (miniaturized total

ISCO Grab Sample Ion Chromatography Analytical Data

Data.gov (United States)

U.S. Environmental Protection Agency — ISCO grab samples were collected from river, wastewater treatment plant discharge, and public drinking water intakes. Samples were analyzed for major ions (ppb)...

Persistent RCSMA: A MAC Protocol for a Distributed Cooperative ARQ Scheme in Wireless Networks

Directory of Open Access Journals (Sweden)

J. Alonso-Zárate

2008-05-01

Full Text Available The persistent relay carrier sensing multiple access (PRCSMA protocol is presented in this paper as a novel medium access control (MAC protocol that allows for the execution of a distributed cooperative automatic retransmission request (ARQ scheme in IEEE 802.11 wireless networks. The underlying idea of the PRCSMA protocol is to modify the basic rules of the IEEE 802.11 MAC protocol to execute a distributed cooperative ARQ scheme in wireless networks in order to enhance their performance and to extend coverage. A closed formulation of the distributed cooperative ARQ average packet transmission delay in a saturated network is derived in the paper. The analytical equations are then used to evaluate the performance of the protocol under different network configurations. Both the accuracy of the analysis and the performance evaluation of the protocol are supported and validated through computer simulations.

VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

Energy Technology Data Exchange (ETDEWEB)

Ekechukwu, A

2009-05-27

Method validation is the process of evaluating whether an analytical method is acceptable for its intended purpose. For pharmaceutical methods, guidelines from the United States Pharmacopeia (USP), International Conference on Harmonisation (ICH), and the United States Food and Drug Administration (USFDA) provide a framework for performing such valications. In general, methods for regulatory compliance must include studies on specificity, linearity, accuracy, precision, range, detection limit, quantitation limit, and robustness. Elements of these guidelines are readily adapted to the issue of validation for beryllium sampling and analysis. This document provides a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers and books reviewed is given in the Appendix. Available validation documents and guides are listed therein; each has a brief description of application and use. In the referenced sources, there are varying approches to validation and varying descriptions of the valication process at different stages in method development. This discussion focuses on valication and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all referenced documents were published in English.

The Nagoya Protocol: Fragmentation or Consolidation?

Directory of Open Access Journals (Sweden)

Carmen Richerzhagen

2014-02-01

Full Text Available In October, 2010, a protocol on access and benefit-sharing (ABS of genetic resources was adopted, the so-called Nagoya Protocol on Access to Genetic Resources and the Fair and Equitable Sharing of Benefits Arising from their Utilization to the Convention on Biological Diversity. Before the adoption of the Nagoya Protocol, the governance architecture of ABS was already characterized by a multifaceted institutional environment. The use of genetic resources is confronted with many issues (conservation, research and development, intellectual property rights, food security, health issues, climate change that are governed by different institutions and agreements. The Nagoya Protocol contributes to increased fragmentation. However, the question arises whether this new regulatory framework can help to advance the implementation of the ABS provisions of the Convention on Biological Diversity (CBD. This paper attempts to find an answer to that question by following three analytical steps. First, it analyzes the causes of change against the background of theories of institutional change. Second, it aims to assess the typology of the architecture in order to find out if this new set of rules will contribute to a more synergistic, cooperative or conflictive architecture of ABS governance. Third, the paper looks at the problem of “fit” and identifies criteria that can be used to assess the new ABS governance architecture with regard to its effectiveness.

Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

Science.gov (United States)

Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

2015-08-28

Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.

Strategies for achieving high sequencing accuracy for low diversity samples and avoiding sample bleeding using illumina platform.

Science.gov (United States)

Mitra, Abhishek; Skrzypczak, Magdalena; Ginalski, Krzysztof; Rowicka, Maga

2015-01-01

Sequencing microRNA, reduced representation sequencing, Hi-C technology and any method requiring the use of in-house barcodes result in sequencing libraries with low initial sequence diversity. Sequencing such data on the Illumina platform typically produces low quality data due to the limitations of the Illumina cluster calling algorithm. Moreover, even in the case of diverse samples, these limitations are causing substantial inaccuracies in multiplexed sample assignment (sample bleeding). Such inaccuracies are unacceptable in clinical applications, and in some other fields (e.g. detection of rare variants). Here, we discuss how both problems with quality of low-diversity samples and sample bleeding are caused by incorrect detection of clusters on the flowcell during initial sequencing cycles. We propose simple software modifications (Long Template Protocol) that overcome this problem. We present experimental results showing that our Long Template Protocol remarkably increases data quality for low diversity samples, as compared with the standard analysis protocol; it also substantially reduces sample bleeding for all samples. For comprehensiveness, we also discuss and compare experimental results from alternative approaches to sequencing low diversity samples. First, we discuss how the low diversity problem, if caused by barcodes, can be avoided altogether at the barcode design stage. Second and third, we present modified guidelines, which are more stringent than the manufacturer's, for mixing low diversity samples with diverse samples and lowering cluster density, which in our experience consistently produces high quality data from low diversity samples. Fourth and fifth, we present rescue strategies that can be applied when sequencing results in low quality data and when there is no more biological material available. In such cases, we propose that the flowcell be re-hybridized and sequenced again using our Long Template Protocol. Alternatively, we discuss how

Strategies for achieving high sequencing accuracy for low diversity samples and avoiding sample bleeding using illumina platform.

Directory of Open Access Journals (Sweden)

Abhishek Mitra

Full Text Available Sequencing microRNA, reduced representation sequencing, Hi-C technology and any method requiring the use of in-house barcodes result in sequencing libraries with low initial sequence diversity. Sequencing such data on the Illumina platform typically produces low quality data due to the limitations of the Illumina cluster calling algorithm. Moreover, even in the case of diverse samples, these limitations are causing substantial inaccuracies in multiplexed sample assignment (sample bleeding. Such inaccuracies are unacceptable in clinical applications, and in some other fields (e.g. detection of rare variants. Here, we discuss how both problems with quality of low-diversity samples and sample bleeding are caused by incorrect detection of clusters on the flowcell during initial sequencing cycles. We propose simple software modifications (Long Template Protocol that overcome this problem. We present experimental results showing that our Long Template Protocol remarkably increases data quality for low diversity samples, as compared with the standard analysis protocol; it also substantially reduces sample bleeding for all samples. For comprehensiveness, we also discuss and compare experimental results from alternative approaches to sequencing low diversity samples. First, we discuss how the low diversity problem, if caused by barcodes, can be avoided altogether at the barcode design stage. Second and third, we present modified guidelines, which are more stringent than the manufacturer's, for mixing low diversity samples with diverse samples and lowering cluster density, which in our experience consistently produces high quality data from low diversity samples. Fourth and fifth, we present rescue strategies that can be applied when sequencing results in low quality data and when there is no more biological material available. In such cases, we propose that the flowcell be re-hybridized and sequenced again using our Long Template Protocol. Alternatively

Effect of variable rates of daily sampling of fly larvae on decomposition and carrion insect community assembly: implications for forensic entomology field study protocols.

Science.gov (United States)

Michaud, Jean-Philippe; Moreau, Gaétan

2013-07-01

Experimental protocols in forensic entomology successional field studies generally involve daily sampling of insects to document temporal changes in species composition on animal carcasses. One challenge with that method has been to adjust the sampling intensity to obtain the best representation of the community present without affecting the said community. To this date, little is known about how such investigator perturbations affect decomposition-related processes. Here, we investigated how different levels of daily sampling of fly eggs and fly larvae affected, over time, carcass decomposition rate and the carrion insect community. Results indicated that a daily sampling of forensic entomology successional field studies.

Non-porous membrane-assisted liquid-liquid extraction of UV filter compounds from water samples.

Science.gov (United States)

Rodil, Rosario; Schrader, Steffi; Moeder, Monika

2009-06-12

A method for the determination of nine UV filter compounds [benzophenone-3 (BP-3), isoamyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene (OC), butyl methoxydibenzoylmethane, ethylhexyl dimethyl p-aminobenzoate (OD-PABA), ethylhexyl methoxycinnamate (EHMC), ethylhexyl salicylate and homosalate] in water samples was developed and evaluated. The procedure includes non-porous membrane-assisted liquid-liquid extraction (MALLE) and LC-atmospheric pressure photoionization (APPI)-MS/MS. Membrane bags made of different polymeric materials were examined to enable a fast and simple extraction of the target analytes. Among the polymeric materials tested, low- and high-density polyethylene membranes proved to be well suited to adsorb the analytes from water samples. Finally, 2 cm length tailor-made membrane bags were prepared from low-density polyethylene in order to accommodate 100 microL of propanol. The fully optimised protocol provides recoveries from 76% to 101% and limits of detection (LOD) between 0.4 ng L(-1) (OD-PABA) and 16 ng L(-1) (EHMC). The interday repeatability of the whole protocol was below 18%. The effective separation of matrix molecules was proved by only marginal matrix influence during the APPI-MS analysis since no ion suppression effects were observed. During the extraction step, the influence of the matrix was only significant when non-treated wastewater was analysed. The analysis of lake water indicated the presence of seven UV filter compounds included in this study at concentrations between 40 ng L(-1) (BP-3) and 4381 ng L(-1) (OC). In non-treated wastewater several UV filters were also detected at concentration levels as high as 5322 ng L(-1) (OC).

Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples.

Science.gov (United States)

Gerace, E; Salomone, A; Abbadessa, G; Racca, S; Vincenti, M

2012-02-01

A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

A rapid and reliable method for Pb isotopic analysis of peat and lichens by laser ablation-quadrupole-inductively coupled plasma-mass spectrometry for biomonitoring and sample screening

International Nuclear Information System (INIS)

Kylander, M.E.; Weiss, D.J.; Jeffries, T.E.; Kober, B.; Dolgopolova, A.; Garcia-Sanchez, R.; Coles, B.J.

2007-01-01

An analytical protocol for rapid and reliable laser ablation-quadrupole (LA-Q)- and multi-collector (MC-) inductively coupled plasma-mass spectrometry (ICP-MS) analysis of Pb isotope ratios ( 207 Pb/ 206 Pb and 208 Pb/ 206 Pb) in peats and lichens is developed. This technique is applicable to source tracing atmospheric Pb deposition in biomonitoring studies and sample screening. Reference materials and environmental samples were dry ashed and pressed into pellets for introduction by laser ablation. No binder was used to reduce contamination. LA-MC-ICP-MS internal and external precisions were 207 Pb/ 206 Pb and 208 Pb/ 206 Pb ratios. LA-Q-ICP-MS internal precisions on 207 Pb/ 206 Pb and 208 Pb/ 206 Pb ratios were lower with values for the different sample sets 208 Pb by Q-ICP-MS are identified as sources of reduced analytical performance

Role of analytical chemistry in environmental monitoring

International Nuclear Information System (INIS)

Kayasth, S.; Swain, K.

2004-01-01

Basic aspects of pollution and the role of analytical chemistry in environmental monitoring are highlighted and exemplified, with emphasis on trace elements. Sources and pathways of natural and especially man-made polluting substances as well as physico-chemical characteristics are given. Attention is paid to adequate sampling in various compartments of the environment comprising both lithosphere and biosphere. Trace analysis is dealt with using a variety of analytical techniques, including criteria for choice of suited techniques, as well as aspects of analytical quality assurance and control. Finally, some data on trace elements levels in soil and water samples from India are presented. (author)

Manual of selected physico-chemical analytical methods. IV

International Nuclear Information System (INIS)

Beran, M.; Klosova, E.; Krtil, J.; Sus, F.; Kuvik, V.; Vrbova, L.; Hamplova, M.; Lengyel, J.; Kelnar, L.; Zakouril, K.

1990-11-01

The Central Testing Laboratory of the Nuclear Research Institute at Rez has for a decade been participating in the development of analytical procedures and has been providing analyses of samples of different types and origin. The analytical procedures developed have been published in special journals and a number of them in the Manuals of analytical methods, in three parts. The 4th part of the Manual contains selected physico-chemical methods developed or modified by the Laboratory in the years 1986-1990 within the project ''Development of physico-chemical analytical methods''. In most cases, techniques are involved for non-nuclear applications. Some can find wider applications, especially in analyses of environmental samples. Others have been developed for specific cases of sample analyses or require special instrumentation (mass spectrometer), which partly restricts their applicability by other institutions. (author)

Chasing the effects of Pre-analytical Confounders - a Multicentre Study on CSF-AD biomarkers

Directory of Open Access Journals (Sweden)

Maria Joao Leitao

2015-07-01

Full Text Available Core cerebrospinal fluid (CSF biomarkers-Aβ42, Tau and pTau–have been recently incorporated in the revised criteria for Alzheimer’s disease (AD. However, their widespread clinical application lacks standardization. Pre-analytical sample handling and storage play an important role in the reliable measurement of these biomarkers across laboratories. In this study, we aim to surpass the efforts from previous studies, by employing a multicentre approach to assess the impact of less studied CSF pre-analytical confounders in AD-biomarkers quantification. Four different centres participated in this study and followed the same established protocol. CSF samples were analysed for three biomarkers (Aβ42, Tau and pTau and tested for different spinning conditions (temperature: Room temperature (RT vs. 4oC; speed: 500g vs. 2000g vs. 3000g, storage volume variations (25%, 50% and 75% of tube total volume as well as freezing-thaw cycles (up to 5 cyles. The influence of sample routine parameters, inter-centre variability and relative value of each biomarker (reported as normal/abnormal, was analysed. Centrifugation conditions did not influence biomarkers levels, except for samples with a high CSF total protein content, where either non centrifugation or centrifugation at RT, compared to 4ºC, led to higher Aβ42 levels. Reducing CSF storage volume from 75% to 50% of total tube capacity, decreased Aβ42 concentration (within analytical CV of the assay, whereas no change in Tau or pTau was observed. Moreover, the concentration of Tau and pTau appears to be stable up to 5 freeze-thaw cycles, whereas Aβ42 levels decrease if CSF is freeze-thawed more than 3 times. This systematic study reinforces the need for CSF centrifugation at 4ºC prior to storage and highlights the influence of storage conditions in Aβ42 levels. This study contributes to the establishment of harmonized standard operating procedures that will help reducing inter-lab variability of CSF

Analytical Validation of Quantitative Real-Time PCR Methods for Quantification of Trypanosoma cruzi DNA in Blood Samples from Chagas Disease Patients.

Science.gov (United States)

Ramírez, Juan Carlos; Cura, Carolina Inés; da Cruz Moreira, Otacilio; Lages-Silva, Eliane; Juiz, Natalia; Velázquez, Elsa; Ramírez, Juan David; Alberti, Anahí; Pavia, Paula; Flores-Chávez, María Delmans; Muñoz-Calderón, Arturo; Pérez-Morales, Deyanira; Santalla, José; Marcos da Matta Guedes, Paulo; Peneau, Julie; Marcet, Paula; Padilla, Carlos; Cruz-Robles, David; Valencia, Edward; Crisante, Gladys Elena; Greif, Gonzalo; Zulantay, Inés; Costales, Jaime Alfredo; Alvarez-Martínez, Miriam; Martínez, Norma Edith; Villarroel, Rodrigo; Villarroel, Sandro; Sánchez, Zunilda; Bisio, Margarita; Parrado, Rudy; Maria da Cunha Galvão, Lúcia; Jácome da Câmara, Antonia Cláudia; Espinoza, Bertha; Alarcón de Noya, Belkisyole; Puerta, Concepción; Riarte, Adelina; Diosque, Patricio; Sosa-Estani, Sergio; Guhl, Felipe; Ribeiro, Isabela; Aznar, Christine; Britto, Constança; Yadón, Zaida Estela; Schijman, Alejandro G

2015-09-01

An international study was performed by 26 experienced PCR laboratories from 14 countries to assess the performance of duplex quantitative real-time PCR (qPCR) strategies on the basis of TaqMan probes for detection and quantification of parasitic loads in peripheral blood samples from Chagas disease patients. Two methods were studied: Satellite DNA (SatDNA) qPCR and kinetoplastid DNA (kDNA) qPCR. Both methods included an internal amplification control. Reportable range, analytical sensitivity, limits of detection and quantification, and precision were estimated according to international guidelines. In addition, inclusivity and exclusivity were estimated with DNA from stocks representing the different Trypanosoma cruzi discrete typing units and Trypanosoma rangeli and Leishmania spp. Both methods were challenged against 156 blood samples provided by the participant laboratories, including samples from acute and chronic patients with varied clinical findings, infected by oral route or vectorial transmission. kDNA qPCR showed better analytical sensitivity than SatDNA qPCR with limits of detection of 0.23 and 0.70 parasite equivalents/mL, respectively. Analyses of clinical samples revealed a high concordance in terms of sensitivity and parasitic loads determined by both SatDNA and kDNA qPCRs. This effort is a major step toward international validation of qPCR methods for the quantification of T. cruzi DNA in human blood samples, aiming to provide an accurate surrogate biomarker for diagnosis and treatment monitoring for patients with Chagas disease. Copyright © 2015 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

Comparison of the analytical methods used to determine natural and artificial radionuclides from environmental samples by gamma, alpha and beta spectrometry

DEFF Research Database (Denmark)

Pöllänen, Roy; Virtanen, Sinikka; Kämäräinen, Meerit

In CAMNAR, an extensive interlaboratory exercise on the analytical methods used to determine several radionuclides present in the environmental samples was organized. Activity concentration of different natural radionuclides, such as Rn-222, Pb-210, Po-210, K-40, Ra-226, Ra-228 and isotopes...... of uranium, in addition to artificial Cs-137 and Am-241 were analysed from lake sediment samples and drinking water. The measurement techniques were gamma-ray spectrometry, alpha spectrometry, liquid scintillation counting and inductively coupled plasma mass spectrometry. Twenty six laboratories from nine...

Development of an analytical microbial consortia method for enhancing performance monitoring at aerobic wastewater treatment plants.

Science.gov (United States)

Razban, Behrooz; Nelson, Kristina Y; McMartin, Dena W; Cullimore, D Roy; Wall, Michelle; Wang, Dunling

2012-01-01

An analytical method to produce profiles of bacterial biomass fatty acid methyl esters (FAME) was developed employing rapid agitation followed by static incubation (RASI) using selective media of wastewater microbial communities. The results were compiled to produce a unique library for comparison and performance analysis at a Wastewater Treatment Plant (WWTP). A total of 146 samples from the aerated WWTP, comprising 73 samples of each secondary and tertiary effluent, were included analyzed. For comparison purposes, all samples were evaluated via a similarity index (SI) with secondary effluents producing an SI of 0.88 with 2.7% variation and tertiary samples producing an SI 0.86 with 5.0% variation. The results also highlighted significant differences between the fatty acid profiles of the tertiary and secondary effluents indicating considerable shifts in the bacterial community profile between these treatment phases. The WWTP performance results using this method were highly replicable and reproducible indicating that the protocol has potential as a performance-monitoring tool for aerated WWTPs. The results quickly and accurately reflect shifts in dominant bacterial communities that result when processes operations and performance change.

Dysphonia risk screening protocol

Science.gov (United States)

Nemr, Katia; Simões-Zenari, Marcia; da Trindade Duarte, João Marcos; Lobrigate, Karen Elena; Bagatini, Flavia Alves

2016-01-01

OBJECTIVE: To propose and test the applicability of a dysphonia risk screening protocol with score calculation in individuals with and without dysphonia. METHOD: This descriptive cross-sectional study included 365 individuals (41 children, 142 adult women, 91 adult men and 91 seniors) divided into a dysphonic group and a non-dysphonic group. The protocol consisted of 18 questions and a score was calculated using a 10-cm visual analog scale. The measured value on the visual analog scale was added to the overall score, along with other partial scores. Speech samples allowed for analysis/assessment of the overall degree of vocal deviation and initial definition of the respective groups and after six months, the separation of the groups was confirmed using an acoustic analysis. RESULTS: The mean total scores were different between the groups in all samples. Values ranged between 37.0 and 57.85 in the dysphonic group and between 12.95 and 19.28 in the non-dysphonic group, with overall means of 46.09 and 15.55, respectively. High sensitivity and specificity were demonstrated when discriminating between the groups with the following cut-off points: 22.50 (children), 29.25 (adult women), 22.75 (adult men), and 27.10 (seniors). CONCLUSION: The protocol demonstrated high sensitivity and specificity in differentiating groups of individuals with and without dysphonia in different sample groups and is thus an effective instrument for use in voice clinics. PMID:27074171

Dysphonia risk screening protocol

Directory of Open Access Journals (Sweden)

Katia Nemr

2016-03-01

Full Text Available OBJECTIVE: To propose and test the applicability of a dysphonia risk screening protocol with score calculation in individuals with and without dysphonia. METHOD: This descriptive cross-sectional study included 365 individuals (41 children, 142 adult women, 91 adult men and 91 seniors divided into a dysphonic group and a non-dysphonic group. The protocol consisted of 18 questions and a score was calculated using a 10-cm visual analog scale. The measured value on the visual analog scale was added to the overall score, along with other partial scores. Speech samples allowed for analysis/assessment of the overall degree of vocal deviation and initial definition of the respective groups and after six months, the separation of the groups was confirmed using an acoustic analysis. RESULTS: The mean total scores were different between the groups in all samples. Values ranged between 37.0 and 57.85 in the dysphonic group and between 12.95 and 19.28 in the non-dysphonic group, with overall means of 46.09 and 15.55, respectively. High sensitivity and specificity were demonstrated when discriminating between the groups with the following cut-off points: 22.50 (children, 29.25 (adult women, 22.75 (adult men, and 27.10 (seniors. CONCLUSION: The protocol demonstrated high sensitivity and specificity in differentiating groups of individuals with and without dysphonia in different sample groups and is thus an effective instrument for use in voice clinics.

System effects in sample self-stacking CZE: Single analyte peak splitting of salt-containing samples

Czech Academy of Sciences Publication Activity Database

Malá, Zdeňka; Gebauer, Petr; Boček, Petr

2009-01-01

Roč. 30, č. 5 (2009), s. 866-874 ISSN 0173-0835 R&D Projects: GA ČR GA203/08/1536; GA AV ČR IAA400310609; GA AV ČR IAA400310703 Institutional research plan: CEZ:AV0Z40310501 Keywords : CZE * peak splitting * self-stacking Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.077, year: 2009

Sampling practices and analytical techniques used in the monitoring of steam and water in CEGB nuclear boilers

International Nuclear Information System (INIS)

Goodfellow, G.I.

1978-01-01

The steam and water in CEGB Magnox and AGR nuclear boilers are continuously monitored, using both laboratory techniques and on-line instrumentation, in order to maintain the chemical quality within pre-determined limits. The sampling systems in use and some of the difficulties associated with sampling requirements are discussed. The relative merits of chemical instruments installed either locally in various parts of the plant or in centralized instrument rooms are reviewed. The quality of water in nuclear boilers, as with all high-pressure steam-raising plant, is extremely high; consequently very sensitive analytical procedures are required, particularly for monitoring the feed-water of 'once-through boiler' systems. Considerable progress has been made in this field and examples are given of some of the techniques developed for analyses at the 'μ/kg' level together with some of the current problems.(author)

Evaluation and standardisation of fast analytical techniques for destructive radwaste control

International Nuclear Information System (INIS)

De Simone, A.; Troiani, F.

2001-01-01

The document describes the work programme carried out by the Laboratorio Nazionale per la 'Caratterizzazione dei Refit Radioattivi', in the frame of the European research project Destructive Radwaste Control. The main tasks of the research work were the evaluation of fast sample pre-treatment procedures and the development of chromatographic methods coupled to fast nuclide detection by Liquid Scintillation Counting. In order to test the High Performance Ion Chromatograph (HPIC) coupled to the Liquid Scintillation Counter (LSC) on high salt content solutions, synthetic cement solutions have been prepared and spiked with several β-emitters hard to be measured with non-destructive analyses, along with other radionuclides important for the determination of the radiological inventory in radwastes. As the validation tests for the new analytical methods involved the manipulation of radioactive solutions, a remote area for HPIC-LSC apparatus has been designed and performed, in order to operate in safe conditions. According to the research programme, fast analytical methods for the chemical separation and radionuclide detection of the radioactive elements of interest, have been developed and qualified. From the results of the work, some protocols of analysis have been defined: they contain all information about operative conditions for HPIC-LSC apparatus, field of applicability, chemical and radioactive detection limits [it

21 CFR 660.6 - Samples; protocols; official release.

Science.gov (United States)

2010-04-01

... product iodinated with 125I means a sample from each lot of diagnostic test kits in a finished package... manufacturer has satisfactorily completed all tests on the samples: (i) One sample until written notification... of this section, a sample of product not iodinated with 125I means a sample from each filling of each...

Dynamic Channel Slot Allocation Scheme and Performance Analysis of Cyclic Quorum Multichannel MAC Protocol

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Xing Hu

2017-01-01

Full Text Available In high diversity node situation, multichannel MAC protocol can improve the frequency efficiency, owing to fewer collisions compared with single-channel MAC protocol. And the performance of cyclic quorum-based multichannel (CQM MAC protocol is outstanding. Based on cyclic quorum system and channel slot allocation, it can avoid the bottleneck that others suffered from and can be easily realized with only one transceiver. To obtain the accurate performance of CQM MAC protocol, a Markov chain model, which combines the channel-hopping strategy of CQM protocol and IEEE 802.11 distributed coordination function (DCF, is proposed. The results of numerical analysis show that the optimal performance of CQM protocol can be obtained in saturation bound situation. And then we obtain the saturation bound of CQM system by bird swarm algorithm. In addition, to improve the performance of CQM protocol in unsaturation situation, a dynamic channel slot allocation of CQM (DCQM protocol is proposed, based on wavelet neural network. Finally, the performance of CQM protocol and DCQM protocol is simulated by Qualnet platform. And the simulation results show that the analytic and simulation results match very well; the DCQM performs better in unsaturation situation.

Efficient MAC Protocol for Hybrid Wireless Network with Heterogeneous Sensor Nodes

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Md. Nasre Alam

2016-01-01

Full Text Available Although several Directional Medium Access Control (DMAC protocols have been designed for use with homogeneous networks, it can take a substantial amount of time to change sensor nodes that are equipped with an omnidirectional antenna for sensor nodes with a directional antenna. Thus, we require a novel MAC protocol for use with an intermediate wireless network that consists of heterogeneous sensor nodes equipped with either an omnidirectional antenna or a directional antenna. The MAC protocols that have been designed for use in homogeneous networks are not suitable for use in a hybrid network due to deaf, hidden, and exposed nodes. Therefore, we propose a MAC protocol that exploits the characteristics of a directional antenna and can also work efficiently with omnidirectional nodes in a hybrid network. In order to address the deaf, hidden, and exposed node problems, we define RTS/CTS for the neighbor (RTSN/CTSN and Neighbor Information (NIP packets. The performance of the proposed MAC protocol is evaluated through a numerical analysis using a Markov model. In addition, the analytical results of the MAC protocol are verified through an OPNET simulation.

ANALYTICAL TECHNIQUES FOR THE DETERMINATION OF MELOXICAM IN PHARMACEUTICAL FORMULATIONS AND BIOLOGICAL SAMPLES

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Aisha Noreen

2016-06-01

Full Text Available Meloxicam (MX belongs to the family of oxicams which is the most important group of non steroidal anti-inflammatory drugs (NSAIDs and is widely used for their analgesics and antipyretic activities. It inhibits both COX-I and COX-II enzymes with less gastric and local tissues irritation. A number of analytical techniques have been used for the determination of MX in pharmaceutical as well as in biological fluids. These techniques include titrimetry, spectrometry, chromatography, flow injection spectrometry, fluorescence spectrometry, capillary zone electrophoresis and electrochemical techniques. Many of these techniques have also been used for the simultaneous determination of MX with other compounds. A comprehensive review of these analytical techniques has been done which could be useful for the analytical chemists and quality control pharmacists.

Prevalence of Pre-Analytical Errors in Clinical Chemistry Diagnostic Labs in Sulaimani City of Iraqi Kurdistan.

Science.gov (United States)

Najat, Dereen

2017-01-01

Laboratory testing is roughly divided into three phases: a pre-analytical phase, an analytical phase and a post-analytical phase. Most analytical errors have been attributed to the analytical phase. However, recent studies have shown that up to 70% of analytical errors reflect the pre-analytical phase. The pre-analytical phase comprises all processes from the time a laboratory request is made by a physician until the specimen is analyzed at the lab. Generally, the pre-analytical phase includes patient preparation, specimen transportation, specimen collection and storage. In the present study, we report the first comprehensive assessment of the frequency and types of pre-analytical errors at the Sulaimani diagnostic labs in Iraqi Kurdistan. Over 2 months, 5500 venous blood samples were observed in 10 public diagnostic labs of Sulaimani City. The percentages of rejected samples and types of sample inappropriateness were evaluated. The percentage of each of the following pre-analytical errors were recorded: delay in sample transportation, clotted samples, expired reagents, hemolyzed samples, samples not on ice, incorrect sample identification, insufficient sample, tube broken in centrifuge, request procedure errors, sample mix-ups, communication conflicts, misinterpreted orders, lipemic samples, contaminated samples and missed physician's request orders. The difference between the relative frequencies of errors observed in the hospitals considered was tested using a proportional Z test. In particular, the survey aimed to discover whether analytical errors were recorded and examine the types of platforms used in the selected diagnostic labs. The analysis showed a high prevalence of improper sample handling during the pre-analytical phase. In appropriate samples, the percentage error was as high as 39%. The major reasons for rejection were hemolyzed samples (9%), incorrect sample identification (8%) and clotted samples (6%). Most quality control schemes at Sulaimani

Prevalence of Pre-Analytical Errors in Clinical Chemistry Diagnostic Labs in Sulaimani City of Iraqi Kurdistan.

Directory of Open Access Journals (Sweden)

Dereen Najat

Full Text Available Laboratory testing is roughly divided into three phases: a pre-analytical phase, an analytical phase and a post-analytical phase. Most analytical errors have been attributed to the analytical phase. However, recent studies have shown that up to 70% of analytical errors reflect the pre-analytical phase. The pre-analytical phase comprises all processes from the time a laboratory request is made by a physician until the specimen is analyzed at the lab. Generally, the pre-analytical phase includes patient preparation, specimen transportation, specimen collection and storage. In the present study, we report the first comprehensive assessment of the frequency and types of pre-analytical errors at the Sulaimani diagnostic labs in Iraqi Kurdistan.Over 2 months, 5500 venous blood samples were observed in 10 public diagnostic labs of Sulaimani City. The percentages of rejected samples and types of sample inappropriateness were evaluated. The percentage of each of the following pre-analytical errors were recorded: delay in sample transportation, clotted samples, expired reagents, hemolyzed samples, samples not on ice, incorrect sample identification, insufficient sample, tube broken in centrifuge, request procedure errors, sample mix-ups, communication conflicts, misinterpreted orders, lipemic samples, contaminated samples and missed physician's request orders. The difference between the relative frequencies of errors observed in the hospitals considered was tested using a proportional Z test. In particular, the survey aimed to discover whether analytical errors were recorded and examine the types of platforms used in the selected diagnostic labs.The analysis showed a high prevalence of improper sample handling during the pre-analytical phase. In appropriate samples, the percentage error was as high as 39%. The major reasons for rejection were hemolyzed samples (9%, incorrect sample identification (8% and clotted samples (6%. Most quality control schemes

Multiple surveys employing a new sample-processing protocol reveal the genetic diversity of placozoans in Japan.

Science.gov (United States)

Miyazawa, Hideyuki; Nakano, Hiroaki

2018-03-01

Placozoans, flat free-living marine invertebrates, possess an extremely simple bauplan lacking neurons and muscle cells and represent one of the earliest-branching metazoan phyla. They are widely distributed from temperate to tropical oceans. Based on mitochondrial 16S rRNA sequences, 19 haplotypes forming seven distinct clades have been reported in placozoans to date. In Japan, placozoans have been found at nine locations, but 16S genotyping has been performed at only two of these locations. Here, we propose a new processing protocol, "ethanol-treated substrate sampling," for collecting placozoans from natural environments. We also report the collection of placozoans from three new locations, the islands of Shikine-jima, Chichi-jima, and Haha-jima, and we present the distribution of the 16S haplotypes of placozoans in Japan. Multiple surveys conducted at multiple locations yielded five haplotypes that were not reported previously, revealing high genetic diversity in Japan, especially at Shimoda and Shikine-jima Island. The observed geographic distribution patterns were different among haplotypes; some were widely distributed, while others were sampled only from a single location. However, samplings conducted on different dates at the same sites yielded different haplotypes, suggesting that placozoans of a given haplotype do not inhabit the same site constantly throughout the year. Continued sampling efforts conducted during all seasons at multiple locations worldwide and the development of molecular markers within the haplotypes are needed to reveal the geographic distribution pattern and dispersal history of placozoans in greater detail.

Report on the second ALMERA network coordination meeting and the ALMERA soil sampling intercomparison exercise IAEA/SIE/01

International Nuclear Information System (INIS)

2006-05-01

The overall aim of the meeting was to evaluate the current status of the ALMERA network laboratories and to help to improve their technical competence through harmonization of sampling, monitoring and measurement protocols and staff training. The meeting was also addressed to defining the structure of the ALMERA network and future proficiency tests and intercomparison trials to be organized by the IAEA to help the laboratories to maintain and improve the quality of their analytical measurements. 45 participants from 29 different institutions attended the meeting

Bayesian adaptive survey protocols for resource management

Science.gov (United States)

Halstead, Brian J.; Wylie, Glenn D.; Coates, Peter S.; Casazza, Michael L.

2011-01-01

Transparency in resource management decisions requires a proper accounting of uncertainty at multiple stages of the decision-making process. As information becomes available, periodic review and updating of resource management protocols reduces uncertainty and improves management decisions. One of the most basic steps to mitigating anthropogenic effects on populations is determining if a population of a species occurs in an area that will be affected by human activity. Species are rarely detected with certainty, however, and falsely declaring a species absent can cause improper conservation decisions or even extirpation of populations. We propose a method to design survey protocols for imperfectly detected species that accounts for multiple sources of uncertainty in the detection process, is capable of quantitatively incorporating expert opinion into the decision-making process, allows periodic updates to the protocol, and permits resource managers to weigh the severity of consequences if the species is falsely declared absent. We developed our method using the giant gartersnake (Thamnophis gigas), a threatened species precinctive to the Central Valley of California, as a case study. Survey date was negatively related to the probability of detecting the giant gartersnake, and water temperature was positively related to the probability of detecting the giant gartersnake at a sampled location. Reporting sampling effort, timing and duration of surveys, and water temperatures would allow resource managers to evaluate the probability that the giant gartersnake occurs at sampled sites where it is not detected. This information would also allow periodic updates and quantitative evaluation of changes to the giant gartersnake survey protocol. Because it naturally allows multiple sources of information and is predicated upon the idea of updating information, Bayesian analysis is well-suited to solving the problem of developing efficient sampling protocols for species of

Multiple analyte adduct formation in liquid chromatography-tandem mass spectrometry - Advantages and limitations in the analysis of biologically-related samples.

Science.gov (United States)

Dziadosz, Marek

2018-05-01

Multiple analyte adduct formation was examined and discussed in the context of reproducible signal detection in liquid chromatography-tandem mass spectrometry applied in the analysis of biologically-related samples. Appropriate infusion solutions were prepared in H 2 O/methanol (3/97, v/v) with 1 mM sodium acetate and 10 mM acetic acid. An API 4000 QTrap tandem mass spectrometer was used for experiments performed in the negative scan mode (-Q1 MS) and the negative enhanced product ion mode (-EPI). γ‑Hydroxybutyrate and its deuterated form were used as model compounds to highlight both the complexity of adduct formation in popular mobile phases used and the effective signal compensation by the application of isotope-labelled analytes as internal standards. Copyright © 2018 Elsevier B.V. All rights reserved.

Ecotoxicity on a stick: A novel analytical tool for predicting the ecotoxicity of petroleum contaminated samples

International Nuclear Information System (INIS)

Parkerton, T.F.; Stone, M.A.

1995-01-01

Hydrocarbons generally elicit toxicity via a nonpolar narcotic mechanism. Recent research suggests that chemicals acting by this mode invoke ecotoxicity when the molar concentration in organisms lipid exceeds a critical threshold. Since ecotoxicity of nonpolar narcotic mixtures appears to be additive, the ecotoxicity of hydrocarbon mixtures thus depends upon: (1) the partitioning of individual hydrocarbons comprising the mixture from the environment to lipids and (2) the total molar sum of the constituent hydrocarbons in lipids. These insights have led previous investigators to advance the concept of biomimetic extraction as a novel tool for assessing potential narcosis-type or baseline ecotoxicity in aqueous samples. Drawing from this earlier work, the authors have developed a method to quantify Bioavailable Petroleum Hydrocarbons (BPHS) in hydrocarbon-contaminated aqueous and soil/sediment samples. A sample is equilibrated with a solid phase microextraction (SPME) fiber that serves as a surrogate for organism lipids. The total moles of hydrocarbons that partition to the SPME fiber is then quantified using a simple GC/FID procedure. Research conducted to support the development and initial validation of this method will be presented. Results suggest that BPH analyses provide a promising, cost-effective approach for predicting the ecotoxicity of environmental samples contaminated with hydrocarbon mixtures. Consequently, BPH analyses may provide a valuable analytical screening tool for ecotoxicity assessment in product and effluent testing, environmental monitoring and site remediation applications

An Energy-Efficient Link Layer Protocol for Reliable Transmission over Wireless Networks

Directory of Open Access Journals (Sweden)

Iqbal Adnan

2009-01-01

Full Text Available In multihop wireless networks, hop-by-hop reliability is generally achieved through positive acknowledgments at the MAC layer. However, positive acknowledgments introduce significant energy inefficiencies on battery-constrained devices. This inefficiency becomes particularly significant on high error rate channels. We propose to reduce the energy consumption during retransmissions using a novel protocol that localizes bit-errors at the MAC layer. The proposed protocol, referred to as Selective Retransmission using Virtual Fragmentation (SRVF, requires simple modifications to the positive-ACK-based reliability mechanism but provides substantial improvements in energy efficiency. The main premise of the protocol is to localize bit-errors by performing partial checksums on disjoint parts or virtual fragments of a packet. In case of error, only the corrupted virtual fragments are retransmitted. We develop stochastic models of the Simple Positive-ACK-based reliability, the previously-proposed Packet Length Optimization (PLO protocol, and the SRVF protocol operating over an arbitrary-order Markov wireless channel. Our analytical models show that SRVF provides significant theoretical improvements in energy efficiency over existing protocols. We then use bit-error traces collected over different real networks to empirically compare the proposed and existing protocols. These experimental results further substantiate that SRVF provides considerably better energy efficiency than Simple Positive-ACK and Packet Length Optimization protocols.

Expressing analytical performance from multi-sample evaluation in laboratory EQA.

Science.gov (United States)

Thelen, Marc H M; Jansen, Rob T P; Weykamp, Cas W; Steigstra, Herman; Meijer, Ron; Cobbaert, Christa M

2017-08-28

To provide its participants with an external quality assessment system (EQAS) that can be used to check trueness, the Dutch EQAS organizer, Organization for Quality Assessment of Laboratory Diagnostics (SKML), has innovated its general chemistry scheme over the last decade by introducing fresh frozen commutable samples whose values were assigned by Joint Committee for Traceability in Laboratory Medicine (JCTLM)-listed reference laboratories using reference methods where possible. Here we present some important innovations in our feedback reports that allow participants to judge whether their trueness and imprecision meet predefined analytical performance specifications. Sigma metrics are used to calculate performance indicators named 'sigma values'. Tolerance intervals are based on both Total Error allowable (TEa) according to biological variation data and state of the art (SA) in line with the European Federation of Clinical Chemistry and Laboratory Medicine (EFLM) Milan consensus. The existing SKML feedback reports that express trueness as the agreement between the regression line through the results of the last 12 months and the values obtained from reference laboratories and calculate imprecision from the residuals of the regression line are now enriched with sigma values calculated from the degree to which the combination of trueness and imprecision are within tolerance limits. The information and its conclusion to a simple two-point scoring system are also graphically represented in addition to the existing difference plot. By adding sigma metrics-based performance evaluation in relation to both TEa and SA tolerance intervals to its EQAS schemes, SKML provides its participants with a powerful and actionable check on accuracy.

Radial line-scans as representative sampling strategy in dried-droplet laser ablation of liquid samples deposited on pre-cut filter paper disks.

Science.gov (United States)

Nischkauer, Winfried; Vanhaecke, Frank; Bernacchi, Sébastien; Herwig, Christoph; Limbeck, Andreas

2014-11-01

Nebulising liquid samples and using the aerosol thus obtained for further analysis is the standard method in many current analytical techniques, also with inductively coupled plasma (ICP)-based devices. With such a set-up, quantification via external calibration is usually straightforward for samples with aqueous or close-to-aqueous matrix composition. However, there is a variety of more complex samples. Such samples can be found in medical, biological, technological and industrial contexts and can range from body fluids, like blood or urine, to fuel additives or fermentation broths. Specialized nebulizer systems or careful digestion and dilution are required to tackle such demanding sample matrices. One alternative approach is to convert the liquid into a dried solid and to use laser ablation for sample introduction. Up to now, this approach required the application of internal standards or matrix-adjusted calibration due to matrix effects. In this contribution, we show a way to circumvent these matrix effects while using simple external calibration for quantification. The principle of representative sampling that we propose uses radial line-scans across the dried residue. This compensates for centro-symmetric inhomogeneities typically observed in dried spots. The effectiveness of the proposed sampling strategy is exemplified via the determination of phosphorus in biochemical fermentation media. However, the universal viability of the presented measurement protocol is postulated. Detection limits using laser ablation-ICP-optical emission spectrometry were in the order of 40 μg mL - 1 with a reproducibility of 10 % relative standard deviation (n = 4, concentration = 10 times the quantification limit). The reported sensitivity is fit-for-purpose in the biochemical context described here, but could be improved using ICP-mass spectrometry, if future analytical tasks would require it. Trueness of the proposed method was investigated by cross-validation with

Radial line-scans as representative sampling strategy in dried-droplet laser ablation of liquid samples deposited on pre-cut filter paper disks

Science.gov (United States)

Nischkauer, Winfried; Vanhaecke, Frank; Bernacchi, Sébastien; Herwig, Christoph; Limbeck, Andreas

2014-11-01

Nebulising liquid samples and using the aerosol thus obtained for further analysis is the standard method in many current analytical techniques, also with inductively coupled plasma (ICP)-based devices. With such a set-up, quantification via external calibration is usually straightforward for samples with aqueous or close-to-aqueous matrix composition. However, there is a variety of more complex samples. Such samples can be found in medical, biological, technological and industrial contexts and can range from body fluids, like blood or urine, to fuel additives or fermentation broths. Specialized nebulizer systems or careful digestion and dilution are required to tackle such demanding sample matrices. One alternative approach is to convert the liquid into a dried solid and to use laser ablation for sample introduction. Up to now, this approach required the application of internal standards or matrix-adjusted calibration due to matrix effects. In this contribution, we show a way to circumvent these matrix effects while using simple external calibration for quantification. The principle of representative sampling that we propose uses radial line-scans across the dried residue. This compensates for centro-symmetric inhomogeneities typically observed in dried spots. The effectiveness of the proposed sampling strategy is exemplified via the determination of phosphorus in biochemical fermentation media. However, the universal viability of the presented measurement protocol is postulated. Detection limits using laser ablation-ICP-optical emission spectrometry were in the order of 40 μg mL- 1 with a reproducibility of 10 % relative standard deviation (n = 4, concentration = 10 times the quantification limit). The reported sensitivity is fit-for-purpose in the biochemical context described here, but could be improved using ICP-mass spectrometry, if future analytical tasks would require it. Trueness of the proposed method was investigated by cross-validation with

Experimental Protocol to Determine the Chloride Threshold Value for Corrosion in Samples Taken from Reinforced Concrete Structures.

Science.gov (United States)

Angst, Ueli M; Boschmann, Carolina; Wagner, Matthias; Elsener, Bernhard

2017-08-31

The aging of reinforced concrete infrastructure in developed countries imposes an urgent need for methods to reliably assess the condition of these structures. Corrosion of the embedded reinforcing steel is the most frequent cause for degradation. While it is well known that the ability of a structure to withstand corrosion depends strongly on factors such as the materials used or the age, it is common practice to rely on threshold values stipulated in standards or textbooks. These threshold values for corrosion initiation (Ccrit) are independent of the actual properties of a certain structure, which clearly limits the accuracy of condition assessments and service life predictions. The practice of using tabulated values can be traced to the lack of reliable methods to determine Ccrit on-site and in the laboratory. Here, an experimental protocol to determine Ccrit for individual engineering structures or structural members is presented. A number of reinforced concrete samples are taken from structures and laboratory corrosion testing is performed. The main advantage of this method is that it ensures real conditions concerning parameters that are well known to greatly influence Ccrit, such as the steel-concrete interface, which cannot be representatively mimicked in laboratory-produced samples. At the same time, the accelerated corrosion test in the laboratory permits the reliable determination of Ccrit prior to corrosion initiation on the tested structure; this is a major advantage over all common condition assessment methods that only permit estimating the conditions for corrosion after initiation, i.e., when the structure is already damaged. The protocol yields the statistical distribution of Ccrit for the tested structure. This serves as a basis for probabilistic prediction models for the remaining time to corrosion, which is needed for maintenance planning. This method can potentially be used in material testing of civil infrastructures, similar to established

Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

Science.gov (United States)

Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

2017-11-24

Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

An overview of the analytical methods for the determination of organic ultraviolet filters in biological fluids and tissues

Energy Technology Data Exchange (ETDEWEB)

Chisvert, Alberto, E-mail: alberto.chisvert@uv.es [Departamento de Quimica Analitica, Facultad de Quimica, Universitat de Valencia, Doctor Moliner St. 50, 46100 Burjassot, Valencia (Spain); Leon-Gonzalez, Zacarias [Unidad Analitica, Instituto de Investigacion Sanitaria Fundacion Hospital La Fe, 46009 Valencia (Spain); Tarazona, Isuha; Salvador, Amparo [Departamento de Quimica Analitica, Facultad de Quimica, Universitat de Valencia, Doctor Moliner St. 50, 46100 Burjassot, Valencia (Spain); Giokas, Dimosthenis [Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina (Greece)

2012-11-08

Highlights: Black-Right-Pointing-Pointer Papers describing the determination of UV filters in fluids and tissues are reviewed. Black-Right-Pointing-Pointer Matrix complexity and low amounts of analytes require effective sample treatments. Black-Right-Pointing-Pointer The published papers do not cover the study of all the substances allowed as UV filters. Black-Right-Pointing-Pointer New analytical methods for UV filters determination in these matrices are encouraged. - Abstract: Organic UV filters are chemical compounds added to cosmetic sunscreen products in order to protect users from UV solar radiation. The need of broad-spectrum protection to avoid the deleterious effects of solar radiation has triggered a trend in the cosmetic market of including these compounds not only in those exclusively designed for sun protection but also in all types of cosmetic products. Different studies have shown that organic UV filters can be absorbed through the skin after topical application, further metabolized in the body and eventually excreted or bioaccumulated. These percutaneous absorption processes may result in various adverse health effects, such as genotoxicity caused by the generation of free radicals, which can even lead to mutagenic or carcinogenic effects, and estrogenicity, which is associated with the endocrine disruption activity caused by some of these compounds. Due to the absence of official monitoring protocols, there is a demand for analytical methods that enable the determination of UV filters in biological fluids and tissues in order to retrieve more information regarding their behavior in the human body and thus encourage the development of safer cosmetic formulations. In view of this demand, there has recently been a noticeable increase in the development of sensitive and selective analytical methods for the determination of UV filters and their metabolites in biological fluids (i.e., urine, plasma, breast milk and semen) and tissues. The complexity of

An overview of the analytical methods for the determination of organic ultraviolet filters in biological fluids and tissues

International Nuclear Information System (INIS)

Chisvert, Alberto; León-González, Zacarías; Tarazona, Isuha; Salvador, Amparo; Giokas, Dimosthenis

2012-01-01

Highlights: ► Papers describing the determination of UV filters in fluids and tissues are reviewed. ► Matrix complexity and low amounts of analytes require effective sample treatments. ► The published papers do not cover the study of all the substances allowed as UV filters. ► New analytical methods for UV filters determination in these matrices are encouraged. - Abstract: Organic UV filters are chemical compounds added to cosmetic sunscreen products in order to protect users from UV solar radiation. The need of broad-spectrum protection to avoid the deleterious effects of solar radiation has triggered a trend in the cosmetic market of including these compounds not only in those exclusively designed for sun protection but also in all types of cosmetic products. Different studies have shown that organic UV filters can be absorbed through the skin after topical application, further metabolized in the body and eventually excreted or bioaccumulated. These percutaneous absorption processes may result in various adverse health effects, such as genotoxicity caused by the generation of free radicals, which can even lead to mutagenic or carcinogenic effects, and estrogenicity, which is associated with the endocrine disruption activity caused by some of these compounds. Due to the absence of official monitoring protocols, there is a demand for analytical methods that enable the determination of UV filters in biological fluids and tissues in order to retrieve more information regarding their behavior in the human body and thus encourage the development of safer cosmetic formulations. In view of this demand, there has recently been a noticeable increase in the development of sensitive and selective analytical methods for the determination of UV filters and their metabolites in biological fluids (i.e., urine, plasma, breast milk and semen) and tissues. The complexity of the biological matrix and the low concentration levels of these compounds inevitably impose sample

Using semantics for representing experimental protocols.

Science.gov (United States)

Giraldo, Olga; García, Alexander; López, Federico; Corcho, Oscar

2017-11-13

An experimental protocol is a sequence of tasks and operations executed to perform experimental research in biological and biomedical areas, e.g. biology, genetics, immunology, neurosciences, virology. Protocols often include references to equipment, reagents, descriptions of critical steps, troubleshooting and tips, as well as any other information that researchers deem important for facilitating the reusability of the protocol. Although experimental protocols are central to reproducibility, the descriptions are often cursory. There is the need for a unified framework with respect to the syntactic structure and the semantics for representing experimental protocols. In this paper we present "SMART Protocols ontology", an ontology for representing experimental protocols. Our ontology represents the protocol as a workflow with domain specific knowledge embedded within a document. We also present the S ample I nstrument R eagent O bjective (SIRO) model, which represents the minimal common information shared across experimental protocols. SIRO was conceived in the same realm as the Patient Intervention Comparison Outcome (PICO) model that supports search, retrieval and classification purposes in evidence based medicine. We evaluate our approach against a set of competency questions modeled as SPARQL queries and processed against a set of published and unpublished protocols modeled with the SP Ontology and the SIRO model. Our approach makes it possible to answer queries such as Which protocols use tumor tissue as a sample. Improving reporting structures for experimental protocols requires collective efforts from authors, peer reviewers, editors and funding bodies. The SP Ontology is a contribution towards this goal. We build upon previous experiences and bringing together the view of researchers managing protocols in their laboratory work. Website: https://smartprotocols.github.io/ .

The Integration of a Small Thermal Desorption (TD) System for Air Monitoring into a Mobile Analytical Laboratory in France Used by the NRBC Emergency First Responder Police Organization

International Nuclear Information System (INIS)

Roberts, G. M.

2007-01-01

A mobile analytical laboratory has been developed in France by Thales Security Systems in conjunction with the French department of defense (DGA) to rapidly identify the composition of toxic substances released accidentally or by terrorist activity at a location of high civilian population density. Accurate and fast identification of toxic material is critical for first responder teams that attend an incident site. Based on this analysis defined decontamination protocols for contaminated people can be implemented, and specific medical treatment can be administered to those worst affected. Analysing samples with high technology instrumentation close to the point of release is therefore highly advantageous and is only possible with mobile analytical platforms. Transporting samples back to a central laboratory for analysis is not realistic due to time limitations. This paper looks at one particular aspect of analysis performed in this mobile multi-technique laboratory namely air monitoring for CW or TIC compounds. Air sampling and pre concentration is achieved using a small, innovative Thermal Desorption system (Unitytm) in combination with a gas chromatograph-mass spectroscopy system for the detection and identification of specific analytes. Implementation of the Unity TD system in the confines of this small mobile environment will be reviewed in this paper. (author)

Future analytical provision - Relocation of Sellafield Ltd Analytical Services Laboratory

International Nuclear Information System (INIS)

Newell, B.

2015-01-01

Sellafield Ltd Analytical Services provide an essential view on the environmental, safety, process and high hazard risk reduction performances by analysis of samples. It is the largest and most complex analytical services laboratory in Europe, with 150 laboratories (55 operational) and 350 staff (including 180 analysts). Sellafield Ltd Analytical Services Main Laboratory is in need of replacement. This is due to the age of the facility and changes to work streams. This relocation is an opportunity to -) design and commission bespoke MA (Medium-Active) cells, -) modify HA (High-Active) cell design to facilitate an in-cell laboratory, -) develop non-destructive techniques, -) open light building for better worker morale. The option chosen was to move the activities to the NNL Central laboratory (NNLCL) that is based at Sellafield and is the UK's flagship nuclear research and development facility. This poster gives a time schedule

Strategies for Distinguishing Abiotic Chemistry from Martian Biochemistry in Samples Returned from Mars

Science.gov (United States)

Glavin, D. P.; Burton, A. S.; Callahan, M. P.; Elsila, J. E.; Stern, J. C.; Dworkin, J. P.

2012-01-01

A key goal in the search for evidence of extinct or extant life on Mars will be the identification of chemical biosignatures including complex organic molecules common to all life on Earth. These include amino acids, the monomer building blocks of proteins and enzymes, and nucleobases, which serve as the structural basis of information storage in DNA and RNA. However, many of these organic compounds can also be formed abiotically as demonstrated by their prevalence in carbonaceous meteorites [1]. Therefore, an important challenge in the search for evidence of life on Mars will be distinguishing between abiotic chemistry of either meteoritic or martian origin from any chemical biosignatures from an extinct or extant martian biota. Although current robotic missions to Mars, including the 2011 Mars Science Laboratory (MSL) and the planned 2018 ExoMars rovers, will have the analytical capability needed to identify these key classes of organic molecules if present [2,3], return of a diverse suite of martian samples to Earth would allow for much more intensive laboratory studies using a broad array of extraction protocols and state-of-theart analytical techniques for bulk and spatially resolved characterization, molecular detection, and isotopic and enantiomeric compositions that may be required for unambiguous confirmation of martian life. Here we will describe current state-of-the-art laboratory analytical techniques that have been used to characterize the abundance and distribution of amino acids and nucleobases in meteorites, Apollo samples, and comet- exposed materials returned by the Stardust mission with an emphasis on their molecular characteristics that can be used to distinguish abiotic chemistry from biochemistry as we know it. The study of organic compounds in carbonaceous meteorites is highly relevant to Mars sample return analysis, since exogenous organic matter should have accumulated in the martian regolith over the last several billion years and the

An efficient multi-carrier position-based packet forwarding protocol for wireless sensor networks

KAUST Repository

Bader, Ahmed

2012-01-01

Beaconless position-based forwarding protocols have recently evolved as a promising solution for packet forwarding in wireless sensor networks. However, as the node density grows, the overhead incurred in the process of relay selection grows significantly. As such, end-to-end performance in terms of energy and latency is adversely impacted. With the motivation of developing a packet forwarding mechanism that is tolerant to variation in node density, an alternative position-based protocol is proposed in this paper. In contrast to existing beaconless protocols, the proposed protocol is designed such that it eliminates the need for potential relays to undergo a relay selection process. Rather, any eligible relay may decide to forward the packet ahead, thus significantly reducing the underlying overhead. The operation of the proposed protocol is empowered by exploiting favorable features of orthogonal frequency division multiplexing (OFDM) at the physical layer. The end-to-end performance of the proposed protocol is evaluated against existing beaconless position-based protocols analytically and as well by means of simulations. The proposed protocol is demonstrated in this paper to be more efficient. In particular, it is shown that for the same amount of energy the proposed protocol transports one bit from source to destination much quicker. © 2012 IEEE.

Determination of 93Zr, 107Pd and 135Cs in zircaloy hulls analytical development on inactive samples

International Nuclear Information System (INIS)

Excoffier, E.; Bienvenu, Ph.; Combes, C.; Pontremoli, S.; Delteil, N.; Ferrini, R.

2000-01-01

A study involving the participation of three laboratories of the Direction of the Fuel Cycle has been undertaken within the framework of a common interest program existing between the COGEMA and the CEA. Its purpose is to develop analytical methods for the determination of long-lived radionuclides in zircaloy hulls coming from spent fuel reprocessing operations. Acting as a complement to work carried out at the DRRV in ATALANTE concerning zircaloy dissolution and direct analysis of hull solutions, a study is now being conducted at the DESD/SCCD/LARC in Cadarache on three of these radionuclides, namely: zirconium 93, palladium 107 and caesium 135. It concerns three radioisotopes having very long periods (∼10 6 y), and which stabilize mainly through emission of β particles. The analytical technique chosen for the final measurement is inductively coupled plasma mass spectrometry (ICP/MS). Prior to the measurement, chemical separation processes are used to extract the radionuclides from the matrix and separate them from interfering elements and β emitters. The method developed initially on inactive solutions is being validated on irradiated samples coming from UP2/800 - UP3 reprocessing plants. (authors)

Demonstration Exercise of a Validated Sample Collection Method for Powders Suspected of Being Biological Agents in Georgia 2006

International Nuclear Information System (INIS)

Marsh, B.

2007-01-01

August 7, 2006 the state of Georgia conducted a collaborative sampling exercise between the Georgia National Guard 4th Civil Support Team Weapons of Mass Destruction (CST-WMD) and the Georgia Department of Human Resources Division of Public Health demonstrating a recently validated bulk powder sampling method. The exercise was hosted at the Federal Law Enforcement Training Center (FLETC) at Glynn County, Georgia and involved the participation of the Georgia Emergency Management Agency (GEMA), Georgia National Guard, Georgia Public Health Laboratories, the Federal Bureau of Investigation Atlanta Office, Georgia Coastal Health District, and the Glynn County Fire Department. The purpose of the exercise was to demonstrate a recently validated national sampling standard developed by the American Standards and Test Measures (ASTM) International; ASTM E2458 S tandard Practice for Bulk Sample Collection and Swab Sample Collection of Visible Powders Suspected of Being Biological Agents from Nonporous Surfaces . The intent of the exercise was not to endorse the sampling method, but to develop a model for exercising new sampling methods in the context of existing standard operating procedures (SOPs) while strengthening operational relationships between response teams and analytical laboratories. The exercise required a sampling team to respond real-time to an incident cross state involving a clandestine bio-terrorism production lab found within a recreational vehicle (RV). Sample targets consisted of non-viable gamma irradiated B. anthracis Sterne spores prepared by Dugway Proving Ground. Various spore concentration levels were collected by the ASTM method, followed by on- and off-scene analysis utilizing the Center for Disease Control (CDC) Laboratory Response Network (LRN) and National Guard Bureau (NGB) CST mobile Analytical Laboratory Suite (ALS) protocols. Analytical results were compared and detailed surveys of participant evaluation comments were examined. I will

8. All Polish Conference on Analytical Chemistry: Analytical Chemistry for the Community of the 21. Century

International Nuclear Information System (INIS)

Koscielniak, P.; Wieczorek, M.; Kozak, J.

2010-01-01

Book of Abstracts contains short descriptions of lectures, communications and posters presented during 8 th All Polish Conference on Analytical Chemistry (Cracow, 4-9.07.2010). Scientific programme consisted of: basic analytical problems, preparation of the samples, chemometry and metrology, miniaturization of the analytical procedures, environmental analysis, medicinal analyses, industrial analyses, food analyses, biochemical analyses, analysis of relicts of the past. Several posters were devoted to the radiochemical separations, radiochemical analysis, environmental behaviour of the elements important for the nuclear science and the professional tests.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

Science.gov (United States)

Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

1997-01-01

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Metabolism of the synthetic cannabinoid 5F-PY-PICA by human and rat hepatocytes and identification of biliary analytical targets by directional efflux in sandwich-cultured rat hepatocytes using UHPLC-HR-MS/MS

DEFF Research Database (Denmark)

Mardal, Marie; Annaert, Pieter; Noble, Carolina

2018-01-01

Analytical strategies for detecting drugs in biological samples rely on information on metabolism and elimination. 5F-PY-PICA belongs to the group of synthetic cannabinoids that are known to undergo excretion into the bile. The aims of this study were the in vitro identification of metabolites of 5......F-PY-PICA and to determine which analytical targets are excreted into the bile and urine. Metabolites identified after incubation of 5F-PY-PICA with pooled human liver microsomes (pHLM), pooled human hepatocytes (pHH), or suspended and sandwich-cultured rat hepatocytes (SCRH). Rat hepatocytes were......-PY-PICA, M4, and M22 are proposed as analytical targets for bile analysis in forensic screening protocols, whereas M6 should be one of the main urinary targets for 5F-PY-PICA analysis....

Verbal protocols as methodological resources: research evidence

Directory of Open Access Journals (Sweden)

Alessandra Baldo

2012-01-01

Full Text Available This article aims at reflecting on the use of verbal protocols as a methodological resource in qualitative research, more specifically on the aspect regarded as the main limitation of a study about lexical inferencing in L2 (BALDO; VELASQUES, 2010: its subjective trait. The article begins with a brief literature review on protocols, followed by a description of the study in which they were employed as methodological resources. Based on that, protocol subjectivity is illustrated through samples of unparalleled data classification, carried out independently by two researchers. In the final section, the path followed to minimize the problem is presented, intending to contribute to improve efficiency in the use of verbal protocols in future research.

Automation of analytical systems in power cycles

International Nuclear Information System (INIS)

Staub Lukas

2008-01-01

'Automation' is a widely used term in instrumentation and is often applied to signal exchange, PLC and SCADA systems. Common use, however, does not necessarily described autonomous operation of analytical devices. We define an automated analytical system as a black box with an input (sample) and an output (measured value). In addition we need dedicated status lines for assessing the validities of the input for our black box and the output for subsequent systems. We will discuss input parameters, automated analytical processes and output parameters. Further considerations will be given to signal exchange and integration into the operating routine of a power plant. Local control loops (chemical dosing) and the automation of sampling systems are not discussed here. (author)

An ultra low-power and traffic-adaptive medium access control protocol for wireless body area network.

Science.gov (United States)

Ullah, Sana; Kwak, Kyung Sup

2012-06-01

Wireless Body Area Network (WBAN) consists of low-power, miniaturized, and autonomous wireless sensor nodes that enable physicians to remotely monitor vital signs of patients and provide real-time feedback with medical diagnosis and consultations. It is the most reliable and cheaper way to take care of patients suffering from chronic diseases such as asthma, diabetes and cardiovascular diseases. Some of the most important attributes of WBAN is low-power consumption and delay. This can be achieved by introducing flexible duty cycling techniques on the energy constraint sensor nodes. Stated otherwise, low duty cycle nodes should not receive frequent synchronization and control packets if they have no data to send/receive. In this paper, we introduce a Traffic-adaptive MAC protocol (TaMAC) by taking into account the traffic information of the sensor nodes. The protocol dynamically adjusts the duty cycle of the sensor nodes according to their traffic-patterns, thus solving the idle listening and overhearing problems. The traffic-patterns of all sensor nodes are organized and maintained by the coordinator. The TaMAC protocol is supported by a wakeup radio that is used to accommodate emergency and on-demand events in a reliable manner. The wakeup radio uses a separate control channel along with the data channel and therefore it has considerably low power consumption requirements. Analytical expressions are derived to analyze and compare the performance of the TaMAC protocol with the well-known beacon-enabled IEEE 802.15.4 MAC, WiseMAC, and SMAC protocols. The analytical derivations are further validated by simulation results. It is shown that the TaMAC protocol outperforms all other protocols in terms of power consumption and delay.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

Directory of Open Access Journals (Sweden)

Ewa Jaszczak

2017-01-01

Full Text Available A simple and accurate ion chromatography (IC method with pulsed amperometric detection (PAD was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R>0.992. Low detection limits (LODs in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n=3 were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection.

Science.gov (United States)

Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100  μ g/L for urine, 5-100  μ g/L for saliva, and 3-100  μ g/L for sweat samples with determination coefficients ( R ) > 0.992. Low detection limits (LODs) in the range of 1.8  μ g/L, 5.1  μ g/L, and 5.8  μ g/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

Analysis of IFR samples at ANL-E

International Nuclear Information System (INIS)

Bowers, D.L.; Sabau, C.S.

1993-01-01

The Analytical Chemistry Laboratory analyzes a variety of samples submitted by the different research groups within IFR. This talk describes the analytical work on samples generated by the Plutonium Electrorefiner, Large Scale Electrorefiner and Waste Treatment Studies. The majority of these samples contain Transuranics and necessitate facilities that safely contain these radioisotopes. Details such as: sample receiving, dissolution techniques, chemical separations, Instrumentation used, reporting of results are discussed. The Importance of Interactions between customer and analytical personnel Is also demonstrated

Sample handling for mass spectrometric proteomic investigations of human urine.

Science.gov (United States)

Petri, Anette Lykke; Høgdall, Claus; Christensen, Ib Jarle; Simonsen, Anja Hviid; T'jampens, Davy; Hellmann, Marja-Leena; Kjaer, Susanne Krüger; Fung, Eric T; Høgdall, Estrid

2008-09-01

Because of its non-invasive sample collection method, human urine is an attractive biological material both for discovering biomarkers and for use in future screening trials for different diseases. Before urine can be used for these applications, standardized protocols for sample handling that optimize protein stability are required. In this explorative study, we examine the influence of different urine collection methods, storage temperatures, storage times, and repetitive freeze-thaw procedures on the protein profiles obtained by surface-enhanced laser desorption/ionization time-of-flight mass spectrometry (SELDI-TOF-MS). Prospectively collected urine samples from 11 women were collected as either morning or midday specimens. The effects of storage temperature, time to freezing, and freeze-thaw cycles were assessed by calculating the number, intensity, and reproducibility of peaks visualized by SELDI-TOF-MS. On the CM10 array, 122 peaks were detected and 28 peaks were found to be significantly different between urine types, storage temperature and time to freezing. On the IMAC-Cu array, 65 peaks were detected and 1 peak was found to be significantly different according to time to freezing. No significant differences were demonstrated for freeze-thaw cycles. Optimal handling and storage conditions are necessary in clinical urine proteomic investigations. Collection of urine with a single and consistently performed protocol is needed to reduce analytical bias. Collecting only one urine type, which is stored for a limited period at 4°C until freezing at -80°C prior to analysis will provide the most stable profiles. Copyright © 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Technical Note: Comparison of storage strategies of sea surface microlayer samples

Directory of Open Access Journals (Sweden)

K. Schneider-Zapp

2013-07-01

Full Text Available The sea surface microlayer (SML is an important biogeochemical system whose physico-chemical analysis often necessitates some degree of sample storage. However, many SML components degrade with time so the development of optimal storage protocols is paramount. We here briefly review some commonly used treatment and storage protocols. Using freshwater and saline SML samples from a river estuary, we investigated temporal changes in surfactant activity (SA and the absorbance and fluorescence of chromophoric dissolved organic matter (CDOM over four weeks, following selected sample treatment and storage protocols. Some variability in the effectiveness of individual protocols most likely reflects sample provenance. None of the various protocols examined performed any better than dark storage at 4 °C without pre-treatment. We therefore recommend storing samples refrigerated in the dark.

Road Transportable Analytical Laboratory system

International Nuclear Information System (INIS)

Finger, S.M.; Keith, V.F.; Spertzel, R.O.; De Avila, J.C.; O'Donnell, M.; Vann, R.L.

1993-09-01

This developmental effort clearly shows that a Road Transportable Analytical Laboratory System is a worthwhile and achievable goal. The RTAL is designed to fully analyze (radioanalytes, and organic and inorganic chemical analytes) 20 samples per day at the highest levels of quality assurance and quality control. It dramatically reduces the turnaround time for environmental sample analysis from 45 days (at a central commercial laboratory) to 1 day. At the same time each RTAL system will save the DOE over $12 million per year in sample analysis costs compared to the costs at a central commercial laboratory. If RTAL systems were used at the eight largest DOE facilities (at Hanford, Savannah River, Fernald, Oak Ridge, Idaho, Rocky Flats, Los Alamos, and the Nevada Test Site), the annual savings would be $96,589,000. The DOE's internal study of sample analysis needs projects 130,000 environmental samples requiring analysis in FY 1994, clearly supporting the need for the RTAL system. The cost and time savings achievable with the RTAL system will accelerate and improve the efficiency of cleanup and remediation operations throughout the DOE complex

Sample preparation guidelines for two-dimensional electrophoresis.

Science.gov (United States)

Posch, Anton

2014-12-01

Sample preparation is one of the key technologies for successful two-dimensional electrophoresis (2DE). Due to the great diversity of protein sample types and sources, no single sample preparation method works with all proteins; for any sample the optimum procedure must be determined empirically. This review is meant to provide a broad overview of the most important principles in sample preparation in order to avoid a multitude of possible pitfalls. Sample preparation protocols from the expert in the field were screened and evaluated. On the basis of these protocols and my own comprehensive practical experience important guidelines are given in this review. The presented guidelines will facilitate straightforward protocol development for researchers new to gel-based proteomics. In addition the available choices are rationalized in order to successfully prepare a protein sample for 2DE separations. The strategies described here are not limited to 2DE and can also be applied to other protein separation techniques.

Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

Science.gov (United States)

Boyacı, Ezel; Pawliszyn, Janusz

2014-09-16

Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

International Congress on Analytical Chemistry. Abstracts. V. 1

International Nuclear Information System (INIS)

1997-01-01

The collection of materials of the international congress on analytical chemistry taken place in Moscow in June 1997. The main directs of investigations in such regions of analytical chemistry as quantitative and qualitative analysis, microanalysis, sample preparation and preconcentration, analytical reagents, chromatography and related techniques, flow analysis, electroanalytical and kinetic methods sensors are elucidated

Protocol voor meting van lachgasemissie uit huisvestingssystemen in de veehouderij 2010 = Measurement protocol for nitrous oxide emission from housing systems in livestock production 2010

NARCIS (Netherlands)

Mosquera Losada, J.; Groenestein, C.M.; Ogink, N.W.M.

2011-01-01

This report describes a measurement protocol for nitrous oxide emissions from animal housing systems. The protocol is based on sampling periods of 24 hours spread over one year and can be applied in specified animal categories.

Radial line-scans as representative sampling strategy in dried-droplet laser ablation of liquid samples deposited on pre-cut filter paper disks

Energy Technology Data Exchange (ETDEWEB)

Nischkauer, Winfried [Institute of Chemical Technologies and Analytics, Vienna University of Technology, Vienna (Austria); Department of Analytical Chemistry, Ghent University, Ghent (Belgium); Vanhaecke, Frank [Department of Analytical Chemistry, Ghent University, Ghent (Belgium); Bernacchi, Sébastien; Herwig, Christoph [Institute of Chemical Engineering, Vienna University of Technology, Vienna (Austria); Limbeck, Andreas, E-mail: Andreas.Limbeck@tuwien.ac.at [Institute of Chemical Technologies and Analytics, Vienna University of Technology, Vienna (Austria)

2014-11-01

Nebulising liquid samples and using the aerosol thus obtained for further analysis is the standard method in many current analytical techniques, also with inductively coupled plasma (ICP)-based devices. With such a set-up, quantification via external calibration is usually straightforward for samples with aqueous or close-to-aqueous matrix composition. However, there is a variety of more complex samples. Such samples can be found in medical, biological, technological and industrial contexts and can range from body fluids, like blood or urine, to fuel additives or fermentation broths. Specialized nebulizer systems or careful digestion and dilution are required to tackle such demanding sample matrices. One alternative approach is to convert the liquid into a dried solid and to use laser ablation for sample introduction. Up to now, this approach required the application of internal standards or matrix-adjusted calibration due to matrix effects. In this contribution, we show a way to circumvent these matrix effects while using simple external calibration for quantification. The principle of representative sampling that we propose uses radial line-scans across the dried residue. This compensates for centro-symmetric inhomogeneities typically observed in dried spots. The effectiveness of the proposed sampling strategy is exemplified via the determination of phosphorus in biochemical fermentation media. However, the universal viability of the presented measurement protocol is postulated. Detection limits using laser ablation-ICP-optical emission spectrometry were in the order of 40 μg mL{sup −1} with a reproducibility of 10 % relative standard deviation (n = 4, concentration = 10 times the quantification limit). The reported sensitivity is fit-for-purpose in the biochemical context described here, but could be improved using ICP-mass spectrometry, if future analytical tasks would require it. Trueness of the proposed method was investigated by cross-validation with

A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

Science.gov (United States)

Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

2015-05-01

The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

Automated processing of whole blood samples for the determination of immunosuppressants by liquid chromatography tandem-mass spectrometry.

Science.gov (United States)

Vogeser, Michael; Spöhrer, Ute

2006-01-01

Liquid chromatography tandem-mass spectrometry (LC-MS/MS) is an efficient technology for routine determination of immunosuppressants in whole blood; however, time-consuming manual sample preparation remains a significant limitation of this technique. Using a commercially available robotic pipetting system (Tecan Freedom EVO), we developed an automated sample-preparation protocol for quantification of tacrolimus in whole blood by LC-MS/MS. Barcode reading, sample resuspension, transfer of whole blood aliquots into a deep-well plate, addition of internal standard solution, mixing, and protein precipitation by addition of an organic solvent is performed by the robotic system. After centrifugation of the plate, the deproteinized supernatants are submitted to on-line solid phase extraction, using column switching prior to LC-MS/MS analysis. The only manual actions within the entire process are decapping of the tubes, and transfer of the deep-well plate from the robotic system to a centrifuge and finally to the HPLC autosampler. Whole blood pools were used to assess the reproducibility of the entire analytical system for measuring tacrolimus concentrations. A total coefficient of variation of 1.7% was found for the entire automated analytical process (n=40; mean tacrolimus concentration, 5.3 microg/L). Close agreement between tacrolimus results obtained after manual and automated sample preparation was observed. The analytical system described here, comprising automated protein precipitation, on-line solid phase extraction and LC-MS/MS analysis, is convenient and precise, and minimizes hands-on time and the risk of mistakes in the quantification of whole blood immunosuppressant concentrations compared to conventional methods.

The combination of four analytical methods to explore skeletal muscle metabolomics: Better coverage of metabolic pathways or a marketing argument?

Science.gov (United States)

Bruno, C; Patin, F; Bocca, C; Nadal-Desbarats, L; Bonnier, F; Reynier, P; Emond, P; Vourc'h, P; Joseph-Delafont, K; Corcia, P; Andres, C R; Blasco, H

2018-01-30

Metabolomics is an emerging science based on diverse high throughput methods that are rapidly evolving to improve metabolic coverage of biological fluids and tissues. Technical progress has led researchers to combine several analytical methods without reporting the impact on metabolic coverage of such a strategy. The objective of our study was to develop and validate several analytical techniques (mass spectrometry coupled to gas or liquid chromatography and nuclear magnetic resonance) for the metabolomic analysis of small muscle samples and evaluate the impact of combining methods for more exhaustive metabolite covering. We evaluated the muscle metabolome from the same pool of mouse muscle samples after 2 metabolite extraction protocols. Four analytical methods were used: targeted flow injection analysis coupled with mass spectrometry (FIA-MS/MS), gas chromatography coupled with mass spectrometry (GC-MS), liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS), and nuclear magnetic resonance (NMR) analysis. We evaluated the global variability of each compound i.e., analytical (from quality controls) and extraction variability (from muscle extracts). We determined the best extraction method and we reported the common and distinct metabolites identified based on the number and identity of the compounds detected with low analytical variability (variation coefficient<30%) for each method. Finally, we assessed the coverage of muscle metabolic pathways obtained. Methanol/chloroform/water and water/methanol were the best extraction solvent for muscle metabolome analysis by NMR and MS, respectively. We identified 38 metabolites by nuclear magnetic resonance, 37 by FIA-MS/MS, 18 by GC-MS, and 80 by LC-HRMS. The combination led us to identify a total of 132 metabolites with low variability partitioned into 58 metabolic pathways, such as amino acid, nitrogen, purine, and pyrimidine metabolism, and the citric acid cycle. This combination also showed

Parameter sampling capabilities of sequential and simultaneous data assimilation: I. Analytical comparison

International Nuclear Information System (INIS)

Fossum, Kristian; Mannseth, Trond

2014-01-01

We assess the parameter sampling capabilities of some Bayesian, ensemble-based, joint state-parameter (JS) estimation methods. The forward model is assumed to be non-chaotic and have nonlinear components, and the emphasis is on results obtained for the parameters in the state-parameter vector. A variety of approximate sampling methods exist, and a number of numerical comparisons between such methods have been performed. Often, more than one of the defining characteristics vary from one method to another, so it can be difficult to point out which characteristic of the more successful method in such a comparison was decisive. In this study, we single out one defining characteristic for comparison; whether or not data are assimilated sequentially or simultaneously. The current paper is concerned with analytical investigations into this issue. We carefully select one sequential and one simultaneous JS method for the comparison. We also design a corresponding pair of pure parameter estimation methods, and we show how the JS methods and the parameter estimation methods are pairwise related. It is shown that the sequential and the simultaneous parameter estimation methods are equivalent for one particular combination of observations with different degrees of nonlinearity. Strong indications are presented for why one may expect the sequential parameter estimation method to outperform the simultaneous parameter estimation method for all other combinations of observations. Finally, the conditions for when similar relations can be expected to hold between the corresponding JS methods are discussed. A companion paper, part II (Fossum and Mannseth 2014 Inverse Problems 30 114003), is concerned with statistical analysis of results from a range of numerical experiments involving sequential and simultaneous JS estimation, where the design of the numerical investigation is motivated by our findings in the current paper. (paper)

SPECT/CT workflow and imaging protocols

Energy Technology Data Exchange (ETDEWEB)

Beckers, Catherine [University Hospital of Liege, Division of Nuclear Medicine and Oncological Imaging, Department of Medical Physics, Liege (Belgium); Hustinx, Roland [University Hospital of Liege, Division of Nuclear Medicine and Oncological Imaging, Department of Medical Physics, Liege (Belgium); Domaine Universitaire du Sart Tilman, Service de Medecine Nucleaire et Imagerie Oncologique, CHU de Liege, Liege (Belgium)

2014-05-15

Introducing a hybrid imaging method such as single photon emission computed tomography (SPECT)/CT greatly alters the routine in the nuclear medicine department. It requires designing new workflow processes and the revision of original scheduling process and imaging protocols. In addition, the imaging protocol should be adapted for each individual patient, so that performing CT is fully justified and the CT procedure is fully tailored to address the clinical issue. Such refinements often occur before the procedure is started but may be required at some intermediate stage of the procedure. Furthermore, SPECT/CT leads in many instances to a new partnership with the radiology department. This article presents practical advice and highlights the key clinical elements which need to be considered to help understand the workflow process of SPECT/CT and optimise imaging protocols. The workflow process using SPECT/CT is complex in particular because of its bimodal character, the large spectrum of stakeholders, the multiplicity of their activities at various time points and the need for real-time decision-making. With help from analytical tools developed for quality assessment, the workflow process using SPECT/CT may be separated into related, but independent steps, each with its specific human and material resources to use as inputs or outputs. This helps identify factors that could contribute to failure in routine clinical practice. At each step of the process, practical aspects to optimise imaging procedure and protocols are developed. A decision-making algorithm for justifying each CT indication as well as the appropriateness of each CT protocol is the cornerstone of routine clinical practice using SPECT/CT. In conclusion, implementing hybrid SPECT/CT imaging requires new ways of working. It is highly rewarding from a clinical perspective, but it also proves to be a daily challenge in terms of management. (orig.)

SPECT/CT workflow and imaging protocols

International Nuclear Information System (INIS)

Beckers, Catherine; Hustinx, Roland

2014-01-01

Introducing a hybrid imaging method such as single photon emission computed tomography (SPECT)/CT greatly alters the routine in the nuclear medicine department. It requires designing new workflow processes and the revision of original scheduling process and imaging protocols. In addition, the imaging protocol should be adapted for each individual patient, so that performing CT is fully justified and the CT procedure is fully tailored to address the clinical issue. Such refinements often occur before the procedure is started but may be required at some intermediate stage of the procedure. Furthermore, SPECT/CT leads in many instances to a new partnership with the radiology department. This article presents practical advice and highlights the key clinical elements which need to be considered to help understand the workflow process of SPECT/CT and optimise imaging protocols. The workflow process using SPECT/CT is complex in particular because of its bimodal character, the large spectrum of stakeholders, the multiplicity of their activities at various time points and the need for real-time decision-making. With help from analytical tools developed for quality assessment, the workflow process using SPECT/CT may be separated into related, but independent steps, each with its specific human and material resources to use as inputs or outputs. This helps identify factors that could contribute to failure in routine clinical practice. At each step of the process, practical aspects to optimise imaging procedure and protocols are developed. A decision-making algorithm for justifying each CT indication as well as the appropriateness of each CT protocol is the cornerstone of routine clinical practice using SPECT/CT. In conclusion, implementing hybrid SPECT/CT imaging requires new ways of working. It is highly rewarding from a clinical perspective, but it also proves to be a daily challenge in terms of management. (orig.)

Enhanced spot preparation for liquid extractive sampling and analysis

Science.gov (United States)

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.

Analytical protocols for the determination of sulphur compounds characteristic of the metabolism of Chlorobium limicola

Directory of Open Access Journals (Sweden)

A. Aliboni

2015-09-01

Full Text Available Chlorobium limicola belongs to the green sulphur bacteria that has a potential for technological applications such as biogas clean up oxidising hydrogen sulphide to elemental sulphur through photosynthetic process. In the present work, analytical methods are described for the determination of different sulphur species in C. limicola cultures – sulphide by GC-FPD, sulphate by ionic HPLC and elemental sulphur by RP HPLC. The latter method eliminates the need for chloroform extraction of water suspensions of elemental sulphur. Data from sulphide and elemental sulphur analyses have been compared with ones coming from more traditional analytical methodologies.

A Business Evaluation Of The Next Generation Ipv6 Protocol In Fixed And Mobile Communication Services

OpenAIRE

Pau, Louis-François

2002-01-01

textabstractThis paper gives an analytical business model of the Internet IPv4 and IPv6 protocols ,focussing on the business implications of intrinsic technical properties of these protocols .The technical properties modeled in business terms are : address space, payload, autoconfiguration, IP mobility , security, and flow label. Three operational cash flow focussed performance indexes are defined for respectively an Internet operator or ISP, for the address domain owner, and for the end user...

Continuous sampling from distributed streams

DEFF Research Database (Denmark)

Graham, Cormode; Muthukrishnan, S.; Yi, Ke

2012-01-01

A fundamental problem in data management is to draw and maintain a sample of a large data set, for approximate query answering, selectivity estimation, and query planning. With large, streaming data sets, this problem becomes particularly difficult when the data is shared across multiple distribu......A fundamental problem in data management is to draw and maintain a sample of a large data set, for approximate query answering, selectivity estimation, and query planning. With large, streaming data sets, this problem becomes particularly difficult when the data is shared across multiple...... distributed sites. The main challenge is to ensure that a sample is drawn uniformly across the union of the data while minimizing the communication needed to run the protocol on the evolving data. At the same time, it is also necessary to make the protocol lightweight, by keeping the space and time costs low...... for each participant. In this article, we present communication-efficient protocols for continuously maintaining a sample (both with and without replacement) from k distributed streams. These apply to the case when we want a sample from the full streams, and to the sliding window cases of only the W most...

Advanced Curation: Solving Current and Future Sample Return Problems

Science.gov (United States)

Fries, M.; Calaway, M.; Evans, C.; McCubbin, F.

2015-01-01

Advanced Curation is a wide-ranging and comprehensive research and development effort at NASA Johnson Space Center that identifies and remediates sample related issues. For current collections, Advanced Curation investigates new cleaning, verification, and analytical techniques to assess their suitability for improving curation processes. Specific needs are also assessed for future sample return missions. For each need, a written plan is drawn up to achieve the requirement. The plan draws while upon current Curation practices, input from Curators, the analytical expertise of the Astromaterials Research and Exploration Science (ARES) team, and suitable standards maintained by ISO, IEST, NIST and other institutions. Additionally, new technologies are adopted on the bases of need and availability. Implementation plans are tested using customized trial programs with statistically robust courses of measurement, and are iterated if necessary until an implementable protocol is established. Upcoming and potential NASA missions such as OSIRIS-REx, the Asteroid Retrieval Mission (ARM), sample return missions in the New Frontiers program, and Mars sample return (MSR) all feature new difficulties and specialized sample handling requirements. The Mars 2020 mission in particular poses a suite of challenges since the mission will cache martian samples for possible return to Earth. In anticipation of future MSR, the following problems are among those under investigation: What is the most efficient means to achieve the less than 1.0 ng/sq cm total organic carbon (TOC) cleanliness required for all sample handling hardware? How do we maintain and verify cleanliness at this level? The Mars 2020 Organic Contamination Panel (OCP) predicts that organic carbon, if present, will be present at the "one to tens" of ppb level in martian near-surface samples. The same samples will likely contain wt% perchlorate salts, or approximately 1,000,000x as much perchlorate oxidizer as organic carbon

Analytical Techniques in the Pharmaceutical Sciences

DEFF Research Database (Denmark)

Leurs, Ulrike; Mistarz, Ulrik Hvid; Rand, Kasper Dyrberg

2016-01-01

Mass spectrometry (MS) offers the capability to identify, characterize and quantify a target molecule in a complex sample matrix and has developed into a premier analytical tool in drug development science. Through specific MS-based workflows including customized sample preparation, coupling...

Flow cytometry for feline lymphoma: a retrospective study regarding pre-analytical factors possibly affecting the quality of samples.

Science.gov (United States)

Martini, Valeria; Bernardi, Serena; Marelli, Priscilla; Cozzi, Marzia; Comazzi, Stefano

2018-06-01

Objectives Flow cytometry (FC) is becoming increasingly popular among veterinary oncologists for the diagnosis of lymphoma or leukaemia. It is accurate, fast and minimally invasive. Several studies of FC have been carried out in canine oncology and applied with great results, whereas there is limited knowledge and use of this technique in feline patients. This is mainly owing to the high prevalence of intra-abdominal lymphomas in this species and the difficulty associated with the diagnostic procedures needed to collect the sample. The purpose of the present study is to investigate whether any pre-analytical factor might affect the quality of suspected feline lymphoma samples for FC analysis. Methods Ninety-seven consecutive samples of suspected feline lymphoma were retrospectively selected from the authors' institution's FC database. The referring veterinarians were contacted and interviewed about several different variables, including signalment, appearance of the lesion, features of the sampling procedure and the experience of veterinarians performing the sampling. Statistical analyses were performed to assess the possible influence of these variables on the cellularity of the samples and the likelihood of it being finally processed for FC. Results Sample cellularity is a major factor in the likelihood of the sample being processed. Moreover, sample cellularity was significantly influenced by the needle size, with 21 G needles providing the highest cellularity. Notably, the sample cellularity and the likelihood of being processed did not vary between peripheral and intra-abdominal lesions. Approximately half of the cats required pharmacological restraint. Side effects were reported in one case only (transient swelling after peripheral lymph node sampling). Conclusions and relevance FC can be safely applied to cases of suspected feline lymphomas, including intra-abdominal lesions. A 21 G needle should be preferred for sampling. This study provides the basis for

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

OpenAIRE

Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detec...

Tank 48H Waste Composition and Results of Investigation of Analytical Methods

Energy Technology Data Exchange (ETDEWEB)

Walker , D.D. [Westinghouse Savannah River Company, AIKEN, SC (United States)

1997-04-02

This report serves two purposes. First, it documents the analytical results of Tank 48H samples taken between April and August 1996. Second, it describes investigations of the precision of the sampling and analytical methods used on the Tank 48H samples.

A distance limited method for sampling downed coarse woody debris

Science.gov (United States)

Jeffrey H. Gove; Mark J. Ducey; Harry T. Valentine; Michael S. Williams

2012-01-01

A new sampling method for down coarse woody debris is proposed based on limiting the perpendicular distance from individual pieces to a randomly chosen sample point. Two approaches are presented that allow different protocols to be used to determine field measurements; estimators for each protocol are also developed. Both protocols are compared via simulation against...

Analytic thinking reduces belief in conspiracy theories.

Science.gov (United States)

Swami, Viren; Voracek, Martin; Stieger, Stefan; Tran, Ulrich S; Furnham, Adrian

2014-12-01

Belief in conspiracy theories has been associated with a range of negative health, civic, and social outcomes, requiring reliable methods of reducing such belief. Thinking dispositions have been highlighted as one possible factor associated with belief in conspiracy theories, but actual relationships have only been infrequently studied. In Study 1, we examined associations between belief in conspiracy theories and a range of measures of thinking dispositions in a British sample (N=990). Results indicated that a stronger belief in conspiracy theories was significantly associated with lower analytic thinking and open-mindedness and greater intuitive thinking. In Studies 2-4, we examined the causational role played by analytic thinking in relation to conspiracist ideation. In Study 2 (N=112), we showed that a verbal fluency task that elicited analytic thinking reduced belief in conspiracy theories. In Study 3 (N=189), we found that an alternative method of eliciting analytic thinking, which related to cognitive disfluency, was effective at reducing conspiracist ideation in a student sample. In Study 4, we replicated the results of Study 3 among a general population sample (N=140) in relation to generic conspiracist ideation and belief in conspiracy theories about the July 7, 2005, bombings in London. Our results highlight the potential utility of supporting attempts to promote analytic thinking as a means of countering the widespread acceptance of conspiracy theories. Copyright © 2014 Elsevier B.V. All rights reserved.

A critical analysis of a locally agreed protocol for clinical practice

International Nuclear Information System (INIS)

Owen, A.; Hogg, P.; Nightingale, J.

2004-01-01

Within the traditional scope of radiographic practice (including advanced practice) there is a need to demonstrate effective patient care and management. Such practice should be set within a context of appropriate evidence and should also reflect peer practice. In order to achieve such practice the use of protocols is encouraged. Effective protocols can maximise care and management by minimising inter- and intra-professional variation; they can also allow for detailed procedural records to be kept in case of legal claims. However, whilst literature exists to encourage the use of protocols there is little published material available to indicate how to create, manage and archive them. This article uses an analytical approach to propose a suitable method for protocol creation and archival, it also offers suggestions on the scope and content of a protocol. To achieve this an existing clinical protocol for radiographer reporting barium enemas is analysed to draw out the general issues. Proposals for protocol creation, management, and archival were identified. The clinical practice described or inferred in the protocol should be drawn from evidence, such evidence could include peer-reviewed material, national standards and peer practice. The protocol should include an explanation of how to proceed when the radiographers reach the limit of their ability. It should refer to the initial training required to undertake the clinical duties as well as the on-going continual professional updating required to maintain competence. Audit of practice should be indicated, including the preferred audit methodology, and associated with this should be a clear statement about standards and what to do if standards are not adequately met. Protocols should be archived, in a paper-based form, for lengthy periods in case of legal claims. On the archived protocol the date it was in clinical use should be included

Soil Gas Sample Handling: Evaluation of Water Removal and Sample Ganging

Energy Technology Data Exchange (ETDEWEB)

Fritz, Brad G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Abrecht, David G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hayes, James C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Mendoza, Donaldo P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2016-10-31

Soil gas sampling is currently conducted in support of Nuclear Test Ban treaty verification. Soil gas samples are collected and analyzed for isotopes of interest. Some issues that can impact sampling and analysis of these samples are excess moisture and sample processing time. Here we discuss three potential improvements to the current sampling protocol; a desiccant for water removal, use of molecular sieve to remove CO₂ from the sample during collection, and a ganging manifold to allow composite analysis of multiple samples.

Flow cytometry for feline lymphoma: a retrospective study about pre-analytical factors possibly affecting the quality of samples

Directory of Open Access Journals (Sweden)

Serena Bernardi

2017-05-01

Full Text Available Introduction Flow cytometry (FC is an increasingly required technique on which veterinary oncologists rely to have an accurate, fast, minimally invasive lymphoma or leukemia diagnosis. FC has been studied and applied with great results in canine oncology, whereas in feline oncology the use of this technique is still to be experienced. This is mainly due to a supposed discomfort in sampling, because of the high prevalence of intra-abdominal lymphomas. The purpose of the present study is to investigate whether any pre-analytical factor might affect the quality of suspected feline lymphoma samples for FC analysis. Methods 97 consecutive samples of suspected feline lymphoma were retrospectively selected from the authors’ institution FC database. The referring veterinarians were recalled and interrogated about several different variables, including signalling, features of the lesion, features of the sampling procedure and the experience of veterinarians performing the sampling. Statistical analyses were performed to assess the possible influence of these variables on the cellularity of the samples and the likelihood of being finally processed for FC. Results None of the investigated variables significantly influenced the quality of the submitted samples, but the needle size, with 21G needles providing the highest cellularity (Table 1. Notably, the samples quality did not vary between peripheral and intra-abdominal lesions. Sample cellularity alone influenced the likelihood of being processed. About a half of the cats required pharmacological restraint. Side effects were reported in one case only (transient swelling after peripheral lymph node sampling. Conclusions FC can be safely applied to cases of suspected feline lymphomas, even for intra-abdominal lesions. 21G needle should be preferred for sampling. This study provides the bases for the spread of this minimally invasive, fast and cost-effective technique in feline medicine.

Multispectral analytical image fusion

International Nuclear Information System (INIS)

Stubbings, T.C.

2000-04-01

With new and advanced analytical imaging methods emerging, the limits of physical analysis capabilities and furthermore of data acquisition quantities are constantly pushed, claiming high demands to the field of scientific data processing and visualisation. Physical analysis methods like Secondary Ion Mass Spectrometry (SIMS) or Auger Electron Spectroscopy (AES) and others are capable of delivering high-resolution multispectral two-dimensional and three-dimensional image data; usually this multispectral data is available in form of n separate image files with each showing one element or other singular aspect of the sample. There is high need for digital image processing methods enabling the analytical scientist, confronted with such amounts of data routinely, to get rapid insight into the composition of the sample examined, to filter the relevant data and to integrate the information of numerous separate multispectral images to get the complete picture. Sophisticated image processing methods like classification and fusion provide possible solution approaches to this challenge. Classification is a treatment by multivariate statistical means in order to extract analytical information. Image fusion on the other hand denotes a process where images obtained from various sensors or at different moments of time are combined together to provide a more complete picture of a scene or object under investigation. Both techniques are important for the task of information extraction and integration and often one technique depends on the other. Therefore overall aim of this thesis is to evaluate the possibilities of both techniques regarding the task of analytical image processing and to find solutions for the integration and condensation of multispectral analytical image data in order to facilitate the interpretation of the enormous amounts of data routinely acquired by modern physical analysis instruments. (author)

Non-Contact Conductivity Measurement for Automated Sample Processing Systems

Science.gov (United States)

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

A ring test of in vitro neutral detergent fiber digestibility: analytical variability and sample ranking.

Science.gov (United States)

Hall, M B; Mertens, D R

2012-04-01

In vitro neutral detergent fiber (NDF) digestibility (NDFD) is an empirical measurement of fiber fermentability by rumen microbes. Variation is inherent in all assays and may be increased as multiple steps or differing procedures are used to assess an empirical measure. The main objective of this study was to evaluate variability within and among laboratories of 30-h NDFD values analyzed in repeated runs. Subsamples of alfalfa (n=4), corn forage (n=5), and grass (n=5) ground to pass a 6-mm screen passed a test for homogeneity. The 14 samples were sent to 10 laboratories on 3 occasions over 12 mo. Laboratories ground the samples and ran 1 to 3 replicates of each sample within fermentation run and analyzed 2 or 3 sets of samples. Laboratories used 1 of 2 NDFD procedures: 8 labs used procedures related to the 1970 Goering and Van Soest (GVS) procedure using fermentation vessels or filter bags, and 2 used a procedure with preincubated inoculum (PInc). Means and standard deviations (SD) of sample replicates within run within laboratory (lab) were evaluated with a statistical model that included lab, run within lab, sample, and lab × sample interaction as factors. All factors affected mean values for 30-h NDFD. The lab × sample effect suggests against a simple lab bias in mean values. The SD ranged from 0.49 to 3.37% NDFD and were influenced by lab and run within lab. The GVS procedure gave greater NDFD values than PInc, with an average difference across all samples of 17% NDFD. Because of the differences between GVS and PInc, we recommend using results in contexts appropriate to each procedure. The 95% probability limits for within-lab repeatability and among-lab reproducibility for GVS mean values were 10.2 and 13.4%, respectively. These percentages describe the span of the range around the mean into which 95% of analytical results for a sample fall for values generated within a lab and among labs. This degree of precision was supported in that the average maximum

Quantification of process induced disorder in milled samples using different analytical techniques

DEFF Research Database (Denmark)

Zimper, Ulrike; Aaltonen, Jaakko; McGoverin, Cushla M.

2012-01-01

The aim of this study was to compare three different analytical methods to detect and quantify the amount of crystalline disorder/ amorphousness in two milled model drugs. X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman spectroscopy were used as analytical methods...... and indomethacin and simvastatin were chosen as the model compounds. These compounds partly converted from crystalline to disordered forms by milling. Partial least squares regression (PLS) was used to create calibration models for the XRPD and Raman data, which were subsequently used to quantify the milling......-induced crystalline disorder/ amorphousness under different process conditions. In the DSC measurements the change in heat capacity at the glass transition was used for quantification. Differently prepared amorphous indomethacin standards (prepared by either melt quench cooling or cryo milling) were compared...