A Thermal Stability Test for Primary Explosive Stab Sensitizers: Study of the Thermal and Hydrolytic Stability of 2-Picryl-5-Nitrotetrazole,

DTIC Science & Technology

1984-02-01

have been described previously (2]. The actual batch used was designated Batch D and was identical to that referred to as Batch C in Reference [2...Tetrazene was type RD1357 prepared at Materials Research Laboratories. The batch used was designated Batch 10/83(A). Lead Azide was type RD1343 and was...Preparation of Experimental Detonators Eperimental detonators were prepared in mild steel tubes, 6 mm o.d., 3.2 mm i.d., length 6 mm, prepared from

[Development and application of reference materials containing mixed degradation products of amoxicillin and ampicillin].

PubMed

Li, Wei; Zhang, Wei-Qing; Li, Xiang; Hu, Chang-Qin

2014-09-01

Reference materials containing mixed degradation products of amoxicillin and ampicillin were developed after optimization of preparation processes. The target impurities were obtained by controlled stress testing, and each major component was identified with HPLC-MS and compared with single traceable reference standard each. The developed reference materials were applied to system suitability test for verifying HPLC system performed in accordance with set forth in China Pharmacopeia and identification of major impurities in samples based on retention and spectra information, which have advantages over the methods put forth in foreign pharmacopoeias. The development and application of the reference materials offer an effective way for rapid identification of impurities in chromatograms, and provide references for analyzing source of impurities and evaluation of drug quality.

Collaborative study for the establishment of the WHO 3(rd) International Standard for Endotoxin, the Ph. Eur. endotoxin biological reference preparation batch 5 and the USP Reference Standard for Endotoxin Lot H0K354.

PubMed

Findlay, L; Desai, T; Heath, A; Poole, S; Crivellone, M; Hauck, W; Ambrose, M; Morris, T; Daas, A; Rautmann, G; Buchheit, K H; Spieser, J M; Terao, E

2015-01-01

An international collaborative study was organised jointly by the World Health Organization (WHO)/National Institute for Biological Standards and Control (NIBSC), the United States Pharmacopeia (USP) and the European Directorate for the Quality of Medicines & HealthCare (EDQM/Council of Europe) for the establishment of harmonised replacement endotoxin standards for these 3 organisations. Thirty-five laboratories worldwide, including Official Medicines Control Laboratories (OMCLs) and manufacturers enrolled in the study. Three candidate preparations (10/178, 10/190 and 10/196) were produced with the same material and same formulation as the current reference standards with the objective of generating a new (3(rd)) International Standard (IS) with the same potency (10 000 IU/vial) as the current (2(nd)) IS, as well as new European Pharmacopoeia (Ph. Eur.). and USP standards. The suitability of the candidate preparations to act as the reference standard in assays for endotoxin performed according to compendial methods was evaluated. Their potency was calibrated against the WHO 2(nd) IS for Endotoxin (94/580). Gelation and photometric methods produced similar results for each of the candidate preparations. The overall potency estimates for the 3 batches were comparable. Given the intrinsic assay precision, the observed differences between the batches may be considered unimportant for the intended use of these materials. Overall, these results were in line with those generated for the establishment of the current preparations of reference standards. Accelerated degradation testing of vials stored at elevated temperatures supported the long-term stability of the 3 candidate preparations. It was agreed between the 3 organisations that batch 10/178 be shared between WHO and EDQM and that batches 10/190 and 10/196 be allocated to USP, with a common assigned value of 10 000 IU/vial. This value maintains the continuity of the global harmonisation of reference materials and unitage for the testing of endotoxins in parenteral pharmaceutical products. Based on the results of the collaborative study, batch 10/178 was established by the European Pharmacopoeia Commission as the Ph. Eur. Endotoxin Biological Reference Preparation (BRP) batch 5. The same batch was also established by the Expert Committee on Biological Standardisation (ECBS) of WHO as the WHO 3(rd) IS for Endotoxin. Batch 10/190 was adopted as the USP Endotoxin Reference Standard, lot H0K354 and vials from this same batch (10/190) will serve as the United States Food and Drug Administration (USFDA) Endotoxin Standard, EC-7.

Research Progress of Building Materials Used in Construction Land

NASA Astrophysics Data System (ADS)

Niu, Yan

2018-01-01

Construction land preparation is an important aspect of land remediation project. The research of materials in the process of land improvement is the foundation and the core. Therefore, it is necessary to study the materials that may be involved in the process of building land preparation. In this paper, the research on the construction materials such as recycled concrete, geosynthetics, soil stabilizers, soil improvers, building insulation materials and inorganic fibrous insulation materials, which are commonly used in construction sites, is reviewed and discussed in this paper. Land remediation project involved in the construction of land materials to provide reference.

INSTRUCTIONAL PROGRAMMING PROCEDURES, A PROGRAMED COURSE IN THE BASIC METHODS AND TECHNIQUES OF PREPARING PROGRAMED INSTRUCTIONAL MATERIALS.

ERIC Educational Resources Information Center

DETERLINE, WILLIAM A.

A PROGRAMED COURSE IN METHODS AND TECHNIQUES OF PREPARING PROGRAMED INSTRUCTIONAL MATERIALS WAS PRESENTED IN THIS DOCUMENT. AN ATTEMPT WAS MADE TO TEACH BASIC PROCEDURES WELL ENOUGH TO PRODUCE AN EMBRYO PROGRAMER AND TO PROVIDE HIM WITH REFERENCES HE WOULD NEED IN ORDER TO PRODUCE PROGRAMS. INCLUDED WERE PROGRAMED INSTRUCTIONS ON PREPARATORY…

Reference Materials: Significance, General Requirements, and Demand.

PubMed

Kiełbasa, Anna; Gadzała-Kopciuch, Renata; Buszewski, Bogusław

2016-05-03

Reference materials play an important part in the quality control of measurements. Rapid development of such new scientific disciplines as proteomics, metabolomics, and genomics also necessitates development of new reference materials. This is a great challenge due to the complexity of the production of new reference materials and difficulties associated with achieving their homogeneity and stability. CRMs of tissue are of particular importance. They can be counted among the matrices that are most complex and time consuming in preparation. Tissue is the place of transformation and accumulation of many substances (e.g., metabolites, which are intermediate or end products resulting from metabolic processes). Trace amounts of many substances in tissues must be determined with adequate precision and accuracy. To meet the needs stemming from research and from problems and challenges faced by chemists, analysts, and toxicologists, the number of certified reference materials should be continuously increased.

Establishing the traceability of a uranyl nitrate solution to a standard reference material

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

Jackson, C.H.; Clark, J.P.

1978-01-01

A uranyl nitrate solution for use as a Working Calibration and Test Material (WCTM) was characterized, using a statistically designed procedure to document traceability to National Bureau of Standards Reference Material (SPM-960). A Reference Calibration and Test Material (PCTM) was prepared from SRM-960 uranium metal to approximate the acid and uranium concentration of the WCTM. This solution was used in the characterization procedure. Details of preparing, handling, and packaging these solutions are covered. Two outside laboratories, each having measurement expertise using a different analytical method, were selected to measure both solutions according to the procedure for characterizing the WCTM. Twomore » different methods were also used for the in-house characterization work. All analytical results were tested for statistical agreement before the WCTM concentration and limit of error values were calculated. A concentration value was determined with a relative limit of error (RLE) of approximately 0.03% which was better than the target RLE of 0.08%. The use of this working material eliminates the expense of using SRMs to fulfill traceability requirements for uranium measurements on this type material. Several years' supply of uranyl nitrate solution with NBS traceability was produced. The cost of this material was less than 10% of an equal quantity of SRM-960 uranium metal.« less

Hazardous materials transportation in Arizona.

DOT National Transportation Integrated Search

2010-03-01

The purpose of this report is to summarize the data that have been collected, provide references to other : researched material that supports the findings of this study, and provide a set of viable recommendations for : moving forward with the prepar...

Reading Materials in Large Type. Reference Circular No. 87-4.

ERIC Educational Resources Information Center

Library of Congress, Washington, DC. National Library Service for the Blind and Physically Handicapped.

This circular provides information about reading materials in large type, i.e., materials set in type that is a minimum size of 14-point and, most commonly, 16- to 18-point size. Most of the materials listed are typeset, but a few are photographically enlarged conventionally printed books or typewritten materials prepared using a large-print…

The influence of Saccharomyces cerevisiae enzyme ratio on preparation virgin coconut oil for candidate in-house reference materials

NASA Astrophysics Data System (ADS)

Rohyami, Yuli; Anjani, Rafika Debby; Purwanti, Napthalina Putri

2017-03-01

Virgin coconut oil is an excellent product which has result of oil processing business opportunities in the international market. Standardization of virgin coconut oil necessary to satisfy the requirements industry needs. This research is expected as procedure preparation of reference materials. Preparation of virgin coconut oil by Sacharomycescerevisiaeenzyme. Based on the results of this study concluded that the ratio of Saccharomyces cerevisiae can affect the yield of virgin coconut oil produced. The preparation of virgin coconut oil enzymatically using a variety of mass ratio of 0.001 to 0.006% is obtained yield average of 12.40%. The optimum separation of virgin coconut oil on the use of enzymes with a mass ratio of 0.002%. The average water content at a ratio of 0.002% is 0.04 % with a value of uncertainty is 0.005%. The average iodine number in virgin coconut oil produced is 2.4403 ± 0,1974 grams of iodine per 100 grams of oil and optimum iodine number is obtained from the manufacturing process virgin coconut oil with a ratio of 0.006% Saccharomyces cerevisiae. Sacharomycescerevisiae with a ratio of 0.002% results virgin coconut oil with acid number 0.3068 ± 0.1098%. The peroxide value of virgin coconut oil between 0.0108 ± 0.009 to 0.0114 ± 0015milli-equivalent per kilograms. Organoleptic test results and test chemical parameters can be used as the test data that can be developed in prototype preparation of candidate in-house reference material in the testing standards of quality virgin coconut oil.

Proyecto Leer Bulletin, Number 10.

ERIC Educational Resources Information Center

Benson, Susan Shattuck

This guide to instructional materials for teachers of Spanish contains references to commercially-prepared works in several classified areas. The works listed are intended for use in grades ranging from kindergarten through senior high school and also include materials for adult education. The 10 categories cover: (1) audiovisual materials, (2)…

International reference preparations of typhoid vaccine

PubMed Central

Melikova, E. N.; Lesnjak, S. V.

1967-01-01

International collaborative laboratory studies on the International Reference Preparations of Typhoid Vaccine have so far failed to provide data on which international units for these vaccines can be based. Further assays carried out using the active mouse protection test, with immunization by the subcutaneous, intraperitoneal or intravenous route, confirmed the findings by some workers that the International Reference Preparation of Typhoid Vaccine (Acetone-Inactivated) (vaccine K) was more effective than the International Reference Preparation of Typhoid Vaccine (Heat-Phenol-Inactivated) (vaccine L), and indicated that intraperitoneal immunization was the most promising method. Vaccine K, together with the material extracted by the acetone in the preparation of the vaccine, had a significantly lower effectiveness (at the 5% probability level) only when intraperitoneal immunization was used. The reasons for the differences found between the various vaccines and routes of immunization are discussed at length. It is suggested that challenge with a strain of Salmonella moscow instead of the strain of Salm. typhi used until now gives a true infection and forms the basis of a reliable method for the potency assay of typhoid vaccines. PMID:5301738

DOE research and development report. Progress report, October 1980-September 1981

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

Bingham, Carleton D.

The DOE New Brunswick Laboratory (NBL) is the US Government's Nuclear Materials Standards and Measurement Laboratory. NBL is assigned the mission to provide and maintain, as an essential part of federal statutory responsibilities related to national and international safeguards of nuclear materials for USA defense and energy programs, an ongoing capability for: the development, preparation, certification, and distribution of reference materials for the calibration and standardization of nuclear materials measurements; the development, improvement, and evaluation of nuclear materials measurement technology; the assessment and evaluation of the practice and application of nuclear materials measurement technology; expert and reliable specialized nuclear materialsmore » measurement services for the government; and technology exchange and training in nuclear materials measurement and standards. Progress reports for this fiscal year are presented under the following sections: (1) development or evaluation of measurement technology (elemental assay of uranium plutonium; isotope composition); (2) standards and reference materials (NBL standards and reference materials; NBS reference materials); and (3) evaluation programs (safeguards analytical laboratory evaluation; general analytical evaluation program; other evaluation programs).« less

Oxygen potential of uranium--plutonium oxide as determined by controlled- atmosphere thermogravimetry

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

Swanson, Gerald C.

1975-10-01

The oxygen-to-metal atom ratio, or O/M, of solid solution uranium- plutonium oxide reactor fuel is a measure of the concentration of crystal defects in the oxide which affect many fuel properties, particularly, fuel oxygen potential. Fabrication of a high-temperature oxygen electrode, employing an electro-active tip of oxygen-deficient solid-state electrolyte, intended to confirm gaseous oxygen potentials is described. Uranium oxide and plutonium oxide O/M reference materials were prepared by in situ oxidation of high purity metals in the thermobalance. A solid solution uranium-plutonium oxide O/M reference material was prepared by alloying the uranium and plutonium metals in a yttrium oxide cruciblemore » at 1200°C and oxidizing with moist He at 250°C. The individual and solid solution oxides were isothermally equilibrated with controlled oxygen potentials between 800 and 1300°C and the equilibrated O/ M ratios calculated with corrections for impurities and buoyancy effects. Use of a reference oxygen potential of -100 kcal/mol to produce an O/M of 2.000 is confirmed by these results. However, because of the lengthy equilibration times required for all oxides, use of the O/M reference materials rather than a reference oxygen potential is recommended for O/M analysis methods calibrations.« less

Preparation and characterization of a suite of ephedra-containing standard reference materials.

PubMed

Sharpless, Katherine E; Anderson, David L; Betz, Joseph M; Butler, Therese A; Capar, Stephen G; Cheng, John; Fraser, Catharine A; Gardner, Graeme; Gay, Martha L; Howell, Daniel W; Ihara, Toshihide; Khan, Mansoor A; Lam, Joseph W; Long, Stephen E; McCooeye, Margaret; Mackey, Elizabeth A; Mindak, William R; Mitvalsky, Staci; Murphy, Karen E; NguyenPho, Agnes; Phinney, Karen W; Porter, Barbara J; Roman, Mark; Sander, Lane C; Satterfield, Mary B; Scriver, Christine; Sturgeon, Ralph; Thomas, Jeanice Brown; Vocke, Robert D; Wise, Stephen A; Wood, Laura J; Yang, Lu; Yen, James H; Ziobro, George C

2006-01-01

The National Institute of Standards and Technology, the U.S. Food and Drug Administration, Center for Drug Evaluation and Research and Center for Food Safety and Applied Nutrition, and the National Institutes of Health, Office of Dietary Supplements, are collaborating to produce a series of Standard Reference Materials (SRMs) for dietary supplements. A suite of ephedra materials is the first in the series, and this paper describes the acquisition, preparation, and value assignment of these materials: SRMs 3240 Ephedra sinica Stapf Aerial Parts, 3241 E. sinica Stapf Native Extract, 3242 E. sinica Stapf Commercial Extract, 3243 Ephedra-Containing Solid Oral Dosage Form, and 3244 Ephedra-Containing Protein Powder. Values are assigned for ephedrine alkaloids and toxic elements in all 5 materials. Values are assigned for other analytes (e.g., caffeine, nutrient elements, proximates, etc.) in some of the materials, as appropriate. Materials in this suite of SRMs are intended for use as primary control materials when values are assigned to in-house (secondary) control materials and for validation of analytical methods for the measurement of alkaloids, toxic elements, and, in the case of SRM 3244, nutrients in similar materials.

Biophysical characterization and structure of the Fab fragment from the NIST reference antibody, RM 8671.

PubMed

Karageorgos, Ioannis; Gallagher, Elyssia S; Galvin, Connor; Gallagher, D Travis; Hudgens, Jeffrey W

2017-11-01

Monoclonal antibody pharmaceuticals are the fastest-growing class of therapeutics, with a wide range of clinical applications. To assure their safety, these protein drugs must demonstrate highly consistent purity and stability. Key to these objectives is higher order structure measurements validated by calibration to reference materials. We describe preparation, characterization, and crystal structure of the Fab fragment prepared from the NIST Reference Antibody RM 8671 (NISTmAb). NISTmAb is a humanized IgG1κ antibody, produced in murine cell culture and purified by standard biopharmaceutical production methods, developed at the National Institute of Standards and Technology (NIST) to serve as a reference material. The Fab fragment was derived from NISTmAb through papain cleavage followed by protein A based purification. The purified Fab fragment was characterized by SDS-PAGE, capillary gel electrophoresis, multi-angle light scattering, size exclusion chromatography, mass spectrometry, and x-ray crystallography. The crystal structure at 0.2 nm resolution includes four independent Fab molecules with complete light chains and heavy chains through Cys 223, enabling assessment of conformational variability and providing a well-characterized reference structure for research and engineering applications. This nonproprietary, publically available reference material of known higher-order structure can support metrology in biopharmaceutical applications, and it is a suitable platform for validation of molecular modeling studies. Published by Elsevier Ltd.

Direct and simultaneous detection of organic and inorganic ingredients in herbal powder preparations by Fourier transform infrared microspectroscopic imaging

NASA Astrophysics Data System (ADS)

Chen, Jian-bo; Sun, Su-qin; Tang, Xu-dong; Zhang, Jing-zhao; Zhou, Qun

2016-08-01

Herbal powder preparation is a kind of widely-used herbal product in the form of powder mixture of herbal ingredients. Identification of herbal ingredients is the first and foremost step in assuring the quality, safety and efficacy of herbal powder preparations. In this research, Fourier transform infrared (FT-IR) microspectroscopic identification method is proposed for the direct and simultaneous recognition of multiple organic and inorganic ingredients in herbal powder preparations. First, the reference spectrum of characteristic particles of each herbal ingredient is assigned according to FT-IR results and other available information. Next, a statistical correlation threshold is determined as the lower limit of correlation coefficients between the reference spectrum and a larger number of calibration characteristic particles. After validation, the reference spectrum and correlation threshold can be used to identify herbal ingredient in mixture preparations. A herbal ingredient is supposed to be present if correlation coefficients between the reference spectrum and some sample particles are above the threshold. Using this method, all kinds of herbal materials in powder preparation Kouqiang Kuiyang San are identified successfully. This research shows the potential of FT-IR microspectroscopic identification method for the accurate and quick identification of ingredients in herbal powder preparations.

Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies

PubMed Central

Harju, Kirsi; Rapinoja, Marja-Leena; Avondet, Marc-André; Arnold, Werner; Schär, Martin; Luginbühl, Werner; Kremp, Anke; Suikkanen, Sanna; Kankaanpää, Harri; Burrell, Stephen; Söderström, Martin; Vanninen, Paula

2015-01-01

A saxitoxin (STX) proficiency test (PT) was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox) project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP) toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC) methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses. PMID:26602927

Thermally Cross-Linkable Hole Transport Materials for Solution Processed Phosphorescent OLEDs

NASA Astrophysics Data System (ADS)

Kim, Beom Seok; Kim, Ohyoung; Chin, Byung Doo; Lee, Chil Won

2018-04-01

Materials for unique fabrication of a solution-processed, multi-layered organic light-emitting diode (OLED) were developed. Preparation of a hole transport layer with a thermally cross-linkable chemical structure, which can be processed to form a thin film and then transformed into an insoluble film by using an amine-alcohol condensation reaction with heat treatment, was investigated. Functional groups, such as triplenylamine linked with phenylcarbazole or biphenyl, were employed in the chemical structure of the hole transport layer in order to maintain high triplet energy properties. When phenylcarbazole or biphenyl compounds continuously react with triphenylamine under acid catalysis, a chemically stable thin film material with desirable energy-level properties for a blue OLED could be obtained. The prepared hole transport materials showed excellent surface roughness and thermal stability in comparison with the commercial reference material. On the solution-processed model hole transport layer, we fabricated a device with a blue phosphorescent OLED by using sequential vacuum deposition. The maximum external quantum, 19.3%, was improved by more than 40% over devices with the commercial reference material (11.4%).

Discovering Historic Iowa. American Revolution Bicentennial Edition.

ERIC Educational Resources Information Center

Pratt, LeRoy G.

Prepared in recognition of the Bicentennial, this historic guide of Iowa is intended to supplement materials prepared by the Iowa Curriculum Division. It provides, in one convenient reference, information for use by teachers, students, tourists, and others interested in Iowa's history. Up-to-date information is given on historical societies,…

Certification of reference materials for the determination of alkylphenols.

PubMed

Hanari, Nobuyasu; Ishikawa, Keiichiro; Shimizu, Yoshitaka; Otsuka, Satoko; Iwasawa, Ryoko; Fujiki, Naomi; Numata, Masahiko; Yarita, Takashi; Kato, Kenji

2015-04-01

Certified reference materials (CRMs) are playing an increasingly important role in national and international standardizing activities. In Japan, primary standard solutions for analyses of endocrine disrupters are supplied under the national standards dissemination system named the Japan Calibration Service System (JCSS). For the traceability on reference materials used for preparation of the primary standard solutions based on the JCSS, the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has developed and certified high-purity reference materials of alkylphenols as NMIJ CRMs, such as 4-n-nonylphenol, 4-tert-octylphenol, 4-n-heptylphenol, 4-tert-butylphenol, and 2,4-dichlorophenol. Thereafter, it is essential to determine the alkylphenols by using these solutions based on the JCSS for environmental monitoring and risk assessments because analytical values obtained by using the solutions can ensure the reliability and traceability of the chemical analyses.

Two new organic reference materials for δ13C and δ15N measurements and a new value for the δ13C of NBS 22 oil

USGS Publications Warehouse

Qi, Haiping; Coplen, Tyler B.; Geilmann, Heike; Brand, Willi A.; Böhlke, J.K.

2003-01-01

Analytical grade L-glutamic acid is chemically stable and has a C/N mole ratio of 5, which is close to that of many of natural biological materials, such as blood and animal tissue. Two L-glutamic acid reference materials with substantially different 13C and 15N abundances have been prepared for use as organic reference materials for C and N isotopic measurements. USGS40 is analytical grade L-glutamic acid and has a δ13C value of −26.24‰ relative to VPDB and a δ15N value of −4.52‰ relative to N2 in air. USGS41 was prepared by dissolving analytical grade L-glutamic acid with L-glutamic acid enriched in 13C and 15N. USGS41 has a δ13C value of +37.76‰ and a δ15N value of +47.57‰. The δ13C and δ15N values of both materials were measured against the international reference materials NBS 19 calcium carbonate (δ13C = +1.95‰), L-SVEC lithium carbonate (δ13C = −46.48‰), IAEA-N-1 ammonium sulfate (δ15N = 0.43‰), and USGS32 potassium nitrate (δ15N = 180‰) by on-line combustion continuous-flow and off-line dual-inlet isotope-ratio mass spectrometry. Both USGS40 and USGS41 are isotopically homogeneous; reproducibility of δ13C is better than 0.13‰, and that of δ15N is better than 0.13‰ in 100-μg amounts. These two isotopic reference materials can be used for (i) calibrating local laboratory reference materials, and (ii) quantifying drift with time, mass-dependent fractionations, and isotope-ratio-scale contraction in the isotopic analysis of various biological materials. Isotopic results presented in this paper yield a δ13C value for NBS 22 oil of −29.91‰, in contrast to the commonly accepted value of −29.78‰ for which off-line blank corrections probably have not been quantified satisfactorily.

Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

PubMed

Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

2000-10-01

Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

Homogeneity study of a corn flour laboratory reference material candidate for inorganic analysis.

PubMed

Dos Santos, Ana Maria Pinto; Dos Santos, Liz Oliveira; Brandao, Geovani Cardoso; Leao, Danilo Junqueira; Bernedo, Alfredo Victor Bellido; Lopes, Ricardo Tadeu; Lemos, Valfredo Azevedo

2015-07-01

In this work, a homogeneity study of a corn flour reference material candidate for inorganic analysis is presented. Seven kilograms of corn flour were used to prepare the material, which was distributed among 100 bottles. The elements Ca, K, Mg, P, Zn, Cu, Fe, Mn and Mo were quantified by inductively coupled plasma optical emission spectrometry (ICP OES) after acid digestion procedure. The method accuracy was confirmed by analyzing the rice flour certified reference material, NIST 1568a. All results were evaluated by analysis of variance (ANOVA) and principal component analysis (PCA). In the study, a sample mass of 400mg was established as the minimum mass required for analysis, according to the PCA. The between-bottle test was performed by analyzing 9 bottles of the material. Subsamples of a single bottle were analyzed for the within-bottle test. No significant differences were observed for the results obtained through the application of both statistical methods. This fact demonstrates that the material is homogeneous for use as a laboratory reference material. Copyright © 2015 Elsevier Ltd. All rights reserved.

Metrological traceability of holmium oxide solution

NASA Astrophysics Data System (ADS)

Gonçalves, D. E. F.; Gomes, J. F. S.; Alvarenga, A. P. D.; Borges, P. P.; Araujo, T. O.

2018-03-01

Holmium oxide solution was prepared as a candidate of certified reference material for spectrophotometer wavelength scale calibration. Here is presented the necessary steps for evaluation of the uncertainty and the establishment of metrological traceability for the production of this material. Preliminary results from the first produced batch are shown.

Standard method of test for grindability of coal by the Hardgrove-machine method

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

Not Available

1975-01-01

A procedure is described for sampling coal, grinding in a Hardgrove grinding machine, and passing through standard sieves to determine the degree of pulverization of coals. The grindability index of the coal tested is calculated from a calibration chart prepared by plotting weight of material passing a No. 200 sieve versus the Hardgrove Grindability Index for the standard reference samples. The Hardgrove machine is shown schematically. The method for preparing and determining grindability indexes of standard reference samples is given in the appendix. (BLM)

Production and certification of NIST Standard Reference Material 2372 Human DNA Quantitation Standard.

PubMed

Kline, Margaret C; Duewer, David L; Travis, John C; Smith, Melody V; Redman, Janette W; Vallone, Peter M; Decker, Amy E; Butler, John M

2009-06-01

Modern highly multiplexed short tandem repeat (STR) assays used by the forensic human-identity community require tight control of the initial amount of sample DNA amplified in the polymerase chain reaction (PCR) process. This, in turn, requires the ability to reproducibly measure the concentration of human DNA, [DNA], in a sample extract. Quantitative PCR (qPCR) techniques can determine the number of intact stretches of DNA of specified nucleotide sequence in an extremely small sample; however, these assays must be calibrated with DNA extracts of well-characterized and stable composition. By 2004, studies coordinated by or reported to the National Institute of Standards and Technology (NIST) indicated that a well-characterized, stable human DNA quantitation certified reference material (CRM) could help the forensic community reduce within- and among-laboratory quantitation variability. To ensure that the stability of such a quantitation standard can be monitored and that, if and when required, equivalent replacement materials can be prepared, a measurement of some stable quantity directly related to [DNA] is required. Using a long-established conventional relationship linking optical density (properly designated as decadic attenuance) at 260 nm with [DNA] in aqueous solution, NIST Standard Reference Material (SRM) 2372 Human DNA Quantitation Standard was issued in October 2007. This SRM consists of three quite different DNA extracts: a single-source male, a multiple-source female, and a mixture of male and female sources. All three SRM components have very similar optical densities, and thus very similar conventional [DNA]. The materials perform very similarly in several widely used gender-neutral assays, demonstrating that the combination of appropriate preparation methods and metrologically sound spectrophotometric measurements enables the preparation and certification of quantitation [DNA] standards that are both maintainable and of practical utility.

Preparation of a PM2.5-like reference material in sufficient quantities for accurate monitoring of anions and cations in fine atmospheric dust.

PubMed

Charoud-Got, Jean; Emma, Giovanni; Seghers, John; Tumba-Tshilumba, Marie-France; Santoro, Anna; Held, Andrea; Snell, James; Emteborg, Håkan

2017-12-01

A reference material of a PM 2.5 -like atmospheric dust material has been prepared using a newly developed method. It is intended to certify values for the mass fraction of SO 4 2- , NO 3 - , Cl - (anions) and Na + , K + , NH 4 + , Ca 2+ , Mg 2+ (cations) in this material. A successful route for the preparation of the candidate reference material is described alongside with two alternative approaches that were abandoned. First, a PM 10 -like suspension was allowed to stand for 72 h. Next, 90% of the volume was siphoned off. The suspension was spiked with appropriate levels of the desired ions just prior to drop-wise shock-freezing in liquid nitrogen. Finally, freeze drying of the resulting ice kernels took place. In using this approach, it was possible to produce about 500 g of PM 2.5 -like material with appropriate characteristics. Fine dust in 150-mg portions was filled into vials under an inert atmosphere. The final candidate material approaches the EN12341 standard of a PM 2.5 -material containing the ions mentioned in Directive 2008/50/EC of the European Union. The material should be analysed using the CEN/TR 16269:2011 method for anions and cations in PM 2.5 collected on filters. The method described here is a relatively rapid means to obtain large quantities of PM 2.5 . With access to smaller freeze dryers, still 5 to 10 g per freeze-drying cycle can be obtained. Access to such quantities of PM 2.5 -like material could potentially be used for different kinds of experiments when performing research in this field. Graphical abstract The novelty of the method lies in transformation of a suspension with fine particulate matter to a homogeneous and stable powder with characteristics similar to air-sampled PM 2,5 . The high material yield in a relatively short time is a distinct advantage in comparison with collection of air-sampled PM 2,5 .

Characterization of Lone Pine, California, tremolite asbestos and preparation of research material

USGS Publications Warehouse

Harper, Martin; Van Gosen, Bradley S.; Crankshaw, Owen S; Doorn, Stacy S; Ennis, J. Todd; Harrison, Sara E

2014-01-01

Well-characterized amphibole asbestos mineral samples are required for use as analytical standards and in future research projects. Currently, the National Institute for Standards and Technology Standard Reference Material samples of asbestos are listed as ‘Discontinued’. The National Institute for Occupational Safety and Health (NIOSH) has a goal under the Asbestos Roadmap of locating and characterizing research materials for future use. Where an initial characterization analysis determines that a collected material is appropriate for use as a research material in terms of composition and asbestiform habit, sufficient amounts of the material will be collected to make it publicly available. An abandoned mine near Lone Pine, California, contains a vein of tremolite asbestos, which was the probable source of a reference material that has been available for the past 17 years from the Health and Safety Laboratory (HSL) in the UK. Newly collected fibrous vein material from this mine was analyzed at Research Triangle Institute (RTI International) with some additional analysis by the US Geological Survey’s Denver Microbeam Laboratory. The analysis at RTI International included: (i) polarized light microscopy (PLM) with a determination of principal optical properties; (ii) X-ray diffraction; (iii) transmission electron microscopy, including energy dispersive X-ray spectroscopy and selected-area electron diffraction; and (iv) spindle stage analysis using PLM to determine whether individual fibers and bundles of the samples were polycrystalline or single-crystal cleavage fragments. The overall findings of the study indicated that the material is tremolite asbestos with characteristics substantially similar to the earlier distributed HSL reference material. A larger quantity of material was prepared by sorting, acid-washing and mixing for sub-division into vials of ~10g each. These vials have been transferred from NIOSH to RTI International, from where they can be obtained on request.

Characterization of Lone Pine, California, Tremolite Asbestos and Preparation of Research Material

PubMed Central

Harper, Martin; Van Gosen, Bradley; Crankshaw, Owen S.; Doorn, Stacy S.; Ennis, Todd J.; Harrison, Sara E.

2016-01-01

Well-characterized amphibole asbestos mineral samples are required for use as analytical standards and in future research projects. Currently, the National Institute for Standards and Technology Standard Reference Material samples of asbestos are listed as ‘Discontinued’. The National Institute for Occupational Safety and Health (NIOSH) has a goal under the Asbestos Roadmap of locating and characterizing research materials for future use. Where an initial characterization analysis determines that a collected material is appropriate for use as a research material in terms of composition and asbestiform habit, sufficient amounts of the material will be collected to make it publicly available. An abandoned mine near Lone Pine, California, contains a vein of tremolite asbestos, which was the probable source of a reference material that has been available for the past 17 years from the Health and Safety Laboratory (HSL) in the UK. Newly collected fibrous vein material from this mine was analyzed at Research Triangle Institute (RTI International) with some additional analysis by the US Geological Survey’s Denver Microbeam Laboratory. The analysis at RTI International included: (i) polarized light microscopy (PLM) with a determination of principal optical properties; (ii) X-ray diffraction; (iii) transmission electron microscopy, including energy dispersive X-ray spectroscopy and selected-area electron diffraction; and (iv) spindle stage analysis using PLM to determine whether individual fibers and bundles of the samples were polycrystalline or single-crystal cleavage fragments. The overall findings of the study indicated that the material is tremolite asbestos with characteristics substantially similar to the earlier distributed HSL reference material. A larger quantity of material was prepared by sorting, acid-washing and mixing for sub-division into vials of ~10 g each. These vials have been transferred from NIOSH to RTI International, from where they can be obtained on request. PMID:25268000

Biological and environmental reference materials in CENAM.

PubMed

Arvizu-Torres, R; Perez-Castorena, A; Salas-Tellez, J A; Mitani-Nakanishi, Y

2001-06-01

Since 1994, when the NIST/NOAA Quality Assurance Program in Chemical Measurements was discussed in Queretaro, CENAM, the National Measurement Institute (NMI) of Mexico, has become involved in the development of reference materials. In the field of biological and environmental reference materials, in particular, the NORAMET collaboration program with NIST and NRC, and the North-American Environmental Cooperation signed among three free-trade treaty organizations, have greatly helped the development of the materials metrology program in the newly established CENAM. This paper describes some particularly significant efforts of CENAM in the development of biological and environmental reference materials, on the basis of inter-comparison studies organized with local and governmental environmental agencies of Mexico. In the field of water pollution CENAM has developed a practical proficiency testing (PT) scheme for field laboratories, as a part of registration by local government in the metropolitan area, according to the Mexican Ecological Regulation. The results from these eight PTs in the last 5 years have demonstrated that this scheme has helped ensure the reliability of analytical capability of more than 50 field laboratories in three states, Mexico, D.F., and the States of Mexico and Queretaro. Similar experience has been obtained for more than 70 service units of stack emission measurements in the three states in 1998 and 1999, as a result of the design of a PT scheme for reference gas mixtures. This PT scheme has been accomplished successfully by 30 analytical laboratories who provide monitoring services and perform research on toxic substances (Hg, methylmercury, PCB, etc.) in Mexico. To support these activities, reference samples have been produced through the NIST SRMs, and efforts have been made to increase CENAM's capability in the preparation of primary reference materials in spectrometric solutions and gas mixtures. Collaboration among NMIs has also successfully overcome the inability of CENAM to prepare biological tissue for mercury assessment and marine sediments for analysis of trace metals. The importance of international collaboration is stressed not only in the NORAMET region but also in the SIM, to provide help for each other and achieve mutual recognition among member countries of the region.

[Report of the NEDO project "Research and development to promote the creation and utilization of an intellectual infrastructure: development of reference materials for laboratory medicine" "Development of pure substance-type certified reference materials"].

PubMed

Takatsu, Akiko

2009-06-01

There is an increasing demand to establish a metrological traceability system for in vitro diagnostics and medical devices. Pure substance-type reference materials are playing key roles in metrological traceability, because they form the basis for many traceability chains in chemistry. The National Metrology Institute of Japan (NMIJ), in the National Institute of Advanced Industrial Science and Technology (AIST), has been developing purity-certified reference materials (CRMs) in this field, such as cholesterol, creatinine, and urea. In the New Energy and Industrial Technology Development Organization (NEDO) project, entitled: "Research and Development to Promote the Creation and Utilization of an Intellectual Infrastructure: Development of Reference Materials for Laboratory Medicine", several pure substance-type CRMs were developed. For a pure protein solution CRM, amino acid analysis and nitrogen determination were chosen as the certification methods. The development and certification processes for the C-reactive protein (CRP) solution CRM were completed, with the recombinant human CRP solution as a candidate material. This CRP solution CRM is now available as NMIJ CRM. For cortisol CRM, a purified candidate material and highly pure primary reference material were prepared. Each impure compound in the materials was identified and quantified. The pure cortisol CRM will be available in 2009. These two CRMs provide a traceability link between routine clinical methods and the SI unit.

Preparation of a sewage sludge laboratory quality control material for butyltin compounds and their determination by isotope-dilution mass spectrometry.

PubMed

Zuliani, Tea; Milačič, Radmila; Ščančar, Janez

2012-05-01

The characterisation of a laboratory quality control material (QCM) for dibutyltin (DBT) and tributyltin (TBT) in sewage sludge is described. The reference values were determined by the use of two different types of isotope-dilution mass spectrometry: gas chromatography-mass spectrometry and gas chromatography-inductively coupled plasma mass spectrometry. To avoid possible analytical errors such as non-quantitative extraction and species degradation during sample preparation, different extraction methods were tested (microwave- and ultrasound-assisted extraction and mechanical stirring). The reference values were based on the unweighted means of results from the homogenisation and characterisation studies. The reference values obtained were 1,553 ± 87 and 534 ± 38 ng Sn g(-1) for DBT and TBT, respectively. In the uncertainty budget estimation, the sample inhomogeneity and between-method imprecision were taken into account. The concentrations of DBT and TBT in QCM are similar to those in the harbour sediment certified reference material PACS-2. Likewise, the levels of DBT and TBT are in the range of these compounds normally present in sewage sludge worldwide. In the future, the QCM will be used for an intercomparison study on DBT and TBT in sewage sludge, and as a day-to-day QCM during studies concerning the application of sewage sludge as an additive to artificial soil or as a raw material in civil engineering construction.

National and international veterinary reference laboratories for infectious diseases.

PubMed

Edwards, S; Alexander, D

1998-08-01

Reference laboratories play an increasingly important role in the harmonisation of laboratory diagnostic tests and the standardisation of veterinary vaccines. This is particularly important in building confidence between international trading partners. The authors review aspects of the organisation, designation and support of reference laboratories for infectious diseases of animals and discuss the principal activities which such laboratories would normally perform. These activities include advice and consultancy, publications and communication, training, research, disease surveillance, maintenance of culture collections, evaluation of reference methods, preparation of reference materials and organisation of inter-laboratory comparisons.

Preparation of candidate reference materials for the determination of phosphorus containing flame retardants in styrene-based polymers.

PubMed

Roth, Thomas; Urpi Bertran, Raquel; Latza, Andreas; Andörfer-Lang, Katrin; Hügelschäffer, Claudia; Pöhlein, Manfred; Puchta, Ralph; Placht, Christian; Maid, Harald; Bauer, Walter; van Eldik, Rudi

2015-04-01

Candidate reference materials (RM) for the analysis of phosphorus-based flame retardants in styrene-based polymers were prepared using a self-made mini-extruder. Due to legal requirements of the current restriction for the use of certain hazardous substances in electrical and electronic equipment, focus now is placed on phosphorus-based flame retardants instead of the brominated kind. Newly developed analytical methods for the first-mentioned substances also require RMs similar to industrial samples for validation and verification purposes. Hence, the prepared candidate RMs contained resorcinol-bis-(diphenyl phosphate), bisphenol A bis(diphenyl phosphate), triphenyl phosphate and triphenyl phosphine oxide as phosphorus-based flame retardants. Blends of polycarbonate and acrylonitrile-co-butadiene-co-styrene as well as blends of high-impact polystyrene and polyphenylene oxide were chosen as carrier polymers. Homogeneity and thermal stability of the candidate RMs were investigated. Results showed that the candidate RMs were comparable to the available industrial materials. Measurements by ICP/OES, FTIR and NMR confirmed the expected concentrations of the flame retardants and proved that analyte loss and degradation, respectively, was below the uncertainty of measurement during the extrusion process. Thus, the candidate RMs were found to be suitable for laboratory use.

Biscayne aquifer drinking water (USGS45): a new isotopic reference material for δ2H and δ18O measurements of water

USGS Publications Warehouse

Lorenz, Jennifer M.; Tarbox, Lauren V.; Buck, Bryan; Qi, Haiping; Coplen, Tyler B.

2014-01-01

RATIONALE As a result of the scarcity of isotopic reference waters for daily use, a new secondary isotopic reference material for international distribution has been prepared from drinking water collected from the Biscayne aquifer in Ft. Lauderdale, Florida. METHODS This isotopic reference water was filtered, homogenized, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and measured by dual-inlet isotope-ratio mass spectrometry. This reference material is available by the case of 144 glass ampoules containing either 4 mL or 5 mL of water in each ampoule. RESULTS The δ2H and δ18O values of this reference material are –10.3 ± 0.4 ‰ and –2.238 ± 0.011 ‰, respectively, relative to VSMOW, on scales normalized such that the δ2H and δ18O values of SLAP reference water are, respectively, –428 and –55.5 ‰. Each uncertainty is an estimated expanded uncertainty (U = 2uc) about the reference value that provides an interval that has about a 95 % probability of encompassing the true value. CONCLUSIONS This isotopic reference material, designated as USGS45, is intended as one of two isotopic reference waters for daily normalization of stable hydrogen and oxygen isotopic analysis of water with an isotope-ratio mass spectrometer or a laser absorption spectrometer. 

Spent Nuclear Fuel (SNF) Project Canister Storage Building (CSB) Process Flow Diagram Mass Balance Calculations

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

KLEM, M.J.

2000-05-11

The purpose of these calculations is to develop the material balances for documentation of the Canister Storage Building (CSB) Process Flow Diagram (PFD) and future reference. The attached mass balances were prepared to support revision two of the PFD for the CSB. The calculations refer to diagram H-2-825869.

The preparation of uranium-adsorbed silica particles as a reference material for the fission track analysis

NASA Astrophysics Data System (ADS)

Park, Y. J.; Lee, M. H.; Pyo, H. Y.; Kim, H. A.; Sohn, S. C.; Jee, K. Y.; Kim, W. H.

2005-06-01

Uranium-adsorbed silica particles were prepared as a reference material for the fission track analysis (FTA) of swipe samples. A modified instrumental setup for particle generation, based on a commercial vibrating orifice aerosol generator to produce various sizes of droplets from a SiO 2 solution, is described. The droplets were transferred into a weak acidic solution bath to produce spherical solid silica particles. The classification of the silica particles in the range from 5 to 20 μm was carried out by the gravitational sedimentation method. The size distribution and morphology of the classified silica particles were investigated by scanning electron microscopy. The physicochemical properties of the classified silica particles such as the surface area, pore size and pore volume were measured. After an adsorption of 5% 235U on the silica particles in a solution adjusted to pH 4.5, the uranium-adsorbed silica particles were calcined up to 950 °C in a furnace to fix the uranium strongly onto the silica particles. The various sizes of uranium-adsorbed silica particles were applied to the FTA for use as a reference material.

Standard Reference Materials (SRMs) for the Calibration and Validation of Analytical Methods for PCBs (as Aroclor Mixtures)

PubMed Central

Poster, Dianne L.; Schantz, Michele M.; Leigh, Stefan D.; Wise, Stephen A.

2004-01-01

Six Standard Reference Materials (SRMs®) have been prepared by the National Institute of Standards and Technology (NIST) for the determination of PCBs as different Aroclor mixtures in methanol. Six additional SRMs of the same Aroclors in transformer oil have also been prepared. Specifically, solutions of Aroclors 1016, 1232, 1242, 1254, and 1260 have been gravimetrically prepared (individually) in methanol and transformer oil, mixed, and transferred to amber glass ampoules in approximately 1.2 mL aliquots. Gas chromatography with electron capture detection (GC-ECD) has been used to verify the gravimetric data for each solution and transformer oil SRM. Liquid chromatography was used for the isolation of the Aroclors from the transformer oil SRMs prior to GC-ECD analysis. Separate calibration solutions and oils were prepared with Aroclor levels similar to those in each methanol solution and transformer oil SRM and were processed alongside the samples. The GC-ECD response of each Aroclor was monitored relative to internal standards that were added to the complex mixtures for quantification. The gravimetric concentrations of Aroclors 1242 and 1254 in methanol were also examined by the same method of analysis (GC-ECD) using several different sources of Aroclors and two different capillary GC columns: a 5 % phenyl methylpolysiloxane phase and a relatively non-polar phase. The preparation of the materials, the gas chromatographic results, and the certified concentration values for each Aroclor SRM are described in this paper. PMID:27366608

[Hygienic study and evaluation of textile materials with reduced combustibility with reference to the use of the new anti-inflammable preparations Pyrofix 2 and Torflam].

PubMed

Uzunova, S; Baĭnova, A; Iordanova, I; Dolova, D

1986-01-01

The new anti-flammable preparations, proposed by the Higher Chemical Technology Institute (Sofia), were studied, namely: Pyrofix 2--for treatment of textile materials and Torflam--for production of anti-inflammable polyester fibres. The following parameters were studied: skin-irritating and skin-sensitizing effect of both preparations, skin toxic effect of Pyrofix 2 and migration of chemicals from the anti-inflammable textile materials (from the composition of the preparations used). The results obtained revealed the absence of skin-irritating and skin-sensitizing effect of both preparations and cumulative dermal toxicity of Pyrofix 2. The textile materials with reduced combustibility are chemically stable and do not release compounds in the contact aqueous medium, imitating the underclothes space. Formaldehyde from recipe for the treatment of Pyrofix 2 migrates in the air environment. In conclusion, Pyrofix 2 could be applied for the final anti-inflammable treatment of the textile materials for industrial needs, working garments and everyday textile (with the elimination of formaldehyde compound from the recipe). Torflam could be used in the production of anti-inflammable polyester fibres for textile materials intended for industry and everyday life without immediate contact with the skin of the consumers.

Individualized Study Guide on Apiculture: Instructor's Guide. Curriculum Materials for Agricultural Education.

ERIC Educational Resources Information Center

Housmam, John L.; And Others

The instructor's guide is coordinated for use with the student guide. The guide includes suggestions for teacher preparation, equipment and supply needs, suggested references, available audiovisual materials, open-ended questions for classroom discussion, educational opportunities for students, and a form for student evaluation of the study guide.…

Preparation of waterproof OSL dosimeters from hygroscopic materials with a special reference to NaCl:Cu

NASA Astrophysics Data System (ADS)

More, Y. K.; Wankhede, S. P.; Patil, R. R.; Kulkarni, M. S.; Kumar, Munish; Moharil, S. V.

2016-05-01

Optically stimulated luminescence (OSL) originally developed for geological/archaeological dating, has been found very useful for diverse applications in the field of radiation dosimetry. There is still a scarcity of OSL materials with demonstrated properties suited to dosimetry applications. Progress on the development of OSL materials with engineered properties has been slow and most research has focused on the OSL characterization of existing materials. One of the reasons for availability of only a handful of OSL dosimetry materials with adequate properties is that they have to satisfy certain stringent conditions necessary for such applications. Especially, hygroscopic materials are considered totally unsuitable. The efforts were made in our laboratory to overcome this problem. It is shown here that "water-proof" dosimeters can be prepared from even hygroscopic materials such as NaCl.

Preparing for Twins

MedlinePlus

... Ribbon Commands Skip to main content Turn off Animations Turn on Animations Our Sponsors Log in | Register Menu Log in | ... challenges with twins. He also can suggest helpful reading material or refer you to organizations that help ...

[Discussion on Technical Evaluation for Medical Device Registration Material].

PubMed

Chu, Yungao; Qian, Hong; Zhu, Yingfeng

2017-07-30

This article first introduces the main contents of the requirements for medical device registration. Secondly, this article chooses the vertebral forming surgery system as an example to discuss the technical evaluation for the registration research material. The article hopes to provide a reference for the applicant who prepare the registration material and the technical evaluator who make the evaluation for the medical device registration.

An approach to shortening the timeframe between the emergence of new compounds on the drugs market and the availability of reference standards: The microscale syntheses of nitrazolam and clonazolam for use as reference materials, utilizing polymer-supported reagents.

PubMed

Dowling, Geraldine; Kavanagh, Pierce V; Eckhardt, Hans-Georg; Twamley, Brendan; Hessman, Gary; McLaughlin, Gavin; O'Brien, John; Brandt, Simon D

2018-03-15

Nitrazolam and clonazolam are 2 designer benzodiazepines available from Internet retailers. There is growing evidence suggesting that such compounds have the potential to cause severe adverse events. Information about tolerability in humans is scarce but typically, low doses can be difficult to administer for users when handling bulk material. Variability of the active ingredient in tablet formulations can also be of a concern. Customs, toxicology and forensic laboratories are increasingly encountering designer benzodiazepines, both in tablet and powdered form. The unavailability of reference standards can impact on the ability to identify these compounds. Therefore, the need arises for exploring in-house approaches to the preparation of new psychoactive substances (NPS) that can be carried out in a timely manner. The present study was triggered when samples of clonazolam were received in powdered and tablet form at a time when reference material for this drug was commercially unavailable. Therefore, microscale syntheses of clonazolam and its deschloro analog nitrazolam were developed utilizing polymer-supported reagents starting from 2-amino-2'-chloro-5-nitrobenzophenone (clonazolam) and 2-amino-5-nitrobenzophenone (nitrazolam). The final reaction step forming the 1,2,4-triazole ring moiety was performed within a gas chromatography-mass spectrometry (GC-MS) injector. A comparison with a preparative scale synthesis of both benzodiazepine derivatives showed that microscale synthesis might be an attractive option for a forensic laboratory in terms of time and cost savings when compared with traditional methods of synthesis and when qualitative identifications are needed to direct forensic casework. The reaction by-product profiles for both the micro and the preparative scale syntheses are also presented. Copyright © 2018 John Wiley & Sons, Ltd.

The development and certification of Standard Reference Materials (SRMs) to assess and ensure accurate measurement of Pb in the environment.

PubMed

Fassett, J D; MacDonald, B S

2001-08-01

The National Institute of Standards and Technology (NIST) has had a major quality-assurance role in the federal effort to reduce lead poisoning of children in the United States through its mission of ensuring the accuracy of chemical measurements. NIST certifies reference materials (standard reference materials--SRMs) that are used to benchmark measurements by secondary and field methods of analysis--to ensure that decisions of great health and economic impact are soundly based on good measurement science. Over the past 10 years, in cooperation with the US Environmental Protection Agency (EPA), US Department of Housing and Urban Development (HUD), and the United States Geological Survey (USGS), NIST has prepared and certified SRMs for lead content in soil, indoor dust, and paint. The role of these materials in meeting regulatory and abatement needs is described and their certified values are summarized.

Aluminium-gold reference material for the k0-standardisation of neutron activation analysis

NASA Astrophysics Data System (ADS)

Ingelbrecht, C.; Peetermans, F.; De Corte, F.; De Wispelaere, A.; Vandecasteele, C.; Courtijn, E.; D'Hondt, P.

1991-05-01

Gold is an excellent comparator material for the k0-standardisation of neutron activation analysis because of its convenient and well defined nuclear properties. The most suitable form for a reference material is a dilute aluminium-gold alloy, for which the self-shielding effect for neutrons is small. Castings of composition Al-0.1 wt.% Au were prepared by crucible-less levitation melting, which gives close control of ingot composition with minimal contamination of the melt. The alloy composition was checked using induction-coupled plasma source emission spectrometry. The homogeneity of the alloy was measured by neutron activation analysis and a relative standard deviation of the gold content of 0.30% was found (10 mg samples). Metallography revealed a homogeneous distribution of AuAl 2 particles. The alloy was certified as Reference Material CBNM-530, with certified gold mass fraction 0.100±0.002 wt.%.

Advanced Curation Activities at NASA: Preparing to Receive, Process, and Distribute Samples Returned from Future Missions

NASA Technical Reports Server (NTRS)

McCubbin, Francis M.; Zeigler, Ryan A.

2017-01-01

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F JSC is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. The Directive goes on to define Curation as including documentation, preservation, preparation, and distribution of samples for research, education, and public outreach. Here we briefly describe NASA's astromaterials collections and our ongoing efforts related to enhancing the utility of our current collections as well as our efforts to prepare for future sample return missions. We collectively refer to these efforts as advanced curation.

Programmable frequency reference for subkilohertz laser stabilization by use of persistent spectral hole burning.

PubMed

Sellin, P B; Strickland, N M; Carlsten, J L; Cone, R L

1999-08-01

We report what is believed to be the first demonstration of laser frequency stabilization directly to persistent spectral holes in a solid-state material. The frequency reference material was deuterated CaF(2): Tm(3+) prepared with 25-MHz-wide persistent spectral holes on the H(6)(3)?H(4)(3) transition at 798 nm. The beat frequency between two lasers that were independently locked to persistent spectral holes in separate crystal samples showed typical root Allan variances of 780+/-120Hz for 20-50-ms integration times.

Determination of polychlorinated biphenyl congeners and chlorinated pesticides in a fish tissue standard reference material.

PubMed

Poster, Dianne L; Kucklick, John R; Schantz, Michele M; Porter, Barbara J; Leigh, Stefan D; Wise, Stephen A

2003-01-01

The concentrations of a wide range of polychlorinated biphenyl congeners (PCBs) and chlorinated pesticides in a fish tissue Standard Reference Material (SRM) have been determined using multiple methods of analysis. This material, SRM 1946, Lake Superior Fish Tissue, was recently issued by the National Institute of Standards and Technology (NIST) and complements a suite of marine environmental natural-matrix SRMs that are currently available from NIST for the determination of organic contaminants such as aliphatic hydrocarbons, polycyclic aromatic hydrocarbons (PAHs), PCBs, and chlorinated pesticides. SRM 1946 is a fresh tissue homogenate (frozen) prepared from filleted adult lake trout (Salvelinus namaycush namaycush) collected from the Apostle Islands region of Lake Superior. SRM 1946 has certified and reference concentrations for PCB congeners, including the three non- ortho PCB congeners, and chlorinated pesticides. Certified concentrations are available for 30 PCB congeners and 15 chlorinated pesticides. Reference concentrations are available for 12 PCB congeners and 2 chlorinated pesticides. In addition, SRM 1946 is characterized for additional chemical constituents and properties: fatty acids, extractable fat, methylmercury, total mercury, selected trace elements, proximates, and caloric content. The characterization of chlorinated compounds is described in this paper with an emphasis on the approach used for the certification of the concentrations of PCB congeners and chlorinated pesticides. The PCB congener and chlorinated pesticide data are also compared to concentrations in other marine natural-matrix reference materials available from NIST (fish oil, mussel tissue, whale blubber, and a second fresh frozen fish tissue homogenate prepared from filleted adult lake trout collected from Lake Michigan) and from other organizations such as the National Research Council Canada (ground whole carp), the International Atomic Energy Agency (fish homogenate), and the European Commission Joint Research Centre [fish oils (cod and mackerel) and mussel tissue].

Effects of preparation process on performance of rubber modified asphalt

NASA Astrophysics Data System (ADS)

Liu, Hanbing; Luo, Guobao; Wang, Xianqiang; Jiao, Yubo

2015-06-01

The rational utilization of waste rubber tire is essential for the environmental protection. Utilizing rubber particles to modify asphalt can not only improve asphalt performance, but also help the recycling of waste materials. Considering the effect of different preparation process parameters on the performance of rubber modified asphalt, this paper analyzes the effects of the shear temperature, shear time and shear rate on the performance of rubber modified asphalt, and provided a reference for its preparation.

Fibrinolysis standards: a review of the current status.

PubMed

Thelwell, C

2010-07-01

Biological standards are used to calibrate measurements of components of the fibrinolytic system, either for assigning potency values to therapeutic products, or to determine levels in human plasma as an indicator of thrombotic risk. Traditionally WHO International Standards are calibrated in International Units based on consensus values from collaborative studies. The International Unit is defined by the response activity of a given amount of the standard in a bioassay, independent of the method used. Assay validity is based on the assumption that both standard and test preparation contain the same analyte, and the response in an assay is a true function of this analyte. This principle is reflected in the diversity of source materials used to prepare fibrinolysis standards, which has depended on the contemporary preparations they were employed to measure. With advancing recombinant technology, and improved analytical techniques, a reference system based on reference materials and associated reference methods has been recommended for future fibrinolysis standards. Careful consideration and scientific judgement must however be applied when deciding on an approach to develop a new standard, with decisions based on the suitability of a standard to serve its purpose, and not just to satisfy a metrological ideal. 2010 The International Association for Biologicals. Published by Elsevier Ltd. All rights reserved.

Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation.

PubMed

Chopade, Sujay A; Anderson, Evan L; Schmidt, Peter W; Lodge, Timothy P; Hillmyer, Marc A; Bühlmann, Philippe

2017-10-27

Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.

Preparation and certification of Re-Os dating reference materials: Molybdenites HLP and JDC

USGS Publications Warehouse

Du, A.; Wu, S.; Sun, D.; Wang, Shaoming; Qu, W.; Markey, R.; Stain, H.; Morgan, J.; Malinovskiy, D.

2004-01-01

Two Re-Os dating reference material molybdenites were prepared. Molybdenite JDC and molybdenite HLP are from a carbonate vein-type molybdenum-(lead)- uranium deposit in the Jinduicheng-Huanglongpu area of Shaanxi province, China. The samples proved to be homogeneous, based on the coefficient of variation of analytical results and an analysis of variance test. The sampling weight was 0.1 g for JDC and 0.025 g for HLP. An isotope dilution method was used for the determination of Re and Os. Sample decomposition and preconcentration of Re and Os prior to measurement were accomplished using a variety of methods: acid digestion, alkali fusion, ion exchange and solvent extraction. Negative thermal ionisation mass spectrometry and inductively coupled plasma-mass spectrometry were used for the determination of Re and 187Os concentration and isotope ratios. The certified values include the contents of Re and Os and the model ages. For HLP, the Re content was 283.8 ?? 6.2 ??g g-1, 187Os was 659 ?? 14 ng g-1 and the Re-Os model age was 221.4 ?? 5.6 Ma. For JDC, the Re content was 17.39 ?? 0.32 ng g-1, 187Os was 25.46 ?? 0.60 ng g-1 and the Re-Os model age was 139.6 ?? 3.8 Ma. Uncertainties for both certified reference materials are stated at the 95% level of confidence. Three laboratories (from three countries: P.R. China, USA, Sweden) joined in the certification programme. These certified reference materials are primarily useful for Re-Os dating of molybdenite, sulfides, black shale, etc.

Preparation of waterproof OSL dosimeters from hygroscopic materials with a special reference to NaCl:Cu

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

More, Y. K., E-mail: moreyogesh153@gmail.com; Moharil, S. V.; Wankhede, S. P.

Optically stimulated luminescence (OSL) originally developed for geological/archaeological dating, has been found very useful for diverse applications in the field of radiation dosimetry. There is still a scarcity of OSL materials with demonstrated properties suited to dosimetry applications. Progress on the development of OSL materials with engineered properties has been slow and most research has focused on the OSL characterization of existing materials. One of the reasons for availability of only a handful of OSL dosimetry materials with adequate properties is that they have to satisfy certain stringent conditions necessary for such applications. Especially, hygroscopic materials are considered totally unsuitable.more » The efforts were made in our laboratory to overcome this problem. It is shown here that “water-proof” dosimeters can be prepared from even hygroscopic materials such as NaCl.« less

Synergy between hexavalent chromium ions and TiO2 nanoparticles inside TUD-1 in the photocatalytic oxidation of propane, a spectroscopic study

NASA Astrophysics Data System (ADS)

Hamdy, Mohamed S.

2016-02-01

Siliceous TUD-1 mesoporous material was bi-functionalized by titanium dioxide nanoparticles and hexavalent chromium ions. The synthesis was carried out by one-pot procedure based on sol-gel technique. The photocatalytic performance of the prepared material was evaluated in the oxidation of propane under the illumination of ultraviolet light (wavelength = 360 nm) and monitored by in situ Fourier transform infrared spectroscopy. The photocatalytic activity of the prepared material exhibited an extra-ordinary activity than the reference samples that contain either hexavalent chromium ions or titanium dioxide nanoparticles only, confirming the true synergy between hexavalent chromium and tetravalent titanium ions of titanium dioxide nanoparticles.

Preparation and certification of hijiki reference material, NMIJ CRM 7405-a, from the edible marine algae hijiki (Hizikia fusiforme).

PubMed

Narukawa, Tomohiro; Inagaki, Kazumi; Zhu, Yanbei; Kuroiwa, Takayoshi; Narushima, Izumi; Chiba, Koichi; Hioki, Akiharu

2012-02-01

A certified reference material, NMIJ CRM 7405-a, for the determination of trace elements and As(V) in algae was developed from the edible marine hijiki (Hizikia fusiforme) and certified by the National Metrology Institute of Japan (NMIJ), the National Institute of Advanced Industrial Science and Technology (AIST). Hijiki was collected from the Pacific coast in the Kanto area of Japan, and was washed, dried, powdered, and homogenized. The hijiki powder was placed in 400 bottles (ca. 20 g each). The concentrations of 18 trace elements and As(V) were determined by two to four independent analytical techniques, including (ID)ICP-(HR)MS, ICP-OES, GFAAS, and HPLC-ICP-MS using calibration solutions prepared from the elemental standard solution of Japan calibration service system (JCSS) and the NMIJ CRM As(V) solution, and whose concentrations are certified and SI traceable. The uncertainties of all the measurements and preparation procedures were evaluated. The values of 18 trace elements and As(V) in the CRM were certified with uncertainty (k = 2).

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

PubMed

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

2002-01-01

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

Development of a candidate reference measurement procedure for the analysis of cortisol in human serum samples by isotope dilution-gas chromatography-mass spectrometry.

PubMed

Kawaguchi, Migaku; Takatsu, Akiko

2009-08-01

A candidate reference measurement procedure involving isotope dilution coupled with gas chromatography-mass spectrometry (GC-MS) has been developed and critically evaluated. An isotopically labeled internal standard, cortisol-d(2), was added to a serum sample. After equilibration, solid-phase extractions (SPE) for sample preparation and derivatization with heptafluorobutyric anhydride (HFBA) were performed for GC-MS analysis. The limit of detection (LOD) and the limit of quantification (LOQ) were 5 and 20 ng g(-1), respectively. The recovery of the added cortisol ranged from 99.8 to 101.0%. Excellent precision was obtained with a within-day variation (RSD) of 0.7% for GC-MS analysis. The accuracy of the measurement was evaluated by comparing of results of this reference measurement procedure on lyophilized human serum reference materials for cortisol (European Reference Materials (ERM)-DA 192) as Certified Reference Materials (CRMs). The results of this method for total cortisol agreed with the certified values within some uncertainty. This method, which demonstrates simply, easy, good accuracy, high precision, and is free from interferences from structural analogues, qualifies as a reference measurement procedure.

Transparent Conducting Oxides—An Up-To-Date Overview

PubMed Central

Stadler, Andreas

2012-01-01

Transparent conducting oxides (TCOs) are electrical conductive materials with comparably low absorption of electromagnetic waves within the visible region of the spectrum. They are usually prepared with thin film technologies and used in opto-electrical apparatus such as solar cells, displays, opto-electrical interfaces and circuitries. Here, based on a modern database-system, aspects of up-to-date material selections and applications for transparent conducting oxides are sketched, and references for detailed information are given. As n-type TCOs are of special importance for thin film solar cell production, indium-tin oxide (ITO) and the reasonably priced aluminum-doped zinc oxide (ZnO:Al), are discussed with view on preparation, characterization and special occurrences. For completion, the recently frequently mentioned typical p-type delafossite TCOs are described as well, providing a variety of references, as a detailed discussion is not reasonable within an overview publication. PMID:28817002

Preparation and stability of milk somatic cell reference materials.

PubMed

Di Marzo, Larissa; Wojciechowski, Karen L; Barbano, David M

2016-09-01

Our objectives were to develop a method to produce milk somatic cell count (SCC) reference materials for calibration of electronic somatic cell count (ESCC) using gravity separation and to determine the effect of refrigerated storage (4°C) and freeze-thaw stability of the skim and whole milk SCC reference materials. Whole raw milk was high-temperature short-time pasteurized and split into 2 portions. One portion was gravity separated at 4°C for 22 h and the second portion was centrifugally separated to produce skim milk that was also gravity separated with somatic cells rising to the surface. After 22 h, stock solutions (low SCC skim milk, high SCC skim milk, high SCC whole milk) were prepared and preserved (bronopol). Two experiments were conducted, one to compare the shelf-life of skim and whole milk SCC standards at 4°C and one to determine the effect of freezing and thawing on SCC standards. Both experiments were replicated 3 times. Gravity separation was an effective approach to isolate and concentrate somatic cells from bovine milk and redistribute them in a skim or whole milk matrix to create a set of reference materials with a wider and more uniformly distributed range of SCC than current calibration sets. The liquid SCC reference materials stored using the common industry practice at 4°C were stable (i.e., fit for purpose, no large decrease in SCC) for a 2-wk period, whereas frozen and thawed reference materials may have a much longer useful life. A gradual decrease occurred in residual difference in ESCC (SCC × 1,000/mL) versus original assigned reference SCC over duration of refrigerated storage for both skim and whole milk SCC samples, indicating that milk ESCC of the preserved milks was gradually decreasing during 28 d of storage at 4°C by about 15,000 SCC/mL. No difference in the ESCC for skim milk was detected between refrigerated and frozen storage, whereas for whole milk the ESCC for frozen was lower than refrigerated samples. Future work is needed to determine the time and temperature of longer term frozen storage over which the SCC results are stable. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Preparation, certification and validation of a stable solid spike of uranium and plutonium coated with a cellulose derivative for the measurement of uranium and plutonium content in dissolved nuclear fuel by isotope dilution mass spectrometry.

PubMed

Surugaya, Naoki; Hiyama, Toshiaki; Verbruggen, André; Wellum, Roger

2008-02-01

A stable solid spike for the measurement of uranium and plutonium content in nitric acid solutions of spent nuclear fuel by isotope dilution mass spectrometry has been prepared at the European Commission Institute for Reference Materials and Measurements in Belgium. The spike contains about 50 mg of uranium with a 19.838% (235)U enrichment and 2 mg of plutonium with a 97.766% (239)Pu abundance in each individual ampoule. The dried materials were covered with a thin film of cellulose acetate butyrate as a protective organic stabilizer to resist shocks encountered during transportation and to eliminate flaking-off during long-term storage. It was found that the cellulose acetate butyrate has good characteristics, maintaining a thin film for a long time, but readily dissolving on heating with nitric acid solution. The solid spike containing cellulose acetate butyrate was certified as a reference material with certified quantities: (235)U and (239)Pu amounts and uranium and plutonium amount ratios, and was validated by analyzing spent fuel dissolver solutions of the Tokai reprocessing plant in Japan. This paper describes the preparation, certification and validation of the solid spike coated with a cellulose derivative.

Development of a Novel Leak-Free Constant-Pressure Cylinder for Certified Reference Materials of Liquid Hydrocarbon Mixtures.

PubMed

Kim, Yong Doo; Kang, Ji Hwan; Bae, Hyun Kil; Kang, Namgoo; Oh, Sang Hyub; Lee, Jin-Hong; Woo, Jin Chun; Lee, Sangil

2017-11-21

Liquid hydrocarbon mixtures such as liquefied petroleum gas and liquefied natural gas are becoming integral parts of the world's energy system. Certified reference materials (CRMs) of liquid hydrocarbon mixtures are necessary to allow assessment of the accuracy and traceability of the compositions of such materials. A piston-type constant-pressure cylinder (PCPC) comprising chambers for a pressurizing gas (helium) and liquid (hydrocarbons) separated by a piston can be used to develop accurate and traceable liquid hydrocarbon mixture CRMs. The development of accurate CRMs relies on the maintenance of their composition. However, a PCPC might allow hydrocarbons to leak owing to the imperfect seal of the piston. In this study, a novel leak-free bellows-type constant-pressure cylinder (BCPC) is designed and evaluated by comparison with PCPCs. Liquid hydrocarbon mixtures consisting of ethane, propane, propene, isobutane, n-butane, 1-butene, and isopentane were prepared in both types of constant pressure cylinders and then monitored to check leakages between the gas and liquid chambers. Overall, notable leakage occurred from and into both chambers in the PCPCs, whereas no leakage occurred in the BCPCs in the three months after their gravimetric preparation. The BCPCs maintained no leakage even 10 months after their preparation, whereas the PCPCs showed significantly increasing leakage during the same period.

Development of new reference material neohesperidin for quality control of dietary supplements.

PubMed

Gong, Ningbo; Zhang, Baoxi; Yang, Dezhi; Gao, Zhaolin; Du, Guanhua; Lu, Yang

2015-07-01

Neohesperidin is an important natural flavanone glycoside distributed in several citrus species. This compound is widely used as a raw material for food additives in the food industry. The request for certified reference materials (CRMs) in dietary supplements was stipulated by the National Administrative Committee for CRMs and was underpinned by the need to improve the accuracy and comparability of measurement data and to establish metrological traceability of analytical results. This paper reports the sample preparation methodology, homogeneity and stability studies, value assignment and uncertainty estimation of a new certified reference material of neohesperidin (GBW09522). Differential scanning calorimetry, coulometric titration and mass balance methods proved to be sufficiently reliable and accurate for certification purposes. The certified value of neohesperidin CRM is 994 g kg(-1) with an expanded uncertainty of 4 g kg(-1) (k = 2). The reference material described above was homogeneous and stable for 12 months at a storage temperature of 25 °C. The new CRM of neohesperidin can be used to validate analytical methods and improve the accuracy of measurement data as well as quality control of neohesperidin-related dietary supplements, foods, traditional herbs and pharmaceutical formulations. © 2014 Society of Chemical Industry.

Preliminary Reports, Memoranda and Technical Notes of the Materials Research Council Summer Conference, La Jolla, California

DTIC Science & Technology

1983-07-01

Multilayer Thin Film materials M. S. Wrighton ...................................... 26 •.. Line Defects in Langmuir - Blodgett Films J. P. Hirth...of Langmuir and Blodgett can be used to prepare monolayers and multilayers of organic materials on a o, variety of substrates. The films of organic...references therein. * 2. Cf. Thin Solid Films, 99, (1982) from the proceedings of the "* . International Conference on Langmuir - Blodgett Films held

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

NASA Astrophysics Data System (ADS)

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

2010-04-01

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

Biscayne aquifer drinking water (USGS45): a new isotopic reference material for δ2H and δ18O measurements of water.

PubMed

Lorenz, Jennifer M; Tarbox, Lauren; Buck, Bryan; Qi, Haiping; Coplen, Tyler B

2014-10-15

As a result of the scarcity of isotopic reference waters for daily use, a new secondary isotopic reference material for international distribution has been prepared from drinking water collected from the Biscayne aquifer in Ft. Lauderdale, Florida. This isotopic reference water was filtered, homogenized, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and measured by dual-inlet isotope-ratio mass spectrometry. This reference material is available by the case of 144 glass ampoules containing either 4 mL or 5 mL of water in each ampoule. The δ(2)H and δ(18)O values of this reference material are -10.3 ± 0.4‰ and -2.238 ± 0.011‰, respectively, relative to VSMOW, on scales normalized such that the δ(2)H and δ(18)O values of SLAP reference water are, respectively, -428 and -55.5‰. Each uncertainty is an estimated expanded uncertainty (U = 2uc ) about the reference value that provides an interval that has about a 95% probability of encompassing the true value. This isotopic reference material, designated as USGS45, is intended as one of two isotopic reference waters for daily normalization of stable hydrogen and oxygen isotopic analysis of water with an isotope-ratio mass spectrometer or a laser absorption spectrometer. Published in 2014. This article is a U.S. Government work and is in the public domain in the USA. Published in 2014. This article is a U.S. Government work and is in the public domain in the USA.

USGS48 Puerto Rico precipitation - A new isotopic reference material for δ2H and δ18O measurements of water

USGS Publications Warehouse

Qi, Haiping; Coplen, Tyler B.; Tarbox, Lauren V.; Lorenz, Jennifer M.; Scholl, Martha A.

2014-01-01

A new secondary isotopic reference material has been prepared from Puerto Rico precipitation, which was filtered, homogenised, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and calibrated by dual-inlet isotope-ratio mass spectrometry. This isotopic reference material, designated as USGS48, is intended to be one of two isotopic reference waters for daily normalisation of stable hydrogen (δ2H) and stable oxygen (δ18O) isotopic analysis of water with a mass spectrometer or a laser absorption spectrometer. The δ2H and δ18O values of this reference water are−2.0±0.4 and−2.224±0.012 ‰, respectively, relative to Vienna Standard Mean Ocean Water on scales normalised such that the δ2H and δ18O values of Standard Light Antarctic Precipitation reference water are−428 and−55.5 ‰, respectively. Each uncertainty is an estimated expanded uncertainty (U=2uc) about the reference value that provides an interval that has about a 95 % probability of encompassing the true value. This isotopic reference water is available by the case of 144 glass ampoules containing 5 mL of water in each ampoule.

A new organic-rich soil reference material certified for its EDTA- and acetic acid- extractable contents of Cd, Cr, Cu, Ni, Pb and Zn, following collaboratively tested and harmonised procedures.

PubMed

Pueyo, M; Rauret, G; Bacon, J R; Gomez, A; Muntau, H; Quevauviller, P; López-Sánchez, J F

2001-02-01

There is an increasing requirement for assessment of the bioavailable metal fraction and the mobility of trace elements in soils upon disposal. One of the approaches is the use of leaching procedures, but the results obtained are operationally defined; therefore, their significance is highly dependent on the extraction protocol performed. So, for this type of study, there is a need for reference materials that allow the quality of measurements to be controlled. This paper describes the steps involved in the certification of an organic-rich soil reference material, BCR-700, for the EDTA- and acetic acid-extractable contents of some trace elements, following collaboratively tested and harmonised extraction procedures. Details are given for the preparation of the soil, homogeneity and stability testing, analytical procedures and the statistical selection of data to be included in the certification.

Rapid Radiochemical Methods for Asphalt Paving Material ...

EPA Pesticide Factsheets

Technical Brief Validated rapid radiochemical methods for alpha and beta emitters in solid matrices that are commonly encountered in urban environments were previously unavailable for public use by responding laboratories. A lack of tested rapid methods would delay the quick determination of contamination levels and the assessment of acceptable site-specific exposure levels. Of special concern are matrices with rough and porous surfaces, which allow the movement of radioactive material deep into the building material making it difficult to detect. This research focuses on methods that address preparation, radiochemical separation, and analysis of asphalt paving materials and asphalt roofing shingles. These matrices, common to outdoor environments, challenge the capability and capacity of very experienced radiochemistry laboratories. Generally, routine sample preparation and dissolution techniques produce liquid samples (representative of the original sample material) that can be processed using available radiochemical methods. The asphalt materials are especially difficult because they do not readily lend themselves to these routine sample preparation and dissolution techniques. The HSRP and ORIA coordinate radiological reference laboratory priorities and activities in conjunction with HSRP’s Partner Process. As part of the collaboration, the HSRP worked with ORIA to publish rapid radioanalytical methods for selected radionuclides in building material matrice

International reference reagents: antihuman globulin. An ISBT/ICSH joint working party report. International Society of Blood Transfusion. International Committee for Standardization in Haematology.

PubMed

Case, J; Ford, D S; Chung, A; Collins, R; Kochman, S; Mazda, T; Overbeeke, M; Perera, R; Sakuldamrongpanich, T; Scott, M; Voak, D; Zupańska, B

1999-01-01

An international working party has conducted a study designed to select a suitable reference reagent for antihuman globulin, to replace those first made available in 1987. The chosen preparation contains levels of anti-IgG and anti-C3 (anti-C3c and anti-C3d) potency that are considered suitable to serve for reference when evaluating either polyspecific antihuman globulin reagents or those containing their separate monospecific components. The reference material is available in 2-ml freeze-dried aliquots from seven assigned distribution centres.

Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation

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

Chopade, Sujay A.; Anderson, Evan L.; Schmidt, Peter W.

Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethylmore » sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.« less

Bibliography on the Design and Performance of Rail Track Structures

DOT National Transportation Integrated Search

1974-01-01

This bibliography was prepared as part of the Rail Supporting Technology Program being sponsored by the Rail Programs Branch of the Urban Mass Transportation Administration. It is based on the reference material that was used to evaluate the technica...

Certification of NIST standard reference material 2389a, amino acids in 0.1 mol/L HCl--quantification by ID LC-MS/MS.

PubMed

Lowenthal, Mark S; Yen, James; Bunk, David M; Phinney, Karen W

2010-05-01

An isotope-dilution liquid chromatography-tandem mass spectrometry (ID LC-MS/MS) measurement procedure was developed to accurately quantify amino acid concentrations in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 2389a-amino acids in 0.1 mol/L hydrochloric acid. Seventeen amino acids were quantified using selected reaction monitoring on a triple quadrupole mass spectrometer. LC-MS/MS results were compared to gravimetric measurements from the preparation of SRM 2389a-a reference material developed at NIST and intended for use in intra-laboratory calibrations and quality control. Quantitative mass spectrometry results and gravimetric values were statistically combined into NIST-certified mass fraction values with associated uncertainty estimates. Coefficients of variation (CV) for the repeatability of the LC-MS/MS measurements among amino acids ranged from 0.33% to 2.7% with an average CV of 1.2%. Average relative expanded uncertainty of the certified values including Types A and B uncertainties was 3.5%. Mean accuracy of the LC-MS/MS measurements with gravimetric preparation values agreed to within |1.1|% for all amino acids. NIST SRM 2389a will be available for characterization of routine methods for amino acid analysis and serves as a standard for higher-order measurement traceability. This is the first time an ID LC-MS/MS methodology has been applied for quantifying amino acids in a NIST SRM material.

Soliciting Strategies for Developing Cell-Based Reference Materials to Advance Mesenchymal Stromal Cell Research and Clinical Translation

PubMed Central

Viswanathan, Sowmya; Keating, Armand; Deans, Robert; Hematti, Peiman; Prockop, Darwin; Stroncek, David F.; Stacey, Glyn; Weiss, Dan J.; Mason, Christopher

2014-01-01

The mesenchymal stromal cell (MSC) field continues to rapidly progress with a number of clinical trials initiated and completed, with some reported successes in multiple clinical indications, and a growing number of companies established. The field, nevertheless, faces several challenges. Persistent issues include the definition of a MSC and comparability between MSC preparations. This is because of inherent cell heterogeneity, the absence of markers that are unique to MSCs, and the difficulty in precisely defining them by developmental origin. Differences in the properties of MSCs also depend on the site of tissue harvest, phenotypic and genotypic characteristics of the donor and the isolation, and storage and expansion methods used. These differences may be sufficient to ensure that attributes of the final MSC product could differ in potentially significant ways. Since there are currently no gold standards, we propose using a reference material to establish methods of comparability among MSC preparations. We suggest four possible “ruler scenarios” and a method for global distribution. We further suggest that critical to establishing a reference material is the need to define protocols for comparing cells. The main purpose of this article is to solicit input in establishing a consensus-based comparison. A comparative approach will be critical to all stages of translation to better clarify mechanisms of MSC actions, define an optimal cell manufacturing process, ensure best practice clinical investigations, extend the use of an MSC product for new indications, protect an MSC product from imitators, and develop uniform reimbursement policies. Importantly, a reference material may enable a consensus on a practical definition of MSCs. PMID:24422625

Characterizing a Full Spectrum of Physico-Chemical Properties of Ginsenosides Rb1 and Rg1 to Be Proposed as Standard Reference Materials

PubMed Central

Kim, Il-Woung; Hong, Hee-Do; Choi, Sang Yoon; Hwang, Da-Hye; Her, Youl; Kim, Si-Kwan

2011-01-01

Good manufacturing practice (GMP)-based quality control is an integral component of the common technical document, a formal documentation process for applying a marketing authorization holder to those countries where ginseng is classified as a medicine. In addition, authentication of the physico-chemical properties of ginsenoside reference materials, and qualitative and quantitative batch analytical data based on validated analytical procedures are prerequisites for certifying GMP. Therefore, the aim of this study was to propose an authentication process for isolated ginsenosides Rb1 and Rg1 as reference materials (RM) and for these compounds to be designated as RMs for ginseng preparations throughout the world. Ginsenoside Rb1 and Rg1 were isolated by Diaion HP-20 adsorption chromatography, silica gel flash chromatography, recrystallization, and preparative HPLC. HPLC fractions corresponding to those two ginsenosides were recrystallized in appropriate solvents for the analysis of physico-chemical properties. Documentation of the isolated ginsenosides was made according to the method proposed by Gaedcke and Steinhoff. The ginsenosides were subjected to analyses of their general characteristics, identification, purity, content quantitation, and mass balance tests. The isolated ginsenosides were proven to be a single compound when analyzed by three different HPLC systems. Also, the water content was found to be 0.940% for Rb1 and 0.485% for Rg1, meaning that the net mass balance for ginsenoside Rb1 and Rg1 were 99.060% and 99.515%, respectively. From these results, we could assess and propose a full spectrum of physicochemical properties for the ginsenosides Rb1 and Rg1 as standard reference materials for GMP-based quality control. PMID:23717096

[Preparation and characterization of follwing the national standard anti-Brucella abortus serum, bovine].

PubMed

Li, Cui; Guan, Fushi; Dai, Zhihong; Jiang, Hui; Wen, Fang; Lu, Lianshou; Wang, Zaishi

2011-05-01

To prepare anti-Brucella abortus serum used for calibrate the agglutination test follwing the national standard, 4 anti-Brucella abortus sera were obtained from 4 cows infected with Brucella abortus naturally. By potency testing, the third serum was selected. Sterility, vaccum degree, residual moisture, uniformity and stability of this standard material were tested and proved to meet the national standard. Referring to the international standard, RBT (Rose-Bengal plate agglutination test), SAT (standard tube agglutination) and CFT (complement fixation test) titers of this standard material were measured to be 1:160 "+" 1:2 400 "++" and 1:800 "++", which are identical with the collaborative assay results. International unit of the standard material is 4 000 IU/mL.

Antarctic ice-core water (USGS49) – A new isotopic reference material for δ2H and δ18O measurements of water

USGS Publications Warehouse

Lorenz, Jennifer M.; Qi, Haiping; Coplen, Tyler B.

2017-01-01

As a result of the scarcity of isotopic reference waters for daily use, a new secondary isotopic reference material for international distribution has been prepared from ice-core water from the Amundsen–Scott South Pole Station. This isotopic reference material, designated as USGS49, was filtered, homogenised, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity and measured by dual-inlet isotope-ratio mass spectrometry. The δ2H and δ18O values of USGS49 are −394.7 ± 0.4 and −50.55 ± 0.04 mUr (where mUr = 0.001 = ‰), respectively, relative to VSMOW, on scales normalised such that the δ2H and δ18O values of SLAP reference water are, respectively, −428 and −55.5 mUr. Each uncertainty is an estimated expanded uncertainty (U = 2uc) about the reference value that provides an interval that has about a 95% probability of encompassing the true value. This isotopic reference material is intended as one of two isotopic reference waters for daily normalisation of stable hydrogen and oxygen isotopic analysis of water with an isotope-ratio mass spectrometer or a laser absorption spectrometer. It is available by the case of 144 glass ampoules or as a set of sixteen glass ampoules containing 5 ml of water in each ampoule.

Validation of reference materials for uranium radiochronometry in the frame of nuclear forensic investigations

DOE PAGES

Varga, Z.; Mayer, K.; Bonamici, C. E.; ...

2015-05-11

The results of a joint effort by expert nuclear forensic laboratories in the area of age dating of uranium, i.e. the elapsed time since the last chemical purification of the material are presented and discussed. Completely separated uranium materials of known production date were distributed among the laboratories, and the samples were dated according to routine laboratory procedures by the measurement of the ²²⁰Th/²³⁴U ratio. The measurement results were in good agreement with the known production date showing that the concept for preparing uranium age dating reference material based on complete separation is valid. Detailed knowledge of the laboratory proceduresmore » used for uranium age dating allows the identification of possible improvements in the current protocols and the development of improved practice in the future. The availability of age dating reference materials as well as the evolvement of the age dating best-practice protocol will increase the relevance and applicability of age dating as part of the tool-kit available for nuclear forensic investigations.« less

Validation of reference materials for uranium radiochronometry in the frame of nuclear forensic investigations

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

Varga, Z.; Mayer, K.; Bonamici, C. E.

The results of a joint effort by expert nuclear forensic laboratories in the area of age dating of uranium, i.e. the elapsed time since the last chemical purification of the material are presented and discussed. Completely separated uranium materials of known production date were distributed among the laboratories, and the samples were dated according to routine laboratory procedures by the measurement of the ²²⁰Th/²³⁴U ratio. The measurement results were in good agreement with the known production date showing that the concept for preparing uranium age dating reference material based on complete separation is valid. Detailed knowledge of the laboratory proceduresmore » used for uranium age dating allows the identification of possible improvements in the current protocols and the development of improved practice in the future. The availability of age dating reference materials as well as the evolvement of the age dating best-practice protocol will increase the relevance and applicability of age dating as part of the tool-kit available for nuclear forensic investigations.« less

MOTHER AND INFANT CARE, PRACTICAL NURSE TRAINING PROGRAM, LESSON PLANS, PREPARED BY PRACTICAL NURSING INSTRUCTORS DURING CONFERENCE (UNIVERSITY OF TENNESSEE, AUGUST 14-18, 1961).

ERIC Educational Resources Information Center

Tennessee State Board for Vocational Education, Murfreesboro. Vocational Curriculum Lab.

PRACTICAL NURSE INSTRUCTORS, IN CONFERENCE, COMPILED THIS INDIVIDUALLY PLANNED AND TESTED MATERIAL TO BE USED IN PRACTICAL NURSE EDUCATION. THIRTY-TWO LESSON PLANS ON THE SUBJECT OF MOTHER AND INFANT CARE COVER TOPICS RANGING FROM THE REPRODUCTIVE SYSTEM TO COMPLICATIONS INVOLVING THE NEWBORN. EACH PLAN INCLUDES AIM, REFERENCES, MATERIALS,…

Quantification of Cells with Specific Phenotypes I: Determination of CD4+ Cell Count Per Microliter in Reconstituted Lyophilized Human PBMC Prelabeled with Anti-CD4 FITC Antibody

PubMed Central

Stebbings, Richard; Wang, Lili; Sutherland, Janet; Kammel, Martin; Gaigalas, Adolfas K; John, Manuela; Roemer, Bodo; Kuhne, Maren; Schneider, Rudolf J; Braun, Michael; Engel, Andrea; Dikshit, Dinesh K; Abbasi, Fatima; Marti, Gerald E; Paola Sassi, Maria; Revel, Laura; Kim, Sook-Kyung; Baradez, Marc-Olivier; Lekishvili, Tamara; Marshall, Damian; Whitby, Liam; Jing, Wang; Ost, Volker; Vonsky, Maxim; Neukammer, Jörg

2015-01-01

A surface-labeled lyophilized lymphocyte (sLL) preparation has been developed using human peripheral blood mononuclear cells prelabeled with a fluorescein isothiocyanate conjugated anti-CD4 monoclonal antibody. The sLL preparation is intended to be used as a reference material for CD4+ cell counting including the development of higher order reference measurement procedures and has been evaluated in the pilot study CCQM-P102. This study was conducted across 16 laboratories from eight countries to assess the ability of participants to quantify the CD4+ cell count of this reference material and to document cross-laboratory variability plus associated measurement uncertainties. Twelve different flow cytometer platforms were evaluated using a standard protocol that included calibration beads used to obtain quantitative measurements of CD4+ T cell counts. There was good overall cross-platform and counting method agreement with a grand mean of the laboratory calculated means of (301.7 ± 4.9) μL−1 CD4+ cells. Excluding outliers, greater than 90% of participant data agreed within ±15%. A major contribution to variation of sLL CD4+ cell counts was tube to tube variation of the calibration beads, amounting to an uncertainty of 3.6%. Variation due to preparative steps equated to an uncertainty of 2.6%. There was no reduction in variability when data files were centrally reanalyzed. Remaining variation was attributed to instrument specific differences. CD4+ cell counts obtained in CCQM-P102 are in excellent agreement and show the robustness of both the measurements and the data analysis and hence the suitability of sLL as a reference material for interlaboratory comparisons and external quality assessment. © 2015 The Authors. Published by Wiley Periodicals, Inc. PMID:25655255

Development of certified reference materials for electrolytes in human serum (GBW09124-09126).

PubMed

Feng, Liuxing; Wang, Jun; Cui, Yanjie; Shi, Naijie; Li, Haifeng; Li, Hongmei

2017-05-01

Three reference materials, at relatively low, middle, and high concentrations, were developed for analysis of the mass fractions of electrolytes (K, Ca, Na, Mg, Cl, and Li) in human serum. The reference materials were prepared by adding high purity chloride salts to normal human serum. The concentration range of the three levels is within ±20% of normal human serum. It was shown that 14 units with duplicate analysis is enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for 1 week at 40 °C and long-term stability test for 14 months. The certification methods of the six elements include isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectroscopy (ICP-OES), atomic absorption spectroscopy (AAS), ion chromatography (IC), and ion-selective electrode (ISE). The certification methods were validated by international comparisons among a number of national metrology institutes (NMIs). The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the analytical methods, homogeneity, and stability. The range of the expanded uncertainties of all the elements is from 2.2% to 3.9%. The certified reference materials (CRMs) are primarily intended for use in the calibration and validation of procedures in clinical analysis for the determination of electrolytes in human serum or plasma. Graphical Abstract Certified reference materials for K, Ca, Mg, Na, Cl and Li in human serum (GBW09124-09126).

Performances of some low-cost counter electrode materials in CdS and CdSe quantum dot-sensitized solar cells.

PubMed

Jun, Hieng Kiat; Careem, Mohamed Abdul; Arof, Abdul Kariem

2014-02-10

Different counter electrode (CE) materials based on carbon and Cu2S were prepared for the application in CdS and CdSe quantum dot-sensitized solar cells (QDSSCs). The CEs were prepared using low-cost and facile methods. Platinum was used as the reference CE material to compare the performances of the other materials. While carbon-based materials produced the best solar cell performance in CdS QDSSCs, platinum and Cu2S were superior in CdSe QDSSCs. Different CE materials have different performance in the two types of QDSSCs employed due to the different type of sensitizers and composition of polysulfide electrolytes used. The poor performance of QDSSCs with some CE materials is largely due to the lower photocurrent density and open-circuit voltage. The electrochemical impedance spectroscopy performed on the cells showed that the poor-performing QDSSCs had higher charge-transfer resistances and CPE values at their CE/electrolyte interfaces.

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

PubMed Central

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

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

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

PubMed

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

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

Quality assurance and quality control in light stable isotope laboratories: A case study of Rio Grande, Texas, water samples

USGS Publications Warehouse

Coplen, T.B.; Qi, H.

2009-01-01

New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory information management system, (9) making at regular intervals a complete backup of laboratory analytical data (both of samples logged into the laboratory and of mass spectrometric analyses), being sure to store one copy of this backup offsite, and (10) participating in interlaboratory comparison exercises sponsored by the IAEA and other agencies at regular intervals. ?? Taylor & Francis.

Certified reference materials and reference methods for nuclear safeguards and security.

PubMed

Jakopič, R; Sturm, M; Kraiem, M; Richter, S; Aregbe, Y

2013-11-01

Confidence in comparability and reliability of measurement results in nuclear material and environmental sample analysis are established via certified reference materials (CRMs), reference measurements, and inter-laboratory comparisons (ILCs). Increased needs for quality control tools in proliferation resistance, environmental sample analysis, development of measurement capabilities over the years and progress in modern analytical techniques are the main reasons for the development of new reference materials and reference methods for nuclear safeguards and security. The Institute for Reference Materials and Measurements (IRMM) prepares and certifices large quantities of the so-called "large-sized dried" (LSD) spikes for accurate measurement of the uranium and plutonium content in dissolved nuclear fuel solutions by isotope dilution mass spectrometry (IDMS) and also develops particle reference materials applied for the detection of nuclear signatures in environmental samples. IRMM is currently replacing some of its exhausted stocks of CRMs with new ones whose specifications are up-to-date and tailored for the demands of modern analytical techniques. Some of the existing materials will be re-measured to improve the uncertainties associated with their certified values, and to enable laboratories to reduce their combined measurement uncertainty. Safeguards involve the quantitative verification by independent measurements so that no nuclear material is diverted from its intended peaceful use. Safeguards authorities pay particular attention to plutonium and the uranium isotope (235)U, indicating the so-called 'enrichment', in nuclear material and in environmental samples. In addition to the verification of the major ratios, n((235)U)/n((238)U) and n((240)Pu)/n((239)Pu), the minor ratios of the less abundant uranium and plutonium isotopes contain valuable information about the origin and the 'history' of material used for commercial or possibly clandestine purposes, and have therefore reached high level of attention for safeguards authorities. Furthermore, IRMM initiated and coordinated the development of a Modified Total Evaporation (MTE) technique for accurate abundance ratio measurements of the "minor" isotope-amount ratios of uranium and plutonium in nuclear material and, in combination with a multi-dynamic measurement technique and filament carburization, in environmental samples. Currently IRMM is engaged in a study on the development of plutonium reference materials for "age dating", i.e. determination of the time elapsed since the last separation of plutonium from its daughter nuclides. The decay of a radioactive parent isotope and the build-up of a corresponding amount of daughter nuclide serve as chronometer to calculate the age of a nuclear material. There are no such certified reference materials available yet. Copyright © 2013 Elsevier Ltd. All rights reserved.

A new organic reference material, L-glutamic acid, USGS41a, for δ13C and δ15N measurements − a replacement for USGS41

USGS Publications Warehouse

Qi, Haiping; Coplen, Tyler B.; Mroczkowski, Stanley J.; Brand, Willi A.; Brandes, Lauren; Geilmann, Heike; Schimmelmann, Arndt

2016-01-01

RationaleThe widely used l-glutamic acid isotopic reference material USGS41, enriched in both 13C and 15N, is nearly exhausted. A new material, USGS41a, has been prepared as a replacement for USGS41.MethodsUSGS41a was prepared by dissolving analytical grade l-glutamic acid enriched in 13C and 15N together with l-glutamic acid of normal isotopic composition. The δ13C and δ15N values of USGS41a were directly or indirectly normalized with the international reference materials NBS 19 calcium carbonate (δ13CVPDB = +1.95 mUr, where milliurey = 0.001 = 1 ‰), LSVEC lithium carbonate (δ13CVPDB = −46.6 mUr), and IAEA-N-1 ammonium sulfate (δ15NAir = +0.43 mUr) and USGS32 potassium nitrate (δ15N = +180 mUr exactly) by on-line combustion, continuous-flow isotope-ratio mass spectrometry, and off-line dual-inlet isotope-ratio mass spectrometry.ResultsUSGS41a is isotopically homogeneous; the reproducibility of δ13C and δ15N is better than 0.07 mUr and 0.09 mUr, respectively, in 200-μg amounts. It has a δ13C value of +36.55 mUr relative to VPDB and a δ15N value of +47.55 mUr relative to N2 in air. USGS41 was found to be hydroscopic, probably due to the presence of pyroglutamic acid. Experimental results indicate that the chemical purity of USGS41a is substantially better than that of USGS41.ConclusionsThe new isotopic reference material USGS41a can be used with USGS40 (having a δ13CVPDB value of −26.39 mUr and a δ15NAir value of −4.52 mUr) for (i) analyzing local laboratory isotopic reference materials, and (ii) quantifying drift with time, mass-dependent isotopic fractionation, and isotope-ratio-scale contraction for isotopic analysis of biological and organic materials. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

A new organic reference material, l-glutamic acid, USGS41a, for δ(13) C and δ(15) N measurements - a replacement for USGS41.

PubMed

Qi, Haiping; Coplen, Tyler B; Mroczkowski, Stanley J; Brand, Willi A; Brandes, Lauren; Geilmann, Heike; Schimmelmann, Arndt

2016-04-15

The widely used l-glutamic acid isotopic reference material USGS41, enriched in both (13) C and (15) N, is nearly exhausted. A new material, USGS41a, has been prepared as a replacement for USGS41. USGS41a was prepared by dissolving analytical grade l-glutamic acid enriched in (13) C and (15) N together with l-glutamic acid of normal isotopic composition. The δ(13) C and δ(15) N values of USGS41a were directly or indirectly normalized with the international reference materials NBS 19 calcium carbonate (δ(13) CVPDB = +1.95 mUr, where milliurey = 0.001 = 1 ‰), LSVEC lithium carbonate (δ(13) CVPDB = -46.6 mUr), and IAEA-N-1 ammonium sulfate (δ(15) NAir = +0.43 mUr) and USGS32 potassium nitrate (δ(15) N = +180 mUr exactly) by on-line combustion, continuous-flow isotope-ratio mass spectrometry, and off-line dual-inlet isotope-ratio mass spectrometry. USGS41a is isotopically homogeneous; the reproducibility of δ(13) C and δ(15) N is better than 0.07 mUr and 0.09 mUr, respectively, in 200-μg amounts. It has a δ(13) C value of +36.55 mUr relative to VPDB and a δ(15) N value of +47.55 mUr relative to N2 in air. USGS41 was found to be hydroscopic, probably due to the presence of pyroglutamic acid. Experimental results indicate that the chemical purity of USGS41a is substantially better than that of USGS41. The new isotopic reference material USGS41a can be used with USGS40 (having a δ(13) CVPDB value of -26.39 mUr and a δ(15) NAir value of -4.52 mUr) for (i) analyzing local laboratory isotopic reference materials, and (ii) quantifying drift with time, mass-dependent isotopic fractionation, and isotope-ratio-scale contraction for isotopic analysis of biological and organic materials. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

Evaluating the quality of a cell counting measurement process via a dilution series experimental design.

PubMed

Sarkar, Sumona; Lund, Steven P; Vyzasatya, Ravi; Vanguri, Padmavathy; Elliott, John T; Plant, Anne L; Lin-Gibson, Sheng

2017-12-01

Cell counting measurements are critical in the research, development and manufacturing of cell-based products, yet determining cell quantity with accuracy and precision remains a challenge. Validating and evaluating a cell counting measurement process can be difficult because of the lack of appropriate reference material. Here we describe an experimental design and statistical analysis approach to evaluate the quality of a cell counting measurement process in the absence of appropriate reference materials or reference methods. The experimental design is based on a dilution series study with replicate samples and observations as well as measurement process controls. The statistical analysis evaluates the precision and proportionality of the cell counting measurement process and can be used to compare the quality of two or more counting methods. As an illustration of this approach, cell counting measurement processes (automated and manual methods) were compared for a human mesenchymal stromal cell (hMSC) preparation. For the hMSC preparation investigated, results indicated that the automated method performed better than the manual counting methods in terms of precision and proportionality. By conducting well controlled dilution series experimental designs coupled with appropriate statistical analysis, quantitative indicators of repeatability and proportionality can be calculated to provide an assessment of cell counting measurement quality. This approach does not rely on the use of a reference material or comparison to "gold standard" methods known to have limited assurance of accuracy and precision. The approach presented here may help the selection, optimization, and/or validation of a cell counting measurement process. Published by Elsevier Inc.

MICROWAVE-ASSISTED EXTRACTION OF ORGANIC COMPOUNDS FROM STANDARD REFERENCE SOILS AND SEDIMENTS

EPA Science Inventory

As part of an ongoing evaluation of new sample preparation techniques by the U.S. Environmental Protection Agency (EPA), especially those that minimize waste solvents, microwave-assisted extraction (MAE) of organic compounds from solid materials (or "matrices") was evaluated. Six...

The Environmental Assessment and Management (TEAM) Guide: North Carolina Supplement

DTIC Science & Technology

2010-03-01

for Federal Regulations incorporated by reference. Definitions • Abrasive - any material used in abrasive blasting operations (15A NCAC 2D.0541...Added March 2001]. • Abrasive Blasting - the operation of cleaning or preparing a surface by forcibly propelling a stream of abrasive material against...the surface. Sandblasting is one form of abrasive blasting (15A NCAC 2D.0541) [Added March 2001]. • Abrasive Blasting Equipment - any equipment

Preventing Supercooling Of Gallium

NASA Technical Reports Server (NTRS)

Massucco, Arthur A.; Wenghoefer, Hans M.; Wilkins, Ronnie

1994-01-01

Principle of heterogeneous nucleation exploited to prevent gallium from supercooling, enabling its use as heat-storage material that crystallizes reproducibly at its freezing or melting temperature of 29 to 30 degrees C. In original intended application, gallium used as heat-storage material in gloves of space suits. Terrestrial application lies in preparation of freezing-temperature reference samples for laboratories. Principle of heterogeneous nucleation also exploited similarly in heat pipes filled with sodium.

Functionally Graded Materials Database

NASA Astrophysics Data System (ADS)

Kisara, Katsuto; Konno, Tomomi; Niino, Masayuki

2008-02-01

Functionally Graded Materials Database (hereinafter referred to as FGMs Database) was open to the society via Internet in October 2002, and since then it has been managed by the Japan Aerospace Exploration Agency (JAXA). As of October 2006, the database includes 1,703 research information entries with 2,429 researchers data, 509 institution data and so on. Reading materials such as "Applicability of FGMs Technology to Space Plane" and "FGMs Application to Space Solar Power System (SSPS)" were prepared in FY 2004 and 2005, respectively. The English version of "FGMs Application to Space Solar Power System (SSPS)" is now under preparation. This present paper explains the FGMs Database, describing the research information data, the sitemap and how to use it. From the access analysis, user access results and users' interests are discussed.

Development, preparation, and characterization of high-performance superconducting materials for space applications

NASA Technical Reports Server (NTRS)

Thorpe, Arthur N.; Barkatt, Aaron

1991-01-01

The preparation of high-temperature superconducting ceramics in bulk form is a major challenge in materials science. The current status of both partial melting and melt quenching techniques, with or without an intermediate powder processing stage, is described in detail, and the problems associated with each of the methods are discussed. Results of studies performed on melt-processed materials are reported and discussed. The discussion places emphasis on magnetization and on other physical properties associated with it, such as critical current density, levitation force, and flux creep. The nature of structural features which give rise to flux pinning, including both small and large defects, is discussed with reference to theoretical considerations. The rates of flux creep and the factors involved in attempting to retard the decay of the magnetization are surveyed.

Three new mussel tissue standard reference materials (SRMs) for the determination of organic contaminants.

PubMed

Poster, Dianne L; Schantz, Michele M; Kucklick, John R; Lopez de Alda, Maria J; Porter, Barbara J; Pugh, Rebecca; Wise, Stephen A

2004-03-01

Three new mussel tissue standard reference materials (SRMs) have been developed by the National Institute of Standards and Technology (NIST) for the determination of the concentrations of organic contaminants. The most recently prepared material, SRM 1974b, is a fresh frozen tissue homogenate prepared from mussels ( Mytilus edulis) collected in Boston Harbor, Massachusetts. The other two materials, SRMs 2977 and 2978, are freeze-dried tissue homogenates prepared from mussels collected in Guanabara Bay, Brazil and Raritan Bay, New Jersey, respectively. All three new mussel tissue SRMs complement the current suite of marine natural-matrix SRMs available from NIST that are characterized for a wide range of contaminants (organic and inorganic). SRM 1974b has been developed to replace its predecessor SRM 1974a, Organics in Mussel Tissue, for which the supply is depleted. Similarly, SRMs 2977 and 2978 were developed to replace a previously available (supply depleted) freeze-dried version of SRM 1974a, SRM 2974, Organics in Freeze-Dried Mussel Tissue. SRM 1974b is the third in a series of fresh frozen mussel tissue homogenate SRMs prepared from mussels collected in Boston Harbor starting in 1988. SRM 1974b has certified concentration values for 22 polycyclic aromatic hydrocarbons (PAHs), 31 polychlorinated biphenyl congeners (PCBs), and 7 chlorinated pesticides. Reference values are provided for additional constituents: 16 PAHs, 8 PCBs plus total PCBs, 6 pesticides, total extractable organics, methylmercury, and 11 trace elements. PAH concentrations range from about 2 ng g(-1 )dry mass (cyclopenta[ cd]pyrene) to 180 ng g(-1 )dry mass (pyrene). PCB concentrations range from about 2 ng g(-1 )dry mass (PCB 157) to 120 ng g(-1 )dry mass (PCB 153). The reference value for total PCBs in SRM 1974b is (2020 +/- 420) ng g(-1 )dry mass. Pesticide concentrations range from about 4 ng g(-1 )dry mass (4,4'-DDT) to 40 ng g(-1 )dry mass (4,4'-DDE). SRM 2977 has certified values for 14 PAHs, 25 PCB congeners, 7 pesticides, 6 trace elements, and methylmercury. Reference values for 16 additional PAHs and 9 inorganic constituents are provided, and information values are given for 23 additional trace elements. SRM 2978 has certified and reference concentrations for 41 and 22 organic compounds, respectively, and contains contaminant levels similar to those of SRM 1974b. Organic contaminant levels in SRM 2977 (mussels from Guanabara Bay, Brazil) are typically a factor of 2 to 4 lower than those in SRM 1974b and SRM 2978. The organic contaminant concentrations in each new mussel tissue SRM are presented and compared in this paper. In addition, a chronological review of contaminant concentrations associated with mussels collected in Boston Harbor is discussed as well as a stability assessment of SRM 1974a.

Polyacrylate microspheres composite for all-solid-state reference electrodes.

PubMed

Kisiel, Anna; Donten, Mikołaj; Mieczkowski, Józef; Rius-Ruiz, F Xavier; Maksymiuk, Krzysztof; Michalska, Agata

2010-09-01

A novel concept is proposed for the encapsulation of components within polyacrylate microspheres, prior to their incorporation into a membrane phase. Thus finer and better controlled dispersion of heterogeneous membrane components can be achieved. This concept was verified by using a poly(n-butyl acrylate) membrane-based reference electrode as an example. In this example the proper dispersion of solid constituents of the heterogeneous membrane and prevention of their leakage are both of primary importance. Potassium chloride-loaded poly(n-butyl acrylate) microspheres were prepared and then left in contact with silver nitrate to convert some of the KCl into AgCl. The material obtained was introduced into a poly(n-butyl acrylate) membrane. The reference electrode membranes obtained in this way were characterized with much more stable potential (both in different electrolytes and over time) compared with electrodes prepared by the direct introduction of KCl and AgCl to the membrane.

Synthesis and Properties of Benzil End-Capped Acetylene Terminated Phenylquinoxalines (BATQs)

DTIC Science & Technology

1978-12-01

ratio of reactants. The ortho diamine end-capped quinoxaline oligomers were then reacted with excess I in m- cresol . All the oligomers prepared were...displacement of the nitro group on 4-nitrobenzil provided a 47% overall yield of I. The material exhibits excellent shelf-life in contrast to the...benzene 1,4-Bis(4-benziloxy)benzene was prepared by the nitro -displacement procedure of Relles et al (Reference 6). 3. Other Bis-benzils Other bis

EDQM biological reference preparation for rabies vaccine (inactivated) for veterinary use.

PubMed

Daas, A; Bruckner, L; Milne, C

2015-01-01

Rabies is a deadly zoonotic disease. Control of rabies in animals by vaccination is an important strategy to protect humans from infection and control the spread of the disease. Requirements for the quality control of rabies vaccines (inactivated) for veterinary use include an in vivo quantitative potency determination as outlined in the Ph. Eur. monograph 0451. Performance of this assay requires a reference preparation calibrated in International Units (IU). A European Pharmacopeia (Ph. Eur.) Biological Reference Preparation (BRP) for rabies vaccines (inactivated) for veterinary use, calibrated in IU, has been established for this purpose. Due to the dwindling stocks of the current batch (batch 4) of Ph. Eur. BRP for rabies vaccines (inactivated) for veterinary use, a collaborative study was run as part of the EDQM Biological Standardisation Programme to establish BRP batch 5. Ten laboratories, including Official Medicines Control Laboratories and manufacturers, participated. The candidate BRP5 was assayed against the 6(th) International Standard for rabies vaccine using the in vivo vaccination-challenge assay (monograph 0451) to assign a potency value. The candidate was also compared to BRP batch 4 to establish continuity. Taking into account the results from the comparisons a potency of 10 IU/vial was assigned and in March 2015 the Ph. Eur. Commission adopted the material as Ph. Eur. BRP for rabies vaccines (inactivated) for veterinary use batch 5. In addition to the in vivo assay 3 laboratories tested the candidate material using their in-house in vitro assays for information.

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

Jackson, L.L.; Engleman, E.E.; Peard, J.L.

Sulfur was determined in plants and lichens by combustion of the sample and infrared detection of evolved sulfur dioxide using an automated sulfur analyzer. Vanadium pentaoxide was used as a combustion accelerator. Pelletization of the sample prior to combustion was not found to be advantageous. Washing studies showed that leaching of sulfur was not a major factor in the sample preparation. The combustion-IR analysis usually gave higher sulfur content than the turbidimetric analysis as well as shorter analysis time. Relative standard deviations of less than 7% were obtained by the combustion-IR technique when sulfur levels in plant material range frommore » 0.05 to 0.70%. Determination of sulfur in National Bureau of Standards botanical reference materials showed good agreement between the combustion-IR technique and other instrumental procedures. Seven NBS botanical reference materials were analyzed.« less

Photocatalysis as an Effective Advanced Oxidation Process

EPA Science Inventory

Photocatalysis is generally referred to as the acceleration of a photoreaction by the presence of a semiconductor catalyst such as titanium dioxide (TiO2) or zinc oxide (ZnO). Photocatalytic materials can be prepared by using various methods such as a sol-gel process, solution pr...

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

USGS Publications Warehouse

Hoffman, Gerald L.

1996-01-01

A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.

Workshop on standards in biomass for energy and chemicals: proceedings

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

Milne, T.A.

1984-11-01

In the course of reviewing standards literature, visiting prominent laboratories and research groups, attending biomass meetings and corresponding widely, a whole set of standards needs was identified, the most prominent of which were: biomass standard reference materials, research materials and sample banks; special collections of microorganisms, clonal material, algae, etc.; standard methods of characterization of substrates and biomass fuels; standard tests and methods for the conversion and end-use of biomass; standard protocols for the description, harvesting, preparation, storage, and measurement of productivity of biomass materials in the energy context; glossaries of terms; development of special tests for assay of enzymaticmore » activity and related processes. There was also a recognition of the need for government, professional and industry support of concensus standards development and the dissemination of information on standards. Some 45 biomass researchers and managers met with key NBS staff to identify and prioritize standards needs. This was done through three working panels: the Panel on Standard Reference Materials (SRM's), Research Materials (RM's), and Sample Banks; the Panel on Production and Characterization; and the Panel on Tests and Methods for Conversion and End Use. This report gives a summary of the action items in standards development recommended unanimously by the workshop attendees. The proceedings of the workshop, and an appendix, contain an extensive written record of the findings of the workshop panelists and others regarding presently existing standards and standards issues and needs. Separate abstracts have been prepared for selected papers for inclusion in the Energy Database.« less

Advanced Curation Activities at NASA: Implications for Astrobiological Studies of Future Sample Collections

NASA Technical Reports Server (NTRS)

McCubbin, F. M.; Evans, C. A.; Fries, M. D.; Harrington, A. D.; Regberg, A. B.; Snead, C. J.; Zeigler, R. A.

2017-01-01

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F JSC is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. The Directive goes on to define Curation as including documentation, preservation, preparation, and distribution of samples for re-search, education, and public outreach. Here we briefly describe NASA's astromaterials collections and our ongoing efforts related to enhancing the utility of our current collections as well as our efforts to prepare for future sample return missions. We collectively refer to these efforts as advanced curation.

CRISPR/Cas9 Technology-Based Xenograft Tumors as Candidate Reference Materials for Multiple EML4-ALK Rearrangements Testing.

PubMed

Peng, Rongxue; Zhang, Rui; Lin, Guigao; Yang, Xin; Li, Ziyang; Zhang, Kuo; Zhang, Jiawei; Li, Jinming

2017-09-01

The echinoderm microtubule-associated protein-like 4 and anaplastic lymphoma kinase (ALK) receptor tyrosine kinase (EML4-ALK) rearrangement is an important biomarker that plays a pivotal role in therapeutic decision making for non-small-cell lung cancer (NSCLC) patients. Ensuring accuracy and reproducibility of EML4-ALK testing by fluorescence in situ hybridization, immunohistochemistry, RT-PCR, and next-generation sequencing requires reliable reference materials for monitoring assay sensitivity and specificity. Herein, we developed novel reference materials for various kinds of EML4-ALK testing. CRISPR/Cas9 was used to edit various NSCLC cell lines containing EML4-ALK rearrangement variants 1, 2, and 3a/b. After s.c. inoculation, the formalin-fixed, paraffin-embedded (FFPE) samples from xenografts were prepared and tested for suitability as candidate reference materials by fluorescence in situ hybridization, immunohistochemistry, RT-PCR, and next-generation sequencing. Sample validation and commutability assessments showed that all types of FFPE samples derived from xenograft tumors have typical histological structures, and EML4-ALK testing results were similar to the clinical ALK-positive NSCLC specimens. Among the four methods for EML4-ALK detection, the validation test showed 100% concordance. Furthermore, these novel FFPE reference materials showed good stability and homogeneity. Without limitations on variant types and production, our novel FFPE samples based on CRISPR/Cas9 editing and xenografts are suitable as candidate reference materials for the validation, verification, internal quality control, and proficiency testing of EML4-ALK detection. Copyright © 2017 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry-recommended reference measurement procedure and reference materials for glycated albumin determination.

PubMed

Takei, Izumi; Hoshino, Tadao; Tominaga, Makoto; Ishibashi, Midori; Kuwa, Katsuhiko; Umemoto, Masao; Tani, Wataru; Okahashi, Mikiko; Yasukawa, Keiko; Kohzuma, Takuji; Sato, Asako

2016-01-01

Glycated albumin is an intermediate glycaemic control marker for which there are several measurement procedures with entirely different reference intervals. We have developed a reference measurement procedure for the purpose of standardizing glycated albumin measurements. The isotope dilution liquid chromatography/tandem mass spectrometry method was developed as a reference measurement procedure for glycated albumin. The stable isotopes of lysine and fructosyl-lysine, which serve as an internal standard, were added to albumin isolated from serum, followed by hydrogenation. After hydrolysis of albumin with hot hydrochloric acid, the liberated lysine and fructosyl-lysine were measured by liquid chromatography/tandem mass spectrometry, and their concentrations were determined from each isotope ratio. The reference materials (JCCRM611) for determining of glycated albumin were prepared from pooled patient blood samples. The isotope dilution-tandem mass spectrometry calibration curve of fructosyl-lysine and lysine showed good linearity (r = 0.999). The inter-assay and intra-assay coefficient of variation values of glycated albumin measurement were 1.2 and 1.4%, respectively. The glycated albumin values of serum in patients with diabetes assessed through the use of this method showed a good relationship with routine measurement procedures (r = 0.997). The relationship of glycated albumin values of the reference material (JCCRM611) between these two methods was the same as the relationship with the patient serum samples. The Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry recommends the isotope dilution liquid chromatography/tandem mass spectrometry method as a reference measurement procedure, and JCCRM611 as a certified reference material for glycated albumin measurement. In addition, we recommend the traceability system for glycated albumin measurement. © The Author(s) 2015.

MYTHS--LITERATURE CURRICULUM I, STUDENT VERSION.

ERIC Educational Resources Information Center

KITZHABER, ALBERT

PRESENTED HERE WAS A STUDY GUIDE FOR STUDENT USE IN A SEVENTH-GRADE LITERATURE CURRICULUM. INTRODUCTORY MATERIAL WAS PRESENTED ON GREEK MYTHS, NORSE MYTHOLOGY, AND AMERICAN INDIAN MYTHOLOGY. STUDY QUESTIONS, SUGGESTED ACTIVITIES, AND A REFERENCE BOOK OF MYTHS WERE PRESENTED. AN ACCOMPANYING GUIDE WAS PREPARED FOR TEACHERS (ED 010 140). (WN)

Resources for Improving Principal Effectiveness. Annotated Bibliography of Packaged Training Programs.

ERIC Educational Resources Information Center

Gaddy, C. Stephen

This annotated bibliography of commercially prepared training materials for management and leadership development programs offers 10 topical sections of references applicable to school principal training. Entries were selected by using the following criteria: (1) programs dealing too specifically with management in sales, manufacturing, finance,…

Economic Evaluation of Building Design, Construction, Operation and Maintenance. Seminar Workbook.

ERIC Educational Resources Information Center

Ruegg, Rosalie T.

This workbook has been prepared for participants in the seminar, "Economic Evaluation of Building Design, Construction, Operation and Maintenance." It has two main functions: (1) to provide basic resource materials, references, and introductions to methods employed in the seminar; and (2) to provide instructional problems for solution by…

The Descriptive Challenges of Fiber Art.

ERIC Educational Resources Information Center

Lunin, Lois F.

1990-01-01

A definition of fiber art, its history, materials and techniques, vocabularies, and creators and users of those vocabularies offer background for understanding the problems in preparing surrogates of this relatively recent art form for text and image databases. Four examples of fiber image information systems are described. (32 references) (EAM)

Fluoride Analysis. Training Module 5.200.2.77.

ERIC Educational Resources Information Center

Kirkwood Community Coll., Cedar Rapids, IA.

This document is an instructional module package prepared in objective form for use by an instructor familiar with fluoride analysis procedures. Included are objectives, an instructor guide, student handouts, and a list of reference material. This module considers the determination of fluoride in water supplies using the SPANDS and electrode…

Development of Biologically Modified Anodes for Energy Harvesting Using Microbial Fuel Cells

DTIC Science & Technology

2012-09-01

also robust and conductive. 2. MATERIALS AND METHODS Artificial, conductive biofilms were prepared of both yeast and bacteria from the genera...written software using LabView. 2.1 Yeast Yeast biofilms were all prepared using a minimal media referred to as M9 with glucose added. M9 consists... yeast was cultured in the presence of a carbon felt electrode (~1cm X4cm) with a titanium wire as the electrical lead. 7 micron carbon fiber was

Piezoelectric and Electrostrictive Materials for Transducer Applications. Volume 3.

DTIC Science & Technology

1988-03-01

the preparation and characterization of these required compositions. High-purity lead acetate, titanium isopropoxide , and zirconium n-propoxide were...method was similar to the procedure used in Reference 4 to prepare PbTiO 3. High-purity lead acetate [Pb(C2 H3 0 2 )2 -3H-2Oj, titanium isopropoxide [Ti(OC...dielectric constant as shown in Figure 14(A). P.𔃿 8 IV. CONCLUSION High-purity lead acetate, titanium isopropoxide and zirconium n-propoxide were used as

Collaborative study for establishment of the European Pharmacopoeia BRP batch 1 for diphtheria toxin.

PubMed

Sesardic, D; Prior, C; Daas, A; Buchheit, K H

2003-07-01

A stable liquid candidate Biological Reference Preparation (BRP) for diphtheria toxin was prepared in peptone buffer (nominal content of diphtheria toxin: 1 Lf/ml, 0.4 micro g/ml), filled in ampoules (filling volume: 1 ml) and characterised in a collaborative study. The toxin is to be used in the test "Absence of toxin and irreversibility of toxoid" as described in the current European Pharmacopoeia (Ph. Eur.) monograph Diphtheria Vaccine (Adsorbed) (2002:0443). Eleven laboratories assessed the specific activity of the preparation by in vivo and in vitro assays. The material is assumed to have satisfactory stability with a calculated predicted loss of activity of <1% per year at 4-8 degrees C. From the collaborative study, the specific activity was calculated as 77.6 (45-113) LD( 50)/ml (lethal challenge) and >75 000 Lr/Lf (intradermal challenge). The candidate BRP was successfully used in nine laboratories and confirmed suitable for use in the Vero cell test for "Absence of toxin and irreversibility of toxoid" as described in the Ph. Eur. monograph 2002:0443; i.e., concentrations of 5 x 10( -5) Lf/ml and below caused cytotoxic effects in the Vero cell test. Due to its liquid nature, the stability of the material will be monitored at regular intervals and preparation of a stable freeze-dried formulation will be considered for long-term use. Additional studies will be performed to confirm suitability of this BRP for other applications. The candidate BRP was adopted as the Ph. Eur. reference material for Diphtheria Toxin Batch 1 by the Ph. Eur. Commission at its session in March 2003.

Critical assessment of the performance of electronic moisture analyzers for small amounts of environmental samples and biological reference materials.

PubMed

Krachler, M

2001-12-01

Two electronic moisture analyzers were critically evaluated with regard to their suitability for determining moisture in small amounts (< or = 200 mg) of various environmental matrices such as leaves, needles, soil, peat, sediments, and sewage sludge, as well as various biological reference materials. To this end, several homogeneous bulk materials were prepared which were subsequently employed for the development and optimization of all analytical procedures. The key features of the moisture analyzers included a halogen or ceramic heater and an integrated balance with a resolution of 0.1 mg, which is an essential prerequisite for obtaining precise results. Oven drying of the bulk materials in a conventional oven at 105 degrees C until constant mass served as reference method. A heating temperature of 65degrees C was found to provide accurate and precise results for almost all matrices investigated. To further improve the accuracy and precision, other critical parameters such as handling of sample pans, standby temperature, and measurement delay were optimized. Because of its ponderous heating behavior, the performance of the ceramic radiator was inferior to that of the halogen heater, which produced moisture results comparable to those obtained by oven drying. The developed drying procedures were successfully applied to the fast moisture analysis (1.4-6.3 min) of certified biological reference materials of similar provenance to the investigated the bulk materials. Moisture results for 200 mg aliquots ranged from 1.4 to 7.8% and good agreement was obtained between the recommended drying procedure for the reference materials and the electronic moisture analyzers with absolute uncertainties amounting to 0.1% and 0.2-0.3%, respectively.

Single-step preparation of TiO2/MWCNT Nanohybrid materials by laser pyrolysis and application to efficient photovoltaic energy conversion.

PubMed

Wang, Jin; Lin, Yaochen; Pinault, Mathieu; Filoramo, Arianna; Fabert, Marc; Ratier, Bernard; Bouclé, Johann; Herlin-Boime, Nathalie

2015-01-14

This paper presents the continuous-flowand single-step synthesis of a TiO2/MWCNT (multiwall carbon nanotubes) nanohybrid material. The synthesis method allows achieving high coverage and intimate interface between the TiO2particles and MWCNTs, together with a highly homogeneous distribution of nanotubes within the oxide. Such materials used as active layer in theporous photoelectrode of solid-state dye-sensitized solar cells leads to a substantial performance improvement (20%) as compared to reference devices.

A test method for determining adhesion forces and Hamaker constants of cementitious materials using atomic force microscopy

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

Lomboy, Gilson; Sundararajan, Sriram, E-mail: srirams@iastate.edu; Wang Kejin

2011-11-15

A method for determining Hamaker constant of cementitious materials is presented. The method involved sample preparation, measurement of adhesion force between the tested material and a silicon nitride probe using atomic force microscopy in dry air and in water, and calculating the Hamaker constant using appropriate contact mechanics models. The work of adhesion and Hamaker constant were computed from the pull-off forces using the Johnson-Kendall-Roberts and Derjagin-Muller-Toropov models. Reference materials with known Hamaker constants (mica, silica, calcite) and commercially available cementitious materials (Portland cement (PC), ground granulated blast furnace slag (GGBFS)) were studied. The Hamaker constants of the reference materialsmore » obtained are consistent with those published by previous researchers. The results indicate that PC has a higher Hamaker constant than GGBFS. The Hamaker constant of PC in water is close to the previously predicted value C{sub 3}S, which is attributed to short hydration time ({<=} 45 min) used in this study.« less

Determination of total sulfur in lichens and plants by combustion-infrared analysis

USGS Publications Warehouse

Jackson, L.L.; Engleman, E.E.; Peard, J.L.

1985-01-01

Sulfur was determined in plants and lichens by combustion of the sample and infrared detection of evolved sulfur dioxide using an automated sulfur analyzer. Vanadium pentaoxide was used as a combustion accelerator. Pelletization of the sample prior to combustion was not found to be advantageous. Washing studies showed that leaching of sulfur was not a major factor in the sample preparation. The combustion-IR analysis usually gave higher sulfur content than the turbidimetric analysis as well as shorter analysis time. Relative standard deviations of less than 7% were obtained by the combustion-IR technique when sulfur levels in plant material ranged from 0.05 to 0.70%. Determination of sulfur in National Bureau of Standards botanical reference materials showed good agreement between the combustion-IR technique and other instrumental procedures. Seven NBS botanical reference materials were analyzed.

Biomedical graphite and CaF2 preparation and measurement at PRIME Lab

NASA Astrophysics Data System (ADS)

Jackson, George S.; Einstein, Jane A.; Kubley, Tom; Martin, Berdine; Weaver, Connie M.; Caffee, Marc

2015-10-01

The biomedical program at PRIME Lab has prepared radiocarbon and 41Ca as tracers for a variety of applications. Over the last decade several hundred 14C samples and several thousand 41Ca samples have been measured per year. Biomedical samples pose challenges that are relatively rare in the AMS community. We will discuss how to prepare and compensate for samples that have isotope ratios above the dynamic range of AMS, high interference rates, and small samples sizes. In the case of 41Ca, the trade off in the chromatography between yield and sample cleanliness will be analyzed. Secondary standards that have isotope ratios commonly encountered in our applications are routinely prepared. We use material from the Joint Research Centre's Institute for Reference Materials and Measurement: IRMM-3701/4, 3701/5, and 3701/6 and a standard produced by PRIME Lab for 41Ca. We use International Atomic Energy Agency's IAEA C-3, IAEA C-7, IAEA C-8, and a ∼12.5× modern oxalic acid secondary standard supplied by Lawrence Livermore National Laboratory for 14C. We will discuss our precision, reproducibility, and the relative agreement between our measured and the reported values for these materials.

Multicentre evaluation of stable reference whole blood for enumeration of lymphocyte subsets by flow cytometry.

PubMed

Edwards, Cherry; Belgrave, Danielle; Janossy, George; Bradley, Nicholas J; Stebbings, Richard; Gaines-Das, Rose; Thorpe, Robin; Sawle, Alex; Arroz, Maria Jorge; Brando, Bruno; Gratama, Jan Willem; Orfao de Matos, Alberto; Papa, Stephano; Papamichail, Michael; Lenkei, Rodica; Rothe, Gregor; Barnett, David

2005-06-22

BACKGROUND: Clinical indications for lymphocyte subset enumeration by flow cytometry include monitoring of disease progression and timing of therapeutic intervention in infection with human immunodeficiency virus. Until recently international standardisation has not been possible due to a lack of suitable stable reference material. METHODS: This study consisted of two trials of a stabilised whole blood preparation. Eleven participants were sent two standard protocols for staining plus gating strategy and asked to report absolute counts for lymphocyte subsets. RESULTS: No significant difference was detected between the two methods when results from the two assays and all partners were pooled. Significant differences in results from the different partners were observed. However, representative mean counts were obtained for geometric means, geometric coefficient of variation, and 95% confidence interval for CD3 910 cells/mul, 9%, and 888 to 933, respectively), CD4 (495 cells/mul, 12%, and 483 to 507), and CD8 (408 cells/mul, 13%, and 393 to 422). CONCLUSION: We have introduced a stabilised blood preparation and a well-characterized biological standard. The availability of this reference material greatly simplifies the validation of new techniques for CD4(+) T-cell enumeration and the expansion of external quality assurance programmes for clinical laboratories, including those that operate in resource-restricted environments. (c) 2005 Wiley-Liss, Inc.

Certification of the Uranium Isotopic Ratios in Nbl Crm 112-A, Uranium Assay Standard (Invited)

NASA Astrophysics Data System (ADS)

Mathew, K. J.; Mason, P.; Narayanan, U.

2010-12-01

Isotopic reference materials are needed to validate measurement procedures and to calibrate multi-collector ion counting detector systems. New Brunswick Laboratory (NBL) provides a suite of certified isotopic and assay standards for the US and international nuclear safeguards community. NBL Certified Reference Material (CRM) 112-A Uranium Metal Assay Standard with a consensus value of 137.88 for the 238U/235U ratio [National Bureau of Standards -- NBS, currently named National Institute for Standards and Technology, Standard Reference Material (SRM) 960 had been renamed CRM 112-A] is commonly used as a natural uranium isotopic reference material within the earth science community. We have completed the analytical work for characterizing the isotopic composition of NBL CRM 112-A Uranium Assay Standard and NBL CRM 145 (uranyl nitrate solution prepared from CRM 112-A). The 235U/238U isotopic ratios were characterized using the total evaporation (TE) and the modified total evaporation (MTE) methods. The 234U/238U isotope ratios were characterized using a conventional analysis technique and verified using the ratios measured in the MTE analytical technique. The analysis plan for the characterization work was developed such that isotopic ratios that are traceable to NBL CRM U030-A are obtained. NBL is preparing a certificate of Analysis and will issue a certificate for Uranium Assay and Isotopics. The results of the CRM 112-A certification measurements will be discussed. These results will be compared with the average values from Richter et al (2010). A comparison of the precision and accuracy of the measurement methods (TE, MTE and Conventional) employed in the certification will be presented. The uncertainties in the 235U/238U and 234U/238U ratios, calculated according to the Guide to the Expression of Uncertainty in Measurements (GUM) and the dominant contributors to the combined standard uncertainty will be discussed.

Inorganic chemical analysis of environmental materials—A lecture series

USGS Publications Warehouse

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

2011-01-01

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

Reference materials and representative test materials to develop nanoparticle characterization methods: the NanoChOp project case

NASA Astrophysics Data System (ADS)

Roebben, Gert; Kestens, Vikram; Varga, Zoltan; Charoud-Got, Jean; Ramaye, Yannic; Gollwitzer, Christian; Bartczak, Dorota; Geißler, Daniel; Noble, James; Mazoua, Stéphane; Meeus, Nele; Corbisier, Philippe; Palmai, Marcell; Mihály, Judith; Krumrey, Michael; Davies, Julie; Resch-Genger, Ute; Kumarswami, Neelam; Minelli, Caterina; Sikora, Aneta; Goenaga-Infante, Heidi

2015-10-01

This paper describes the production and characteristics of the nanoparticle test materials prepared for common use in the collaborative research project NanoChOp (Chemical and optical characterisation of nanomaterials in biological systems), in casu suspensions of silica nanoparticles and CdSe/CdS/ZnS quantum dots. This paper is the first to illustrate how to assess whether nanoparticle test materials meet the requirements of a 'reference material' (ISO Guide 30:2015) or rather those of the recently defined category of 'representative test material' (ISO TS 16195:2013). The NanoChOp test materials were investigated with small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and centrifugal liquid sedimentation (CLS) to establish whether they complied with the required monomodal particle size distribution. The presence of impurities, aggregates, agglomerates and viable microorganisms in the suspensions was investigated with DLS, CLS, optical and electron microscopy and via plating on nutrient agar. Suitability of surface functionalization was investigated with attenuated total reflection Fourier transform infrared spectrometry (ATR-FTIR) and via the capacity of the nanoparticles to be fluorescently labeled or to bind antibodies. Between-unit homogeneity and stability were investigated in terms of particle size and zeta potential. This paper shows that only based on the outcome of a detailed characterization process one can raise the status of a test material to representative test material or reference material, and how this status depends on its intended use.

New quality-control materials for the determination of alkylphenols and alkylphenol ethoxylates in sewage sludge.

PubMed

Fernández-Sanjuan, María; Lacorte, Silvia; Rigol, Anna; Sahuquillo, Angels

2012-11-01

The determination of alkylphenols in sewage sludge is still hindered by the complexity of the matrix and of the analytes, some of which are a mixture of isomers. Most of the methods published in the literature have not been validated, due to the lack of reference materials for the determination of alkylphenols in sludge. Given this situation, the objectives of the present study were to develop a new quality-control material for determining octylphenol, nonylphenol and nonylphenol monoethoxylate in sludge. The material was prepared from an anaerobically digested sewage sludge, which was thermally dried, sieved, homogenized and bottled after checking for the bulk homogeneity of the processed material. Together with the sewage sludge, an extract was also prepared, in order to provide a quality-control material for allowing laboratories to test the measuring step. The homogeneity and 1-year stability of the two materials were evaluated. Statistical analysis proved that the materials were homogeneous and stable for at least 1 year stored at different temperatures. These materials are intended to assist in the quality control of the determination of alkylphenols and alkylphenol ethoxylates in sewage sludge.

Chinese-English Technical Dictionaries. Volume 1, Aviation and Space.

ERIC Educational Resources Information Center

Library of Congress, Washington, DC. Aerospace Technology Div.

The present dictionary is the first of a series of Chinese-English technical dictionaries under preparation by the Aerospace Technology Division of the Library of Congress. The purpose of the series is to provide rapid reference tools for translators, abstractors, and research analysts concerned with scientific and technical materials published in…

Microemulsion flame pyrolysis for hopcalite nanoparticle synthesis: a new concept for catalyst preparation.

PubMed

Biemelt, T; Wegner, K; Teichert, J; Kaskel, S

2015-04-07

A new route to highly active hopcalite catalysts via flame spray pyrolysis of an inverse microemulsion precursor is reported. The nitrate derived nanoparticles are around 15 nm in diameter and show excellent conversion of CO under ambient conditions, outperforming commercial reference hopcalite materials produced by co-precipitation.

SMALL CRAFT OPERATION AND NAVIGATION.

ERIC Educational Resources Information Center

Louisiana State Dept. of Education, Baton Rouge.

THIS REFERENCE TEXTBOOK WAS PREPARED FOR USE IN THE FIRST PART OF A TWO-PART COURSE IN MARINE NAVIGATION AND SMALL CRAFT OPERATION ON INLAND AND INTERNATIONAL WATERS. THE MATERIAL WAS DEVELOPED BY AN INDIVIDUAL AUTHOR FOR USE IN TRADE SCHOOL PREPARATORY AND EXTENSION CLASSES FOR MALE ADULTS WHO PLAN TO OPERATE BOATS. IT IS MAINLY CONCERNED WITH…

Unit: Water, Inspection Pack, National Trial Print.

ERIC Educational Resources Information Center

Australian Science Education Project, Toorak, Victoria.

The teachers' guide to this unit, prepared for use in grades seven or eight of Australian secondary schools, contains a list of unit objectives, teaching notes on each activity, lists of required apparatus, suggested teacher and student reference materials, and appropriate audio-visual aids. The core of the unit explores the importance of water…

Certified reference materials (GBW09170 and 09171) of creatinine in human serum.

PubMed

Dai, Xinhua; Fang, Xiang; Shao, Mingwu; Li, Ming; Huang, Zejian; Li, Hongmei; Jiang, You; Song, Dewei; He, Yajuan

2011-02-15

Creatinine is the most widely used clinical marker for assessing renal function. Concentrations of creatinine in human serum need to be carefully checked in order to ensure accurate diagnosis of renal function. Therefore, development of certified reference materials (CRMs) of creatinine in serum is of increasing importance. In this study, two new CRMs (Nos. GBW09170 and 09171) for creatinine in human serum have been developed. They were prepared with mixtures of several dozens of healthy people's and kidney disease patient's serum, respectively. The certified values of 8.10, 34.1 mg/kg for these two CRMs have been assigned by liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) method which was validated by using standard reference material (SRM) of SRM909b (a reference material obtained from National Institute of Standards and Technology, NIST). The expanded uncertainties of certified values for low and high concentrations were estimated to be 1.2 and 1.1%, respectively. The certified values were further confirmed by an international intercomparison for the determination of creatinine in human serum (Consultative Committee for Amount of Substance, CCQM) of K80 (CCQM-K80). These new CRMs of creatinine in human serum pool are totally native without additional creatinine spiked for enrichment. These new CRMs are capable of validating routine clinical methods for ensuring accuracy, reliability and comparability of analytical results from different clinical laboratories. They can also be used for instrument validation, development of secondary reference materials, and evaluating the accuracy of high order clinical methods for the determination of creatinine in human serum. Copyright © 2011 Elsevier B.V. All rights reserved.

Pulsed laser deposition of functionalized Mg-Al layered double hydroxide thin films

NASA Astrophysics Data System (ADS)

Vlad, A.; Birjega, R.; Tirca, I.; Matei, A.; Mardare, C. C.; Hassel, A. W.; Nedelcea, A.; Dinescu, M.; Zavoianu, R.

2018-02-01

In this paper, magnesium-aluminium layered double hydroxide (LDH) has been functionalized with sodium dodecyl sulfate (DS) and deposited as thin film by pulsed laser deposition (PLD). Mg, Al-LDH powders were prepared by co-precipitation and used as reference material. Intercalation of DS as an anionic surfactant into the LDHs host layers has been prepared in two ways: co-precipitation (P) and reconstruction (R). DS intercalation occurred in LDH powder via both preparation methods. The films deposited via PLD, in particular at 532 and 1064 nm, preserve the organic intercalated layered structure of the targets prepared from these powders. The results reveal the ability of proposed deposition technique to produce functional composite organo-modified LDHs thin films.

Modifications to the NIST reference measurement procedure (RMP) for the determination of serum glucose by isotope dilution gas chromatography/mass spectrometry.

PubMed

Prendergast, Jocelyn L; Sniegoski, Lorna T; Welch, Michael J; Phinney, Karen W

2010-07-01

The definitive method (DM), now known as the reference measurement procedure (RMP), for the analysis of glucose in serum was originally published in 1982 by the National Institute of Standards and Technology (NIST). Over the years the method has been subject to a number of modifications to adapt to newer technologies and simplify sample preparation. We discuss here an adaptation of the method associated with serum glucose measurements using a modified isotope dilution gas chromatography/mass spectrometry (ID-GC/MS) method. NIST has used this modified method to certify the concentrations of glucose in SRM 965b, Glucose in Frozen Human Serum, and SRM 1950, Metabolites in Human Plasma. Comparison of results from the revised method with certified values for existing Standard Reference Materials (SRMs) demonstrated that these modifications have not affected the quality of the measurements, giving both good precision and accuracy, while reducing the sample preparation time by a day and a half.

Investigation of preparation techniques for δ2H analysis of keratin materials and a proposed analytical protocol

USGS Publications Warehouse

Qi, H.; Coplen, T.B.

2011-01-01

Accurate hydrogen isotopic measurements of keratin materials have been a challenge due to exchangeable hydrogen in the sample matrix and the paucity of appropriate isotopic reference materials for calibration. We found that the most reproducible δ2HVSMOW-SLAP and mole fraction of exchangeable hydrogen, x(H)ex, of keratin materials were measured with equilibration at ambient temperature using two desiccators and two different equilibration waters with two sets of the keratin materials for 6 days. Following equilibration, drying the keratin materials in a vacuum oven for 4 days at 60 °C was most critical. The δ2H analysis protocol also includes interspersing isotopic reference waters in silver tubes among samples in the carousel of a thermal conversion elemental analyzer (TC/EA) reduction unit. Using this analytical protocol, δ2HVSMOW-SLAP values of the non-exchangeable fractions of USGS42 and USGS43 human-hair isotopic reference materials were determined to be –78.5 ± 2.3 ‰ and –50.3 ± 2.8 ‰, respectively. The measured x(H)ex values of keratin materials analyzed with steam equilibration and N2 drying were substantially higher than those previously published, and dry N2 purging was unable to remove absorbed moisture completely, even with overnight purging. The δ2H values of keratin materials measured with steam equilibration were about 10 ‰ lower than values determined with equilibration in desiccators at ambient temperatures when on-line evacuation was used to dry samples. With steam equilibrations the x(H)ex of commercial keratin powder was as high as 28 %. Using human-hair isotopic reference materials to calibrate other keratin materials, such as hoof or horn, can introduce bias in δ2H measurements because the amount of absorbed water and the x(H)ex values may differ from those of unknown samples. Correct δ2HVSMOW-SLAP values of the non-exchangeable fractions of unknown human-hair samples can be determined with atmospheric moisture equilibration by normalizing with USGS42 and USGS43 human-hair reference materials when all materials have the same powder size.

Titanium oxo-clusters: precursors for a Lego-like construction of nanostructured hybrid materials.

PubMed

Rozes, Laurence; Sanchez, Clément

2011-02-01

Titanium oxo-clusters, well-defined monodispersed nano-objects, are appropriate nano-building blocks for the preparation of organic-inorganic materials by a bottom up approach. This critical review proposes to present the different structures of titanium oxo-clusters referenced in the literature and the different strategies followed to build up hybrid materials with these versatile building units. In particular, this critical review cites and reports on the most important papers in the literature, concentrating on recent developments in the field of synthesis, characterization, and the use of titanium oxo-clusters for the construction of advanced hybrid materials (137 references).

Emerging applications of phase-change materials (PCMs): teaching an old dog new tricks.

PubMed

Hyun, Dong Choon; Levinson, Nathanael S; Jeong, Unyong; Xia, Younan

2014-04-07

The nebulous term phase-change material (PCM) simply refers to any substance that has a large heat of fusion and a sharp melting point. PCMs have been used for many years in commercial applications, mainly for heat management purposes. However, these fascinating materials have recently been rediscovered and applied to a broad range of technologies, such as smart drug delivery, information storage, barcoding, and detection. With the hope of kindling interest in this incredibly versatile range of materials, this Review presents an array of aspects related to the compositions, preparations, and emerging applications of PCMs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Approaches for enantioselective resolution of pharmaceuticals by miniaturised separation techniques with new chiral phases based on nanoparticles and monolithis.

PubMed

Sierra, Isabel; Marina, Maria Luisa; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Silva, Mariana

2016-10-01

This article discusses new developments in the preparation of nanoparticles and monoliths with emphasis upon their application as the stationary and pseudo-stationary phases for miniaturised liquid phase separation techniques, which have occurred in the last 10 years (from 2006 to the actuality). References included in this review represent current trends and state of the art in the application of these materials to the analysis, by EKC, CEC and miniaturised chromatography, of chiral compounds with environmental interest such as pharmaceuticals. Due to their extraordinary properties, columns prepared with these new chiral stationary or pseudo-stationary phases, based on materials such as gold nanoparticles, metal-organic frameworks, ordered mesoporous silicas, carbonaceous materials, polymeric-based and silica-based monoliths or molecularly imprinted materials, can usually show some improvements in the separation selectivity, column efficiency and chemical stability in comparison with conventional chiral columns available commercially. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a new chlorogenic acid certified reference material for food and drug analysis.

PubMed

Yang, Dezhi; Jiao, LingTai; Zhang, Baoxi; Du, Guanhua; Lu, Yang

2017-06-05

This paper reports the preparation and characterization of a new chlorogenic acid (CHA) certified reference material (CRM), which is unavailable commercially. CHA is an active ingredient found in many geo-authentic Chinese medicinal materials and developed as an anti-cancer drug. In this work, trace impurities were isolated and identified through various techniques. CHA CRM was quantified with two analytical methods, and their results were in good agreement with each other. The certified value and corresponding expanded uncertainty of CHA CRM reached 99.4%±0.2%, which was calculated by multiplying the combined standard uncertainty by the coverage factor (k=2), at a confidence level of 95%. This CRM can be used to calibrate measurement system, evaluate or validate measurement procedures, assign traceable property values to non-CRMs, and conduct quality control assays. Copyright © 2017 Elsevier B.V. All rights reserved.

Two New Reference Materials Based on Tobacco Leaves: Certification for over a Dozen of Toxic and Essential Elements

PubMed Central

Samczyński, Zbigniew; Dybczyński, Rajmund S.; Polkowska-Motrenko, Halina; Chajduk, Ewelina; Pyszynska, Marta; Danko, Bożena; Czerska, Elżbieta; Kulisa, Krzysztof; Doner, Katarzyna; Kalbarczyk, Paweł

2012-01-01

The preparation, certification, and characterization of two new biological certified reference materials for inorganic trace analysis have been presented. They are based on two different varieties of tobacco leaves, namely, Oriental Basma Tobacco Leaves (INCT-OBTL-5), grown in Greece, and Polish Virginia Tobacco Leaves (INCT-PVTL-6), grown in Poland. Certification of the materials was based on the statistical evaluation of results obtained in a worldwide interlaboratory comparison, in which 87 laboratories from 18 countries participated, providing 2568 laboratory averages on nearly 80 elements. It was possible to establish the certified values of concentration for many elements in the new materials, that is, 37 in INCT-OBTL-5 and 36 in INCT-PVTL-6, including several toxic ones like As, Cd, Hg, Pb, and so forth. The share and the role of instrumental analytical techniques used in the process of certification of the new CRMs are discussed. PMID:22536124

Feasibility study on production of a matrix reference material for cyanobacterial toxins.

PubMed

Hollingdale, Christie; Thomas, Krista; Lewis, Nancy; Békri, Khalida; McCarron, Pearse; Quilliam, Michael A

2015-07-01

The worldwide increase in cyanobacterial contamination of freshwater lakes and rivers is of great concern as many cyanobacteria produce potent hepatotoxins and neurotoxins (cyanotoxins). Such toxins pose a threat to aquatic ecosystems, livestock, and drinking water supplies. In addition, dietary supplements prepared from cyanobacteria can pose a risk to consumers if they contain toxins. Analytical monitoring for toxins in the environment and in consumer products is essential for the protection of public health. Reference materials (RMs) are an essential tool for the development and validation of analytical methods and are necessary for ongoing quality control of monitoring operations. Since the availability of appropriate RMs for cyanotoxins has been very limited, the present study was undertaken to examine the feasibility of producing a cyanobacterial matrix RM containing various cyanotoxins. The first step was large-scale culturing of various cyanobacterial cultures that produce anatoxins, microcystins, and cylindrospermopsins. After harvesting, the biomass was lyophilized, blended, homogenized, milled, and bottled. The moisture content and physical characteristics were assessed in order to evaluate the effectiveness of the production process. Toxin levels were measured by liquid chromatography with tandem mass spectrometry and ultraviolet detection. The reference material was found to be homogeneous for toxin content. Stability studies showed no significant degradation of target toxins over a period of 310 days at temperatures up to +40 °C except for the anatoxin-a, which showed some degradation at +40 °C. These results show that a fit-for-purpose matrix RM for cyanotoxins can be prepared using the processes and techniques applied in this work.

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

NASA Astrophysics Data System (ADS)

Papadopoulou, D. N.; Zachariadis, G. A.; Anthemidis, A. N.; Tsirliganis, N. C.; Stratis, J. A.

2004-12-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level).

Development of a NIST standard reference material containing thirty volatile organic compounds at 5 nmol/mol in nitrogen.

PubMed

Rhoderick, George C; Yen, James H

2006-05-01

Primary gravimetric gas cylinder standards containing 30 volatile organic compounds (VOCs) in nitrogen were prepared using a procedure previously developed to prepare gas mixture cylinder standards of VOCs at the 5 nmol/mol level. This set of primary standards was intercompared to existing gas cylinder standards, containing as many as 19 of the 30 volatile organics present in these new primaries, using gas chromatography with a hydrogen flame ionization detector coupled with cryogenic preconcentration. The linear regression analysis showed excellent agreement among the standards for each compound. Similar mixtures containing many of these compounds in treated aluminum gas cylinders have been evaluated over time and have shown stability for as much as 10 years. The development of these 30-component primary standards led to the preparation and certification of a reissue of Standard Reference Material (SRM) 1804 at the nominal amount-of-substance fraction of 5 nmol/mol for each analyte. A lot of 20 cylinders containing the mixture was prepared at NIST following previously demonstrated protocols for preparation of the cylinders. Each cylinder was analyzed against one cylinder from the lot, designated as the "lot standard," for each of the 30 compounds. As a result of the uncertainty analysis, the data showed that rather than declaring the lot homogeneous with a much higher uncertainty, each cylinder could be individually certified. The expanded uncertainty limits ranged from 1.5 to 10% for 28 of the 30 analytes, with two of the analytes having uncertainties as high as 19% in those SRM cylinders certified. Due to stability issues and some high uncertainties for a few analytes in 2 of the samples, 18 of the 20 candidate SRM samples were certified. These volatile organic gas mixtures represent the most complex gas SRMs developed at NIST.

Electroactive materials for organic electronics: preparation strategies, structural aspects and characterization techniques.

PubMed

Pron, Adam; Gawrys, Pawel; Zagorska, Malgorzata; Djurado, David; Demadrille, Renaud

2010-07-01

This critical review discusses specific chemical and physicochemical requirements which must be met for organic compounds to be considered as promising materials for applications in organic electronics. Although emphasis is put on molecules and macromolecules suitable for fabrication of field effect transistors (FETs), a large fraction of the discussed compounds can also be applied in other organic or hybrid (organic-inorganic) electronic devices such as photodiodes, light emitting diodes, photovoltaic cells, etc. It should be of interest to chemists, physicists, material scientists and electrical engineers working in the domain of organic electronics (423 references).

Polychlorinated biphenyls (PCB), chlorinated pesticides, and polycyclic aromatic hydrocarbons (PAHs) in environmental standard reference materials

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

Poster, D.L.; Schantz, M.M.; Parris, R.M.

1995-12-31

Standard reference materials (SRMs) are certified reference materials issued by the National Institute of Standards and Technology (NIST). Natural matrix environmental sample SRMs have been developed the Analytical Chemistry Division to assist in validating measurements for organic contaminants in the environment. Many of these are well characterized for contaminants such as polychlorinated biphenyls (PCBs), chlorinated pesticides, and polycyclic aromatic hydrocarbons (PAHs). SRM 1649, Organics in Urban Dust, is currently available with certified concentrations for 5 PAHs but because of the widespread use of this material in air pollution monitoring programs and to expand the usefulness of this material, the authorsmore » are further characterizing the material for a larger number of PAHs as well as PCBs and chlorinated pesticides. They will also soon issue a diesel particulate extract (SRM 1975) that is well characterized for PAHS, including many nitrogen substituted compounds. In addition to natural matrix materials, solutions useful for calibrating chromatographic detector response factors and retention times, and spiking sample blanks for determination of analyte recoveries, are also available. Solution SRMs currently available contain PCS congeners, chlorinated pesticides, and PAHs. New solution SRMs in preparation will contain additional chlorinated pesticides, PCB congeners (e.g., non-ortho substituted chlorobiphenyls), and perdeuterated PAHs. Recent SRM work will be presented with particular attention on the methods used for determining organic contaminant concentrations in the urban dust material and in the diesel particulate extract.« less

Taenia solium metacestode preparation in rural areas of sub-Saharan Africa: a source for diagnosis and research on cysticercosis.

PubMed

Schmidt, V; Sikasunge, C S; Odongo-Aginya, E; Simukoko, C; Mwanjali, G; Alarakol, S; Ovuga, E; Matuja, W; Kihamia, C; Löscher, T; Winkler, A S; Bretzel, G

2015-03-01

Taenia solium metacestodes/cysts obtained from pig carcasses constitute a primary source for diagnostic tools used for the detection of human cysticercosis. Data on T. solium cyst preparation in Africa is still scarce but required to establish independent reference laboratories. The aim of the present study is a) to present the likely yield of T. solium cyst material by the use of two different preparation methods in the field and b) to investigate its suitability for immunodiagnosis of human cysticercosis. In Zambia, Uganda and Tanzania 670 pigs were screened for T. solium infection. Cysts were prepared by 'shaking method' and 'washing method'. Generated crude antigens were applied in a standard western blot assay. 46 out of 670 pigs (6.9%) were found positive for T. solium (Zambia: 12/367, 3.3%; Uganda: 11/217, 5.1%; Tanzania 23/86, 26.7%). Mean values of 77.7 ml whole cysts, 61.8 ml scolices/membranes and 10.9 ml cyst fluid were obtained per pig. Suitability of collected material for the use as crude antigen and molecular diagnostic techniques was demonstrated. This study clearly shows that T. solium cyst preparation in African settings by simple field methods constitutes an effective way to obtain high quality material as source for diagnostic tools and research purposes.

Simultaneous determination of theobromine, (+)-catechin, caffeine, and (-)-epicatechin in standard reference material baking chocolate 2384, cocoa, cocoa beans, and cocoa butter.

PubMed

Risner, Charles H

2008-01-01

A reverse-phase liquid chromatography analysis is used to access the quantity of theobromine, (+)-catechin, caffeine, and (-)-epicatechin in Standard Reference Material 2384 Baking Chocolate, cocoa, cocoa beans, and cocoa butter using water or a portion of the mobile phase as the extract. The procedure requires minimal sample preparation. Theobromine, (+)-catechin, caffeine, and (-)-epicatechin are detected by UV absorption at 273 nm after separation using a 0.3% acetic acid-methanol gradient (volume fractions) and quantified using external standards. The limit of detection for theobromine, (+)-catechin, caffeine, and (-)-epicatechin averages 0.08, 0.06, 0.06, and 0.06 microg/mL, respectively. The method when applied to Standard Reference Material 2384 Baking Chocolate; baking chocolate reference material yields results that compare to two different, separate procedures. Theobromine ranges from 26000 mg/kg in cocoa to 140 mg/kg in cocoa butter; (+)-catechin from 1800 mg/kg in cocoa to below detection limits of < 32 mg/kg in cocoa butter; caffeine from 2400 mg/kg in cocoa to 400 mg/kg in cocoa butter, and (-)-epicatechin from 3200 mg/kg in cocoa to BDL, < 27 mg/kg, in cocoa butter. The mean recoveries from cocoa are 102.4 +/- 0.6% for theobromine, 100.0 +/- 0.6 for (+)-catechin, 96.2 +/- 2.1 for caffeine, and 106.2 +/- 1.7 for (-)-epicatechin.

CIVIL TECHNOLOGY, HIGHWAY AND STRUCTURAL OPTIONS, A SUGGESTED 2-YEAR POST HIGH SCHOOL CURRICULUM. TECHNICAL EDUCATION PROGRAM SERIES, NUMBER 8.

ERIC Educational Resources Information Center

BEAUMONT, JOHN A; AND OTHERS

DESIGNED TO ASSIST ADMINISTRATORS, SUPERVISORS, AND TEACHERS TO PLAN, DEVELOP, AND EVALUATE PROGRAMS, THIS CURRICULUM GUIDE OFFERS COURSE OUTLINES, PROCEDURES, LABORATORY LAYOUTS, TEXTS AND REFERENCES, LISTS OF LABORATORY EQUIPMENT AND ITS COST, AND A SELECTED LIST OF SCIENTIFIC AND TECHNICAL SOCIETIES. BASIC MATERIALS WERE PREPARED AT THE…

MECHANIZATION STUDY OF THE TECHNICAL LIBRARY U.S. NAVAL AVIONICS FACILITY, INDIANAPOLIS, INDIANA.

ERIC Educational Resources Information Center

KERSHAW, G.A.; AND OTHERS

THE NAVAL AVIONICS FACILITY, INDIANAPOLIS (NAFI) TECHNICAL LIBRARY IS PLANNING A MECHANIZED SYSTEM TO PRODUCE A PERMUTED INDEX OF PERTINENT PERIODICAL REFERENCES AND PROCEEDINGS, WITH BOOKS AND DOCUMENTS TO BE ADDED LATER. INPUT TO THE SYSTEM IS PUNCHED PAPER TAPE PREPARED FROM THE SOURCE MATERIAL, AND THE PRIMARY PROGRAM IS A "CANNED"…

Basic English Writers' Japanese-English Wordbook.

ERIC Educational Resources Information Center

Daniels, F. J.

The author of this Japanese-English wordbook suggests that it may be used by Japanese writers of English, by those translating from Japanese into English, and by learners of Japanese, in addition to its main intended uses as an aid to the preparation of teaching material and as a work of reference for teachers. A translator will need to supplement…

A review on preparation of silver nano-particles

NASA Astrophysics Data System (ADS)

Haider, Adawiya J.; Haider, Mohammad J.; Mehde, Mohammad S.

2018-05-01

The term "nano particle" (NP) refers to particle diameter in nanometers in size. Nanoparticles contain a small number of constituent atoms or molecules that differ from the properties inherent in their bulk counterparts, found in various forms such as spherical, triangular, cubic, pentagonal, rod-shaped, shells, elliptical and so on. In this chapter, it has been presented the theoretical concepts of the preparation of AgNPS as powders and collide nanoparticles, techniques of preparation with their characterization (morphology, sign charge and potential value, particle distribution ….etc.). Also, included unique properties of AgNPS that are different from those of their bulk materials like: High surface area to volume ratio effects Quantization of electronic and vibration properties.

Design and evaluation of enteric-coated tablets for rifampicin and isoniazid combinations.

PubMed

Wang, Yongjun; Liu, Hongzhuo; Liu, Kai; Sun, Jin; He, Zhonggui

2013-01-01

In order to improve the bioavailability of rifampicin (RIF) from rifampicin and isoniazid (INH) combination formulations, the physicochemical characteristics of RIF, stability of RIF in different pH buffers in the presence of INH, as well as the effect of particle size of RIF materials on the dissolution rate were investigated. On the basis of the above examinations, enteric-coated tablets for RIF and INH combinations were designed and prepared. RIF showed low solubility and high apparent distribution coefficient in the intestinal pH (pH 4.0-7.4). With the decrease in pH, the degradation of RIF increase and the presence of INH deepen the degradation. Enteric-coated tablets were prepared after grinding the RIF materials by dry granulation technique. The pharmacokinetics of RIF and INH of self-made enteric-coated tablets in dogs were studied by comparing with the reference tablets. The AUC(0-48) of RIF in both reference and test tablets were 304.77 ± 42.27 and 353.79 ± 31.63 µg·h·mL(-1), respectively. The AUC(0-48) of INH in both reference and test tablets were 17.14 ± 8.59 and 19.62 ± 10.57 µg·h·mL(-1), respectively. Enteric-coated tablets may minimize the decomposition of RIF in gastrointestinal tract and improve the bioavailability.

Preparative isolation of oligomeric procyanidins from Hawthorn (Crataegus spp.).

PubMed

Zumdick, S; Petereit, F; Luftmann, H; Hensel, A

2009-04-01

The oligomeric procyanidins (OPC) from Hawthorn leaves and flowers (Crataegi folium cum flore) are considered to be in part responsible for the cardiotonic clinical activity of the herbal material. Effective methods for rapid isolation of these heterogenous oligomeric clusters with defined molecular weight as reference compounds are not published until now. Therefore the water soluble fraction of an acetone/water (7 + 3) extract of Hawthorn leaves and flowers was fractionated by a combination of MPLC on RP-18 material and preparative HPLC using a diol stationary phase. This procedure resulted in the effective isolation of procyanidins with a distinct degree of polymerization (DP) from dimers DP2 up to tridecamers DP13. Exact mass measurements with negative ESI-TOF/MS were employed to confirm the respective structures of the isolated procyanidins.

An assessment of contemporary atomic spectroscopic techniques for the determination of lead in blood and urine matrices

NASA Astrophysics Data System (ADS)

Parsons, Patrick J.; Geraghty, Ciaran; Verostek, Mary Frances

2001-09-01

The preparation and validation of a number of clinical reference materials for the determination of lead in blood and urine is described. Four candidate blood lead reference materials (Lots, 047-050), and four candidate urine lead reference materials (Lots, 034, 035, 037 and 038), containing physiologically-bound lead at clinically relevant concentrations, were circulated to up to 21 selected laboratories specializing in this analysis. Results from two interlaboratory studies were used to establish certified values and uncertainty estimates for these reference materials. These data also provided an assessment of current laboratory techniques for the measurement of lead in blood and urine. For the blood lead measurements, four laboratories used electrothermal atomization AAS, three used anodic stripping voltammetry and one used both ETAAS and ICP-MS. For the urine lead measurements, 11 laboratories used ETAAS (most with Zeeman background correction) and 10 used ICP-MS. Certified blood lead concentrations, ±S.D., ranged from 5.9±0.4 μg/dl (0.28±0.02 μmol/l) to 76.0±2.2 μg/dl (3.67±0.11 μmol/l) and urine lead concentrations ranged from 98±5 μg/l (0.47±0.02 μmol/l) to 641±36 μg/l (3.09±0.17 μmol/l). The highest concentration blood lead material was subjected to multiple analyses using ETAAS over an extended time period. The data indicate that more stringent internal quality control practices are necessary to improve long-term precision. While the certification of blood lead materials was accomplished in a manner consistent with established practices, the urine lead materials proved more troublesome, particularly at concentrations above 600 μg/l (2.90 μmol/l).

Compositional analysis of biomass reference materials: Results from an interlaboratory study

DOE PAGES

Templeton, David W.; Wolfrum, Edward J.; Yen, James H.; ...

2015-10-29

Biomass compositional methods are used to compare different lignocellulosic feedstocks, to measure component balances around unit operations and to determine process yields and therefore the economic viability of biomass-to-biofuel processes. Four biomass reference materials (RMs NIST 8491–8494) were prepared and characterized, via an interlaboratory comparison exercise in the early 1990s to evaluate biomass summative compositional methods, analysts, and laboratories. Having common, uniform, and stable biomass reference materials gives the opportunity to assess compositional data compared to other analysts, to other labs, and to a known compositional value. The expiration date for the original characterization of these RMs was reached andmore » an effort to assess their stability and recharacterize the reference values for the remaining material using more current methods of analysis was initiated. We sent samples of the four biomass RMs to 11 academic, industrial, and government laboratories, familiar with sulfuric acid compositional methods, for recharacterization of the component reference values. In this work, we have used an expanded suite of analytical methods that are more appropriate for herbaceous feedstocks, to recharacterize the RMs’ compositions. We report the median values and the expanded uncertainty values for the four RMs on a dry-mass, whole-biomass basis. The original characterization data has been recalculated using median statistics to facilitate comparisons with this data. We found improved total component closures for three out of the four RMs compared to the original characterization, and the total component closures were near 100 %, which suggests that most components were accurately measured and little double counting occurred. Here, the major components were not statistically different in the recharacterization which suggests that the biomass materials are stable during storage and that additional components, not seen in the original characterization, were quantified here.« less

Survey material choices in haematology EQA: a confounding factor in automated counting performance assessment.

PubMed

De la Salle, Barbara

2017-02-15

The complete blood count (CBC) is one of the most frequently requested tests in laboratory medicine, performed in a range of healthcare situations. The provision of an ideal assay material for external quality assessment is confounded by the fragility of the cellular components of blood, the lack of commutability of stabilised whole blood material and the lack of certified reference materials and methods to which CBC results can be traced. The choice of assay material between fresh blood, extended life assay material and fully stabilised, commercially prepared, whole blood material depends upon the scope and objectives of the EQA scheme. The introduction of new technologies in blood counting and the wider clinical application of parameters from the extended CBC will bring additional challenges for the EQA provider.

The use of reference materials in quality assurance programmes in food microbiology laboratories.

PubMed

In't Veld, P H

1998-11-24

Nine different reference materials (RMs) for use in food and water microbiology have been developed with the support of the European Commission (EC). The production process of RMs is based on spray drying bacteria suspended in milk. The highly contaminated milk powder (HCMP) obtained is mixed with sterile milk powder to achieve the desired level of contamination and is subsequently filled into gelatine capsules. The HCMP may need to be stabilised by storage for more than a year before a stable RM can be prepared. The HCMP are mixed with sterile milk powder using a pestle and mortar in order to produce homogeneous RMs. For routine use of RMs Shewhart control charts can be produced. Based on log10 transformed counts, control limits are calculated. Rules for the interpretation of results facilitate the detection of out of control situations. Besides RMs there are also CRMs (Certified Reference Materials) that are certified by the EC Community Bureau of Reference (BCR) and are intended for occasional use. Based on the BCR certificate, user tables are produced presenting the 95% confidence limits for the number of capsules likely to be examined in practice. Also power analysis is made to indicate the minimum difference between the certified value and the observed geometric mean value in relation to the number of capsules examined.

Encapsulated Vanadium-Based Hybrids in Amorphous N-Doped Carbon Matrix as Anode Materials for Lithium-Ion Batteries.

PubMed

Long, Bei; Balogun, Muhammad-Sadeeq; Luo, Lei; Luo, Yang; Qiu, Weitao; Song, Shuqin; Zhang, Lei; Tong, Yexiang

2017-11-01

Recently, researchers have made significant advancement in employing transition metal compound hybrids as anode material for lithium-ion batteries and developing simple preparation of these hybrids. To this end, this study reports a facile and scalable method for fabricating a vanadium oxide-nitride composite encapsulated in amorphous carbon matrix by simply mixing ammonium metavanadate and melamine as anode materials for lithium-ion batteries. By tuning the annealing temperature of the mixture, different hybrids of vanadium oxide-nitride compounds are synthesized. The electrode material prepared at 700 °C, i.e., VM-700, exhibits excellent cyclic stability retaining 92% of its reversible capacity after 200 cycles at a current density of 0.5 A g -1 and attractive rate performance (220 mAh g -1 ) under the current density of up to 2 A g -1 . The outstanding electrochemical properties can be attributed to the synergistic effect from heterojunction form by the vanadium compound hybrids, the improved ability of the excellent conductive carbon for electron transfer, and restraining the expansion and aggregation of vanadium oxide-nitride in cycling. These interesting findings will provide a reference for the preparation of transition metal oxide and nitride composites as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enantioseparation of omeprazole--effect of different packing particle size on productivity.

PubMed

Enmark, Martin; Samuelsson, Jörgen; Forssén, Patrik; Fornstedt, Torgny

2012-06-01

Enantiomeric separation of omeprazole has been extensively studied regarding both product analysis and preparation using several different chiral stationary phases. In this study, the preparative chiral separation of omeprazole is optimized for productivity using three different columns packed with amylose tris (3,5-dimethyl phenyl carbamate) coated macroporous silica (5, 10 and 25 μm) with a maximum allowed pressure drop ranging from 50 to 400 bar. This pressure range both covers low pressure process systems (50-100 bar) and investigates the potential for allowing higher pressure limits in preparative applications in a future. The process optimization clearly show that the larger 25 μm packing material show higher productivity at low pressure drops whereas with increasing pressure drops the smaller packing materials have substantially higher productivity. Interestingly, at all pressure drops, the smaller packing material result in lower solvent consumption (L solvent/kg product); the higher the accepted pressure drop, the larger the gain in reduced solvent consumption. The experimental adsorption isotherms were not identical for the different packing material sizes; therefore all calculations were recalculated and reevaluated assuming identical adsorption isotherms (with the 10 μm isotherm as reference) which confirmed the trends regarding productivity and solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.

[The application of inductively coupled plasma atomic emission spectrometry/mass spectrometry to the analysis of advanced ceramic materials].

PubMed

Wang, Zheng; Wang, Shi-Wei; Qiu, De-Ren; Yang, Peng-Yuan

2009-10-01

Advanced ceramics have been applied to various important fields such as information science, aeronautics and astronautics, and life sciences. However, the optics and electric properties of ceramics are significantly affected by the micro and trace impurities existing in the material even at very low concentration level. Thus, the accurate determination of impurities is important for materials preparation and performance. Methodology of the analysis of advanced ceramic materials using ICP-AES/MS was reviewed in the present paper for the past decade. Various techniques of sample introduction, especially advances in the authors' recent work, are described in detail. The developing trend is also presented. Sixty references are cited.

The Third International Reference Preparation of Egg Lecithin

PubMed Central

Krag, P.; Bentzon, M. Weis

1961-01-01

The Third International Reference Preparation of Egg Lecithin was produced (in a quantity of 5000 ml) at the WHO Serological Reference Centre, Copenhagen, and assayed in 1958 against the Second International Reference Preparation by four laboratories in three countries. Complement-fixation and slide-flocculation tests were used. The new preparation was found acceptable, and its establishment was authorized by the WHO Expert Committee on Biological Standardization. The average log10 titres and results of analyses of variances are shown. The variances were of the usual order of magnitude, and the differences in titre between antigens containing the Second and the Third International Reference Preparations varied from -0.011 to 0.116; only one of the differences exceeded the 5% limit of significance. The use of the Third International Reference Preparation in tests for the acceptability of lecithin preparations is described. PMID:13753864

Preparation and value assignment of standard reference material 968e fat-soluble vitamins, carotenoids, and cholesterol in human serum.

PubMed

Thomas, Jeanice B; Duewer, David L; Mugenya, Isaac O; Phinney, Karen W; Sander, Lane C; Sharpless, Katherine E; Sniegoski, Lorna T; Tai, Susan S; Welch, Michael J; Yen, James H

2012-01-01

Standard Reference Material 968e Fat-Soluble Vitamins, Carotenoids, and Cholesterol in Human Serum provides certified values for total retinol, γ- and α-tocopherol, total lutein, total zeaxanthin, total β-cryptoxanthin, total β-carotene, 25-hydroxyvitamin D(3), and cholesterol. Reference and information values are also reported for nine additional compounds including total α-cryptoxanthin, trans- and total lycopene, total α-carotene, trans-β-carotene, and coenzyme Q(10). The certified values for the fat-soluble vitamins and carotenoids in SRM 968e were based on the agreement of results from the means of two liquid chromatographic methods used at the National Institute of Standards and Technology (NIST) and from the median of results of an interlaboratory comparison exercise among institutions that participate in the NIST Micronutrients Measurement Quality Assurance Program. The assigned values for cholesterol and 25-hydroxyvitamin D(3) in the SRM are the means of results obtained using the NIST reference method based upon gas chromatography-isotope dilution mass spectrometry and liquid chromatography-isotope dilution tandem mass spectrometry, respectively. SRM 968e is currently one of two available health-related NIST reference materials with concentration values assigned for selected fat-soluble vitamins, carotenoids, and cholesterol in human serum matrix. This SRM is used extensively by laboratories worldwide primarily to validate methods for determining these analytes in human serum and plasma and for assigning values to in-house control materials. The value assignment of the analytes in this SRM will help support measurement accuracy and traceability for laboratories performing health-related measurements in the clinical and nutritional communities.

EMP Interaction: Principles, Techniques and Reference Data (A Compleat concatenation of Technology from the EMP Interaction Notes). EMP Interaction 2-1

DTIC Science & Technology

1980-12-01

staff of Dikewood, Santa Monica, no. only has contributed a large amount of material to this document, but also proofread the typescript . In...assistance and skills in the preparation of the entire typescript . Dikewood Industries, Inc. K.S.H. LEE Santa Monica, California September, 1979 xJ

Literature Related to Planning, Design and Construction of Science Facilities.

ERIC Educational Resources Information Center

National Science Foundation, Washington, DC.

A list of the articles and papers in the science facilities collection of the Architectural Services Staff is presented. It has been prepared to serve as a bibliography that may be useful to persons searching for data on the design of science facilities, and as a means of informing such persons of the material available for reference in the…

Characterization of Ricin and R. communis Agglutinin Reference Materials.

PubMed

Worbs, Sylvia; Skiba, Martin; Söderström, Martin; Rapinoja, Marja-Leena; Zeleny, Reinhard; Russmann, Heiko; Schimmel, Heinz; Vanninen, Paula; Fredriksson, Sten-Åke; Dorner, Brigitte G

2015-11-26

Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon "gold standards" are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120), a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS), and matrix-assisted laser desorption ionization-time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test.

Characterization of Ricin and R. communis Agglutinin Reference Materials

PubMed Central

Worbs, Sylvia; Skiba, Martin; Söderström, Martin; Rapinoja, Marja-Leena; Zeleny, Reinhard; Russmann, Heiko; Schimmel, Heinz; Vanninen, Paula; Fredriksson, Sten-Åke; Dorner, Brigitte G.

2015-01-01

Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon “gold standards” are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120), a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS), and matrix-assisted laser desorption ionization–time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test. PMID:26703723

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

PubMed

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

2014-12-03

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

Development of a standard reference material containing 22 chlorinated hydrocarbon gases at 1 μmol/mol in nitrogen.

PubMed

Li, Ning; Du, Jian; Yang, Jing; Fan, Qiang; Tian, Wen

2017-11-01

A gas standard mixture containing 22 chlorinated hydrocarbons in high purity nitrogen was prepared using a two-step weighing method and a gasifying apparatus developed in-house. The concentration of each component was determined using a gas chromatograph with flame ionization detection (GC/FID). Linear regression analysis of every component was performed using the gas standard mixture with concentrations ranging from 1 to 10 μmol/mol, showing the complete gasification of volatile organic compound (VOCs) species in a selected cylinder. Repeatability was also examined to ensure the reliability of the preparation method. In addition, no significant difference was observed between domestic treated and imported treated cylinders, which were conducive to reduction of the cost of raw materials. Moreover, the results of stability testing at different pressures and long-term stability tests indicated that the gas standard at 1 μmol/mol level with relative expanded uncertainties of 5% was stable above 2 MPa for a minimum of 12 months. Finally, a quantity comparison was conducted between the gas standard and a commercial gas standard from Scott Specialty Gases (now Air Liquide America Specialty Gases). The excellent agreement of every species suggested the favorable accuracy of our gas standard. Therefore, this reference material can be applied to routine observation of VOCs and for other purposes.

Criticality Safety Evaluation for Small Sample Preparation and Non-Destructive Assay (NDA) Operations in Wing 7 Basement of the CMR Facility

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

Kunkle, Paige Elizabeth; Zhang, Ning

Nuclear Criticality Safety (NCS) has reviewed the fissionable material small sample preparation and NDA operations in Wing 7 Basement of the CMR Facility. This is a Level-1 evaluation conducted in accordance with NCS-AP-004 [Reference 1], formerly NCS-GUIDE-01, and the guidance set forth on use of the Standard Criticality Safety Requirements (SCSRs) [Reference 2]. As stated in Reference 2, the criticality safety evaluation consists of both the SCSR CSED and the SCSR Application CSED. The SCSR CSED is a Level-3 CSED [Reference 3]. This Level-1 CSED is the SCSR Application CSED. This SCSR Application (Level-1) evaluation does not derive controls, itmore » simply applies controls derived from the SCSR CSED (Level-3) for the application of operations conducted here. The controls derived in the SCSR CSED (Level-3) were evaluated via the process described in Section 6.6.5 of SD-130 (also reproduced in Section 4.3.5 of NCS-AP-004 [Reference 1]) and were determined to not meet the requirements for consideration of elevation into the safety basis documentation for CMR. According to the guidance set forth on use of the SCSRs [Reference 2], the SCSR CSED (Level-3) is also applicable to the CMR Facility because the process and the normal and credible abnormal conditions in question are bounded by those that are described in the SCSR CSED. The controls derived in the SCSR CSED include allowances for solid materials and solution operations. Based on the operations conducted at this location, there are less-than-accountable (LTA) amounts of 233U. Based on the evaluation documented herein, the normal and credible abnormal conditions that might arise during the execution of this process will remain subcritical with the following recommended controls.« less

Homogeneity of the geochemical reference material BRP-1 (paraná basin basalt) and assessment of minimum mass

USGS Publications Warehouse

Cotta, Aloisio J. B.; Enzweiler, Jacinta; Wilson, Stephen A.; Perez, Carlos A.; Nardy, Antonio J. R.; Larizzatti, Joao H.

2007-01-01

Reference materials (RM) are required for quantitative analyses and their successful use is associated with the degree of homogeneity, and the traceability and confidence limits of the values established by characterisation. During the production of a RM, the chemical characterisation can only commence after it has been demonstrated that the material has the required level of homogeneity. Here we describe the preparation of BRP-1, a proposed geochemical reference material, and the results of the tests to evaluate its degree of homogeneity between and within bottles. BRP-1 is the first of two geochemical RM being produced by Brazilian institutions in collaboration with the United States Geological Survey (USGS) and the International Association of Geoanalysts (IAG). Two test portions of twenty bottles of BRP-1 were analysed by wavelength dispersive-XRF spectrometry and major, minor and eighteen trace elements were determined. The results show that for most of the investigated elements, the units of BRP-1 were homogeneous at conditions approximately three times more rigorous than those strived for by the test of “sufficient homogeneity”. Furthermore, the within bottle homogeneity of BRP-1 was evaluated using small beam (1 mm2) synchrotron radiation XRF spectrometry and, for comparison, the USGS reference materials BCR-2 and GSP-2 were also evaluated. From our data, it has been possible to assign representative minimum masses for some major constituents (1 mg) and for some trace elements (1-13 mg), except Zr in GSP-2, for which test portions of 74 mg are recommended.

Biological and chemical sensors based on graphene materials.

PubMed

Liu, Yuxin; Dong, Xiaochen; Chen, Peng

2012-03-21

Owing to their extraordinary electrical, chemical, optical, mechanical and structural properties, graphene and its derivatives have stimulated exploding interests in their sensor applications ever since the first isolation of free-standing graphene sheets in year 2004. This article critically and comprehensively reviews the emerging graphene-based electrochemical sensors, electronic sensors, optical sensors, and nanopore sensors for biological or chemical detection. We emphasize on the underlying detection (or signal transduction) mechanisms, the unique roles and advantages of the used graphene materials. Properties and preparations of different graphene materials, their functionalizations are also comparatively discussed in view of sensor development. Finally, the perspective and current challenges of graphene sensors are outlined (312 references).

Establishment of a biological reference preparation for hepatitis A vaccine (inactivated, non-adsorbed).

PubMed

Stalder, J; Costanzo, A; Daas, A; Rautmann, G; Buchheit, K-H

2010-04-01

A reference standard calibrated in International Units (IU) is needed for the in vitro potency assay of hepatitis A vaccines prepared by formalin-inactivation of purified hepatitis A virus grown in cell cultures. Thus, a project was launched by the European Directorate for the Quality of Medicines & HealthCare (EDQM) to establish one or more non-adsorbed inactivated hepatitis A vaccine reference preparation(s) as working standard(s), calibrated against the 1st International Standard (IS), for the in vitro potency assay (ELISA) of all vaccines present on the European market. Four non-adsorbed liquid preparations of formalin-inactivated hepatitis A antigen with a known antigen content were obtained from 3 manufacturers as candidate Biological Reference Preparations (BRPs). Thirteen laboratories participated in the collaborative study. They were asked to use an in vitro ELISA method adapted from a commercially available kit for the detection of antibodies to hepatitis A virus. In-house validated assays were to be run in parallel, where available. Some participants also included commercially available hepatitis A vaccines in the assays, after appropriate desorption. During the collaborative study, several participants using the standard method were faced with problems with some of the most recent lots of the test kits. Due to these problems, the standard method did not perform satisfactorily and a high number of assays were invalid, whereas the in-house methods appeared to perform better. Despite this, the overall mean results of the valid assays using both methods were in agreement. Nonetheless, it was decided to base the assignment of the potency values on the in-house methods only. The results showed that all candidate BRPs were suitable for the intended purpose. However, based on availability of the material and on the results of end-product testing, 2 candidate reference preparations, Samples C and D, were selected. Both were from the same batch but filled on different days; no statistically significant difference in potency was observed. They were thus combined in 1 single batch. The candidate preparation (Sample C/D) was adopted at the June 2009 session of the European Pharmacopoeia (Ph. Eur.) Commission as the Ph. Eur. BRP batch 1 for hepatitis A vaccine (inactivated, non-adsorbed), with an assigned potency of 12 IU/ml for in vitro antigen content assays. Accelerated degradation studies have been initiated. The preliminary data show that the BRP is stable at the recommended storage temperature (< -50 degrees C). The BRP will be monitored at regular intervals throughout its lifetime.

Applications of New Synthetic Uranium Reference Materials for Geochemistry Research (Invited)

NASA Astrophysics Data System (ADS)

Richter, S.; Weyer, S.; Alonso, A.; Aregbe, Y.; Kuehn, H.; Eykens, R.; Verbruggen, A.; Wellum, R.

2009-12-01

For many applications in geochemistry research isotope ratio measurements play a significant role. In geochronology isotope abundances of uranium and its daughter products thorium and lead are being used to determine the age and history of various samples of geological interest. For measuring the isotopic compositions of these elements by mass spectrometry, suitable isotope reference materials are needed to validate measurement procedures and to calibrate multi-collector and ion counting detector systems. IRMM is a recognized provider for nuclear isotope reference materials to the nuclear industry and nuclear safeguards authorities, which are also being applied widely for geochemical applications. The preparation of several new synthetic uranium reference materials at IRMM during the recent five years has provided significant impacts on geochemical research. As an example, the IRMM-074 series of gravimetrically prepared uranium mixtures for linearity testing of secondary electron multipliers (SEMs) has been applied for the redetermination of the secular equilibrium 234U/238U value and the 234U half-life by Cheng et al (2009). Due to the use of IRMM-074, results with smaller uncertainties were obtained, which are shifted by about 0.04% compared to the commonly used values published earlier by Cheng et al. in 2000. This has a significant impact for U isotope measurements in geochemistry.. As a further example, the new double spike IRMM-3636 with a 233U/236U ratio of 1:1 and an expanded uncertainty as low as 0.016% (coverage factor k=2, 95% confidence level) was prepared gravimetrically. This double spike allows internal mass fractionation correction for high precision 235U/238U ratio measurements of close to natural samples. Using the new double spike IRMM-3636, the 235U/238U ratios for several commonly used natural U standard materials from NIST/NBL and IRMM, such as e.g. NBS960 (=NBL CRM-112a), NBS950a,b and IRMM-184, have been re-measured with improved precision and accuracy. The (preliminary) result of 137.836(23) for the 238U/235U ratio of NBS960, measured using the new gravimetrically prepared 233U/236U-Double Spike IRMM-3636, is deviating by -0.032% from the well-known and widely used consensus value of 137.88. For the consensus value no uncertainty has ever been assigned, but it is outside the uncertainty limits of the new measurement result. The re-measured 238U/235U ratio of 137.689(22) of IRMM-184 agrees quite well with the certified value of 137.697(41), the calculated difference is only -0.006(34)% which is insignificant. The results for both NBS960 and IRMM-184, obtained using multi-dynamic TIMS at IRMM and using high efficiency MC-ICPMS at the University of Frankfurt, agree well with each other. As a conclusion, the IRMM-3636 Double Spike has been successfully applied for measurements of important uranium isotopic standards like NBS960 and IRMM-184, with improved uncertainties at the level of 0.016%.

Proof of concept testing of a positive reference material for in vivo and in vitro skin irritation testing.

PubMed

Nomura, Yusuke; Lee, Michelle; Fukui, Chie; Watanabe, Kayo; Olsen, Daniel; Turley, Audrey; Morishita, Yuki; Kawakami, Tsuyoshi; Yuba, Toshiyasu; Fujimaki, Hideo; Inoue, Kaoru; Yoshida, Midori; Ogawa, Kumiko; Haishima, Yuji

2017-12-11

In vivo and in vitro irritation testing is important for evaluating the biological safety of medical devices. Here, the performance of positive reference materials for skin irritation testing was evaluated. Four reference standards, referred to as Y-series materials, were analyzed: a polyvinyl chloride (PVC) sheet spiked with 0 (Y-1), 1.0 (Y-2), 1.5 (Y-3), or 10 (Y-4) parts of Genapol X-080 per 100 parts of PVC by weight. Y-1, Y-2, and Y-3 did not induce skin irritation responses in an in vitro reconstructed human epidermis (RhE) tissue model, as measured by tissue viability or interleukin-1α release, or in an in vivo intracutaneous response test using rabbits. In contrast, Y-4 extracts prepared with saline or sesame oil at 37°C and 50°C clearly elicited positive irritation responses, including reduced viability (< 50%) and significantly higher interleukin-1α release compared with the solvent alone group, in the RhE tissue model and an intracutaneous response test, where substantial necrosis was observed by histopathology. The positive skin irritation responses induced in vitro under various extraction conditions, as well as those elicited in vivo, indicate that Y-4 is an effective extractable positive control material for in vivo and in vitro skin irritation tests of medical devices. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2017. © 2017 Wiley Periodicals, Inc.

Comparison of δ18O measurements in nitrate by different combustion techniques

USGS Publications Warehouse

Revesz, Kinga; Böhlke, John Karl

2002-01-01

Three different KNO3 salts with δ18O values ranging from about −31 to +54‰ relative to VSMOW were used to compare three off-line, sealed glass tube combustion methods (widely used for isotope studies) with a more recently developed on-line carbon combustion technique. All methods yielded roughly similar isotope ratios for KNO3 samples with δ18O values in the midpoint of the δ18O scale near that of the nitrate reference material IAEA-NO-3 (around +21 to +25‰). This reference material has been used previously for one-point interlaboratory and intertechnique calibrations. However, the isotope ratio scale factors by all of the off-line combustion techniques are compressed such that they are between 0.3 and 0.7 times that of the on-line combustion technique. The contraction of the δ18O scale in the off-line preparations apparently is caused by O isotope exchange between the sample and the glass combustion tubes. These results reinforce the need for nitrate reference materials with δ18O values far from that of atmospheric O2, to improve interlaboratory comparability.

Preparation and provisional certification of NBL Spectrographic Impurity Standards, CRM 123 (1-7) and 124 (1-7)

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

Santoliquido, P.M.

This report describes the design, production, and provisional certification of two new certified reference materials (CRMs): CRM No. 123 (1-7), U/sub 3/O/sub 8/ containing 18 trace elements, and CRM No. 124 (1-7), U/sub 3/O/sub 8/ containing 24 trace elements. The elements to be included and concentrations to be used were decided on the basis of information gathered from users of a previous CRM of this type, CRM No. 98 (1-7). The new CRMs were prepared by the addition of trace elements to high purity U/sub 3/O/sub 8/. Provisional certification was accomplished by an interlaboratory program in which four different laboratoriesmore » analyzed the materials by carrier distillation dc arc emission spectrography.« less

Visible light photoactivity of Polypropylene coated Nano-TiO2 for dyes degradation in water

PubMed Central

Giovannetti, R.; Amato, C. A. D’; Zannotti, M.; Rommozzi, E.; Gunnella, R.; Minicucci, M.; Di Cicco, A.

2015-01-01

The use of Polypropylene as support material for nano-TiO2 photocatalyst in the photodegradation of Alizarin Red S in water solutions under the action of visible light was investigated. The optimization of TiO2 pastes preparation using two commercial TiO2, Aeroxide P-25 and Anatase, was performed and a green low-cost dip-coating procedure was developed. Scanning electron microscopy, Atomic Force Microscopy and X-Ray Diffraction analysis were used in order to obtain morphological and structural information of as-prepared TiO2 on support material. Equilibrium and kinetics aspects in the adsorption and successive photodegradation of Alizarin Red S, as reference dye, are described using polypropylene-TiO2 films in the Visible/TiO2/water reactor showing efficient dyes degradation. PMID:26627118

Ultrapure glass optical waveguide development in microgravity by the sol-gel process

NASA Technical Reports Server (NTRS)

Mukherjee, S. P.; Holman, R. A.

1981-01-01

Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process referred to here is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation. The use of gels offers several advantages such as high purity and lower melting times and temperatures. The sol-gel process is studied for utilization in the preparation of multicomponent ultrapure glass batches for subsequent containerless melting of the batches in space to prepare glass blanks for optical waveguides.

Patch testing custom isocyanate materials from the workplace.

PubMed

Burrows, Dianne; Houle, Marie-Claude; Holness, D Linn; DeKoven, Joel; Skotnicki, Sandy

2015-01-01

Patch testing with standard trays of commercially available allergens is the current practice for investigating suspected cases of isocyanate-induced allergic contact dermatitis (ACD). In some facilities, these standard trays are further supplemented with custom preparations of isocyanate-containing materials. The aim was to determine whether added value exists in patch testing patients to custom isocyanate preparations in suspected cases of ACD. We performed a retrospective analysis of 11 patients referred to our specialty clinic between January 2003 and March 2011 for suspected patients of ACD who had custom testing with isocyanate materials from their workplace. In addition to standard trays of allergens, all patients were patch tested with custom isocyanate materials from their workplaces. Three (27%) of 11 patients showed an added value in testing to custom isocyanate allergens. Of these 3 patients, one had a reaction that reinforced positive reactions to the standard isocyanate tray, but the other 2 (18%) had no reactions to any of the commercially available allergens. Because of the high proportion of reactions (27%), we recommend the use of custom testing to workplace isocyanate products as a supplement to current standard patch testing procedures.

Analysis of street drugs in seized material without primary reference standards.

PubMed

Laks, Suvi; Pelander, Anna; Vuori, Erkki; Ali-Tolppa, Elisa; Sippola, Erkki; Ojanperä, Ilkka

2004-12-15

A novel approach was used to analyze street drugs in seized material without primary reference standards. Identification was performed by liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS), essentially based on accurate mass determination using a target library of 735 exact monoisotopic masses. Quantification was carried out by liquid chromatography/chemiluminescence nitrogen detection (LC/CLND) with a single secondary standard (caffeine), utilizing the detector's equimolar response to nitrogen. Sample preparation comprised dilution, first with methanol and further with the LC mobile phase. Altogether 21 seized drug samples were analyzed blind by the present method, and results were compared to accredited reference methods utilizing identification by gas chromatography/mass spectrometry and quantification by gas chromatography or liquid chromatography. The 31 drug findings by LC/TOFMS comprised 19 different drugs-of-abuse, byproducts, and adulterants, including amphetamine and tryptamine designer drugs, with one unresolved pair of compounds having an identical mass. By the reference methods, 27 findings could be confirmed, and among the four unconfirmed findings, only 1 apparent false positive was found. In the quantitative analysis of 11 amphetamine, heroin, and cocaine findings, mean relative difference between the results of LC/CLND and the reference methods was 11% (range 4.2-21%), without any observable bias. Mean relative standard deviation for three parallel LC/CLND results was 6%. Results suggest that the present combination of LC/TOFMS and LC/CLND offers a simple solution for the analysis of scheduled and designer drugs in seized material, independent of the availability of primary reference standards.

Long-term stability and temporal trends of organic contaminants in four collections of mussel tissue frozen standard reference materials.

PubMed

Schantz, Michele M; Pugh, Rebecca S; Pol, Stacy S Vander; Wise, Stephen A

2015-04-01

The stability of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and chlorinated pesticides in frozen mussel tissue Standard Reference Materials (SRMs) stored at -80 °C was assessed by analyzing samples of SRM 1974, SRM 1974a, and SRM 1974b Organics in Mussel Tissue (Mytilus edulis) periodically over 25 y, 20 y, and 12 y, respectively. The most recent analyses were performed during the certification of the fourth release of this material, SRM 1974c. Results indicate the concentrations of these persistent organic pollutants have not changed during storage at -80 °C. In addition, brominated diphenyl ethers (BDEs) were quantified in each of the materials during this study. The stability information is important for on-going monitoring studies collecting large quantities of samples for future analyses (i.e., formally established specimen banking programs). Since all four mussel tissue SRMs were prepared from mussels collected at the same site in Dorchester Bay, MA, USA, the results provide a temporal trend study for these contaminants over a 17 year period (1987 to 2004).

Oxygen isotopes in nitrate: New reference materials for 18O:17O:16O measurements and observations on nitrate-water equilibration

USGS Publications Warehouse

Böhlke, J.K.; Mroczkowski, S.J.; Coplen, T.B.

2003-01-01

Despite a rapidly growing literature on analytical methods and field applications of O isotope-ratio measurements of NO3− in environmental studies, there is evidence that the reported data may not be comparable because reference materials with widely varying δ18O values have not been readily available. To address this problem, we prepared large quantities of two nitrate salts with contrasting O isotopic compositions for distribution as reference materials for O isotope-ratio measurements: USGS34 (KNO3) with low δ18O and USGS35 (NaNO3) with high δ18O and ‘mass-independent’ δ17O. The procedure used to produce USGS34 involved equilibration of HNO3 with 18O-depleted meteoric water. Nitric acid equilibration is proposed as a simple method for producing laboratory NO3− reference materials with a range of δ18O values and normal (mass-dependent) 18O:17O:16O variation. Preliminary data indicate that the equilibrium O isotope-fractionation factor (α) between [NO3−] and H2O decreases with increasing temperature from 1.0215 at 22°C to 1.0131 at 100°C. USGS35 was purified from the nitrate ore deposits of the Atacama Desert in Chile and has a high 17O:18O ratio owing to its atmospheric origin. These new reference materials, combined with previously distributed NO3− isotopic reference materials IAEA-N3 (=IAEA-NO-3) and USGS32, can be used to calibrate local laboratory reference materials for determining offset values, scale factors, and mass-independent effects on N and O isotope-ratio measurements in a wide variety of environmental NO3− samples. Preliminary analyses yield the following results (normalized with respect to VSMOW and SLAP, with reproducibilities of ±0.2–0.3‰, 1σ): IAEA-N3 has δ18O = +25.6‰ and δ17O = +13.2‰; USGS32 has δ18O = +25.7‰; USGS34 has δ18O = −27.9‰ and δ17O = −14.8‰; and USGS35 has δ18O = +57.5‰ and δ17O = +51.5‰.

Just Watch What I'm Saying: A Television Teaching Course for the Deaf and the Hard of Hearing.

ERIC Educational Resources Information Center

Wermer, F. E.

1969-01-01

The Netherlands Television Academy Foundation prepared a weekly television series intended to teach lip reading to the deaf and to the hard of hearing. This article outlines the scope of this project, referring to the format of the 18 half-hour lessons, to the supplementary written materials employed, to the nature of the criticism received, and…

Troubleshooting, Section Two, Boilers: Flame Reading. Part 4, Air Pollution Training Institute Self-Instructional Course SI-466.

ERIC Educational Resources Information Center

Environmental Protection Agency, Research Triangle Park, NC. Air Pollution Training Inst.

This workbook is part four of a self-instructional course prepared for the United States Environmental Protection Agency. The student proceeds at his own pace and when questions are asked, after answering, he either turns to the next page to check his response or refers to the previously covered material. The purpose of this course is to prepare…

Correction: Hood, M.A., et al. Synthetic Strategies in the Preparation of Polymer/Inorganic Hybrid Nanoparticles. Materials 2014, 7, 4057-4087.

PubMed

Office, Materials Editorial

2014-11-24

In [1], several sentences were repeated three times on pages 4062, 4063 and 4065. In addition, many references were incorrect. The errors were introduced by the editorial office during the editing process. We apologize for this mistake and any inconvenience this may have caused to authors and readers. The corrected manuscript is given below.[...].

JPRS Report, Science & Technology, USSR: Science & Technology Policy

DTIC Science & Technology

1988-09-23

number of library personnel for preparing survey -analyt- ical references, but by equipping them with modern computer hardware for acquiring information...of manpower, material, technical, and financial resources and limits of capital investments and planning, surveying , and contractual work, which...USSR State Prize for the development and introduction of a technology of the production of shampoo from fish protein. During the period under review

A comparative study of 129I content in environmental standard materials IAEA-375, NIST SRM 4354 and NIST SRM 4357 by Thermal Ionization Mass Spectrometry and Accelerator Mass Spectrometry

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

Olson, John; Adamic, Mary; Snyder, Darin

Iodine environmental measurements have consistently been backed up in the literature by standard materials like IAEA-375, Chernobyl Soil. There are not many other sources of a certified reference material for 129I content for mass spectrometry measurements. Some that have been found in the literature include NIST-4354 and NIST-4357. They are still available at the time of this writing. They don’t have certified content or isotopic values. There has been some work in the literature to show that iodine is present, but there hasn’t been enough to establish a consensus value. These materials have been analyzed at INL through two separatemore » mass spectrometry techniques. They involve a combustion method of the starting material in oxygen, followed by TIMS analysis and a leaching preparation analyzed by accelerator mass spectrometry. Combustion/TIMS preparation of NIST SRM-4354 resulted in a 129I/127I ratio of 1.92 x 10-6 which agrees with AMS measurements which measured the 129I/127I ratio to be 1.93 x 10-6.« less

Actuating materials. Voxelated liquid crystal elastomers.

PubMed

Ware, Taylor H; McConney, Michael E; Wie, Jeong Jae; Tondiglia, Vincent P; White, Timothy J

2015-02-27

Dynamic control of shape can bring multifunctionality to devices. Soft materials capable of programmable shape change require localized control of the magnitude and directionality of a mechanical response. We report the preparation of soft, ordered materials referred to as liquid crystal elastomers. The direction of molecular order, known as the director, is written within local volume elements (voxels) as small as 0.0005 cubic millimeters. Locally, the director controls the inherent mechanical response (55% strain) within the material. In monoliths with spatially patterned director, thermal or chemical stimuli transform flat sheets into three-dimensional objects through controlled bending and stretching. The programmable mechanical response of these materials could yield monolithic multifunctional devices or serve as reconfigurable substrates for flexible devices in aerospace, medicine, or consumer goods. Copyright © 2015, American Association for the Advancement of Science.

Dielectric elastomers with novel highly-conducting electrodes

NASA Astrophysics Data System (ADS)

Böse, Holger; Uhl, Detlev

2013-04-01

Beside the characteristics of the elastomer material itself, the performance of dielectric elastomers in actuator, sensor as well as generator applications depends also on the properties of the electrode material. Various electrode materials based on metallic particles dispersed in a silicone matrix were manufactured and investigated. Anisotropic particles such as silver-coated copper flakes and silver-coated glass flakes were used for the preparation of the electrodes. The concentration of the metallic particles and the thickness of the electrode layers were varied. Specific conductivities derived from resistance measurements reached about 100 S/cm and surmount those of the reference materials based on graphite and carbon black by up to three orders of magnitude. The high conductivities of the new electrode materials can be maintained even at very large stretch deformations up to 200 %.

Properties of PMR Polyimides Improved by Preparation of Polyhedral Oligomeric Silsesquioxane (POSS) Nanocomposites

NASA Technical Reports Server (NTRS)

Campbell, Sandi G.; Lee, Andre

2005-01-01

The field of hybrid organic-inorganic materials has grown drastically over the last several years. This interest stems from our ever-increasing ability to custom-build and control molecular structure at several length scales. This ability to control both the composition and structure of hybrid materials is sometimes broadly referred to as nanocomposite systems. One class of hybrid (organic-inorganic) nanostructured material is polyhedral oligomeric silsesquioxane (POSS), shown in the preceding diagram. The hybrid composition gives POSS materials dramatically enhanced properties relative to traditional hydrocarbons and inorganics. An important benefit of this technology is that it makes possible the formulations of nanostructured chemicals with excellent thermal and oxidative stability. This is largely due to the inorganic component.

USGS42 and USGS43: Human-hair stable hydrogen and oxygen isotopic reference materials and analytical methods for forensic science and implications for published measurement results

USGS Publications Warehouse

Coplen, T.B.; Qi, H.

2012-01-01

Because there are no internationally distributed stable hydrogen and oxygen isotopic reference materials of human hair, the U.S. Geological Survey (USGS) has prepared two such materials, USGS42 and USGS43. These reference materials span values commonly encountered in human hair stable isotope analysis and are isotopically homogeneous at sample sizes larger than 0.2 mg. USGS42 and USGS43 human-hair isotopic reference materials are intended for calibration of δ(2)H and δ(18)O measurements of unknown human hair by quantifying (1) drift with time, (2) mass-dependent isotopic fractionation, and (3) isotope-ratio-scale contraction. While they are intended for measurements of the stable isotopes of hydrogen and oxygen, they also are suitable for measurements of the stable isotopes of carbon, nitrogen, and sulfur in human and mammalian hair. Preliminary isotopic compositions of the non-exchangeable fractions of these materials are USGS42(Tibetan hair)δ(2)H(VSMOW-SLAP) = -78.5 ± 2.3‰ (n = 62) and δ(18)O(VSMOW-SLAP) = +8.56 ± 0.10‰ (n = 18) USGS42(Indian hair)δ(2)H(VSMOW-SLAP) = -50.3 ± 2.8‰ (n = 64) and δ(18)O(VSMOW-SLAP) = +14.11 ± 0.10‰ (n = 18). Using recommended analytical protocols presented herein for δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) measurements, the least squares fit regression of 11 human hair reference materials is δ(2)H(VSMOW-SLAP) = 6.085δ(2)O(VSMOW-SLAP) - 136.0‰ with an R-square value of 0.95. The δ(2)H difference between the calibrated results of human hair in this investigation and a commonly accepted human-hair relationship is a remarkable 34‰. It is critical that readers pay attention to the δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) of isotopic reference materials in publications, and they need to adjust the δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) measurement results of human hair in previous publications, as needed, to ensure all results on are on the same scales.

European Proficiency testing of national reference laboratories for the confirmation of sulfonamide residues in muscle and milk.

PubMed

Juhel-Gaugain, Murielle; Fourmond, Marie-Pierre; Delepine, Bernard; Laurentie, Michel; Brigitte, Roudaut; Sanders, Pascal

2005-03-01

Two interlaboratory studies were organized in 2002-2003 in order to check the proficiency of laboratories in confirming the presence of sulfonamide residues in muscle and milk. These studies involved 25 EU National Reference Laboratories (NRLs) from 21 different European Countries in charge of statutory monitoring of antimicrobial residues in food of animal origin at a national level. The study was conducted according to international and national guidelines by the Community Reference Laboratory (CRL) in charge of antimicrobial substances. Four different test matrices of sheep muscle and four different test matrices of bovine milk containing different sulfonamide substances were prepared and sent to the participants. Each participant was asked to use his own routine confirmatory method and to analyse each sample in triplicate within a period of about six weeks during which the stability of the materials was checked by the organizer. The sulfonamide content of each material was determined by calculating the robust means of all the results and the deviation of the results from the assigned values was assessed by calculating Z-scores. Overall, results were satisfactory, particularly considering that it was the first proficiency test dealing with sulfonamides organised by the Community Reference Laboratory.

Establishment of hepatitis A vaccine (inactivated, non-adsorbed) BRP batches 2 and 3.

PubMed

Morgeaux, S; Manniam, I; Variot, P; Buchheit, K H; Daas, A; Wierer, M; Costanzo, A

2015-01-01

The current hepatitis A vaccine (HAV), inactivated, non-adsorbed, European Pharmacopoeia (Ph. Eur.) Biological Reference Preparation (BRP) is used for the in vitro potency assay of HAV as prescribed by the Ph. Eur. general chapter 2.7.14 Assay of hepatitis A vaccine. This reference preparation was calibrated in 2008 through an international collaborative study and was assigned a potency of 12 IU/mL. During use of this BRP it appeared to be inapplicable in certain cases due to a low nominal antigen content. Consequently, the European Directorate for the Quality of Medicines and HealthCare (EDQM) established replacement batches for this BRP, calibrated against the 1(st) WHO International Standard (IS) for HAV (inactivated), using the standard in vitro ELISA (enzyme-linked immunosorbent assay) method validated previously. The results of the study showed that the candidate BRPs were suitable for the intended purpose, and following completion of the study, they were adopted in November 2014 by the Ph. Eur. Commission as HAV (inactivated, non-adsorbed) BRP batches 2 and 3, with an assigned potency of 1350 IU/mL, for in vitro antigen content determination by ELISA. As the amount of material in each vial largely exceeds the amount required for the performance of a single assay, the BRPs are to be aliquoted by users as single-use aliquots and refrozen below -50 °C prior to their use as reference preparations.

Comprehensive inter-laboratory calibration of reference materials for δ18O versus VSMOW using various on-line high-temperature conversion techniques

USGS Publications Warehouse

Brand, Willi A.; Coplen, Tyler B.; Aerts-Bijma, Anita T.; Bohlke, John Karl; Gehre, Matthias; Geilmann, Heike; Groning, Manfred; Jansen, Henk G.; Meijer, Harro A. J.; Mroczkowski, Stanley J.; Qi, Haiping; Soergel, Karin; Stuart-Williams, Hilary; Weise, Stephan M.; Werner, Roland A.

2009-01-01

Internationally distributed organic and inorganic oxygen isotopic reference materials have been calibrated by six laboratories carrying out more than 5300 measurements using a variety of high-temperature conversion techniques (HTC) in an evaluation sponsored by the International Union of Pure and Applied Chemistry (IUPAC). To aid in the calibration of these reference materials, which span more than 125‰, an artificially enriched reference water (δ18O of +78.91‰) and two barium sulfates (one depleted and one enriched in 18O) were prepared and calibrated relative to VSMOW2 and SLAP reference waters. These materials were used to calibrate the other isotopic reference materials in this study, which yielded:Reference materialδ18O and estimated combined uncertainty IAEA-602 benzoic acid+71.28 ± 0.36‰USGS35 sodium nitrate+56.81 ± 0.31‰IAEA-NO-3 potassium nitrate+25.32 ± 0.29‰IAEA-601 benzoic acid+23.14 ± 0.19‰IAEA-SO-5 barium sulfate+12.13 ± 0.33‰NBS 127 barium sulfate+8.59 ± 0.26‰VSMOW2 water0‰IAEA-600 caffeine−3.48 ± 0.53‰IAEA-SO-6 barium sulfate−11.35 ± 0.31‰USGS34 potassium nitrate−27.78 ± 0.37‰SLAP water−55.5‰The seemingly large estimated combined uncertainties arise from differences in instrumentation and methodology and difficulty in accounting for all measurement bias. They are composed of the 3-fold standard errors directly calculated from the measurements and provision for systematic errors discussed in this paper. A primary conclusion of this study is that nitrate samples analyzed for δ18O should be analyzed with internationally distributed isotopic nitrates, and likewise for sulfates and organics. Authors reporting relative differences of oxygen-isotope ratios (δ18O) of nitrates, sulfates, or organic material should explicitly state in their reports the δ18O values of two or more internationally distributed nitrates (USGS34, IAEA-NO-3, and USGS35), sulfates (IAEA-SO-5, IAEA-SO-6, and NBS 127), or organic material (IAEA-601 benzoic acid, IAEA-602 benzoic acid, and IAEA-600 caffeine), as appropriate to the material being analyzed, had these reference materials been analyzed with unknowns. This procedure ensures that readers will be able to normalize the δ18O values at a later time should it become necessary.The high-temperature reduction technique for analyzing δ18O and δ2H is not as widely applicable as the well-established combustion technique for carbon and nitrogen stable isotope determination. To obtain the most reliable stable isotope data, materials should be treated in an identical fashion; within the same sequence of analyses, samples should be compared with working reference materials that are as similar in nature and in isotopic composition as feasible.

230Th-234U Model-Ages of Some Uranium Standard Reference Materials

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

Williams, R W; Gaffney, A M; Kristo, M J

The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the {sup 230}Th-{sup 234}U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumptionmore » of the initial {sup 230}Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U{sub 3}O{sub 8}) may be assumed with confidence. We present here {sup 230}Th-{sup 234}U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history.« less

Joint Test Report for Validation of Alternative Low-Emission Surface Preparation/Depainting Technologies for Structural Steel

NASA Technical Reports Server (NTRS)

Lewis, Pattie

2007-01-01

Headquarters National Aeronautics and Space Administration (NASA) chartered the NASA Acquisition Pollution Prevention (AP2) Office to coordinate agency activities affecting pollution prevention issues identified during system and component acquisition and sustainment processes. The primary objectives of the AP2 Office are to: (1) Reduce or eliminate the use of hazardous materials or hazardous processes at manufacturing, remanufacturing, and sustainment locations. (2) Avoid duplication of effort in actions required to reduce or eliminate hazardous materials through joint center cooperation and technology sharing. The objective of this project was to qualify candidate alternative Low-Emission Surface Preparation/Depainting Technologies for Structural Steel applications at NASA facilities. This project compares the surface preparation/depainting performance of the proposed alternatives to existing surface preparation/depainting systems or standards. This Joint Test Report (JTR) contains the results of testing as per the outlines of the Joint Test Protocol (JTP), Joint Test Protocol for Validation of Alternative Low-Emission Surface Preparation/Depainting Technologies for Structural Steel, and the Field Test Plan (FTP), Field Evaluations Test Plan for Validation of Alternative Low-Emission Surface Preparation/Depainting Technologies for Structural Steel, for critical requirements and tests necessary to qualify alternatives for coating removal systems. These tests were derived from engineering, performance, and operational impact (supportability) requirements defined by a consensus of government and industry participants. This JTR documents the results of the testing as well as any test modifications made during the execution of the project. This JTR is made available as a reference for future pollution prevention endeavors by other NASA Centers, the Department of Defense and commercial users to minimize duplication of effort. The current coating removal processes identified herein are for polyurethane, epoxy and other paint systems applied by conventional wet-spray processes. A table summarizes the target hazardous materials, processes and materials, applications, affected programs, and candidate substrates.

Applications of New Synthetic Uranium Reference Materials for Research in Geochemistry

NASA Astrophysics Data System (ADS)

Richter, Stephan; Alonso, Adolfo; Aregbe, Yetunde; Eykens, Roger; Jacobsson, Ulf; Kuehn, Heinz; Verbruggen, Andre; Weyer, Stefan

2010-05-01

For many applications in geochemistry research isotope ratio measurements play a significant role. In geochronology isotope abundances of uranium and its daughter products thorium and lead are being used to determine the age and history of various samples of geological interest. For measuring the isotopic compositions of these elements by mass spectrometry, suitable isotope reference materials are needed to validate measurement procedures and to calibrate multi-collector and ion counting detector systems. IRMM is a recognized provider for nuclear isotope reference materials to the nuclear industry and nuclear safeguards authorities, which are also being applied widely for geochemical applications. Firstly, the double spike IRMM-3636 with a 233U/236U ratio of 1:1 was prepared which allows internal mass fractionation correction for high precision 235U/238U ratio measurements. The 234U abundance of this double spike material is low enough to allow an accurate and precise correction of 234U/238U ratios, even for measurements of close to equilibrium uranium samples. The double spike IRMM-3636 is offered in 3 concentrations: 1mg/g, 0.1mg/g and 0.005mg/g. Secondly, the 236U single spike IRMM-3660 was prepared and is offered in 3 concentrations: 1mg/g, 0.1mg/g and 0.01mg/g. Thirdly, a "Quad"-isotope reference material, IRMM-3101, has been prepared which is characterized by 233U/235U/236U/238U=1/1/1/1. This material is useful for checking Faraday cup efficiencies and inter-calibration of MIC (multiple ion counting) detectors. The quad-IRM is offered in 3 concentrations: 1mg/g, 0.1mg/g and 0.01mg/g. As one example for the significant influence of synthetic reference materials for geochemical research, the IRMM-074 series of gravimetrically prepared uranium mixtures for linearity testing of secondary electron multipliers (SEMs) has been applied for the redetermination of the secular equilibrium 234U/238U value and the 234U half-life by Cheng et al (2009). Due to the use of IRMM-074, results with smaller uncertainties were obtained, which are shifted by about 0.04% compared to the commonly used values published earlier by Cheng et al. in 2000. This has a significant impact for U isotope measurements in geochemistry. As another example for a geochemical application, by using the new double spike IRMM-3636, the 235U/238U ratios for several commonly used natural U standard materials from NIST/NBL and IRMM, such as e.g. NBS960 (=NBL CRM-112a), NBS950a,b and IRMM-184, have been re-measured at IRMM and other laboratories with improved precision and accuracy. The (preliminary) new result of 137.839(24) for the 238U/235U ratio of NBL CRM-112a is deviating by -0.030% from the well-known and widely used old consensus value of 137.88. For this old consensus value no uncertainty has ever been assigned, but it is outside the uncertainty limits of the new measurement result. The new result is based on measurements made at several laboratories worldwide, such as University of Frankfurt (Germany), National Taiwan University, NERC (University of Nottingham, UK), UNM (University of Minnesota, US), Thermo Fisher Scientific, LLNL (Lawrence Livermore National Laboratory, US.DOE), SAL/IAEA and IRMM. The (preliminary) new result of 137.839(24) can therefore be proposed as a new consensus value for the 238U/235U ratio of NBL CRM-112a. In contrast to the older consensus value, this new result is traceable to the common SI system of units and has an uncertainty assigned to it. For the close to natural standard IRMM-184, the re-measured 238U/235U ratio of 137.683(23) agrees quite well with the certified value of 137.697(41), the calculated difference is only -0.010(35)% which is insignificant. As a conclusion, the IRMM-3636 Double Spike has been successfully applied for measurements of important uranium isotopic standards like NBL CRM-112a and IRMM-184, with improved uncertainties at the level of 0.016% and traceability to the SI system.

Comparative study between structural and electrical properties of geopolymers applied to a green concrete

NASA Astrophysics Data System (ADS)

Montaño, A. M.; González, C. P.; Pérez, J.; Royero, C.; Sandoval, D.; Gutiérrez, J.

2013-11-01

This work shows a comparative analysis of geopolymers obtained by alkaline activation of two aluminosilicates: bentonite and metakaolin. With the goal of to replace some cement percentage, both aluminosilicates were added in several proportions (10, 20 and 30%) to concrete mixes. Portland Type I cement was used to prepare the reference concrete (without geopolymer). X-ray diffraction of geopolymers allowed to find new crystallographic phases that was not present in precursor's minerals. To evaluate mechanical properties of concrete prepared with geopolymers, test tubes with 7, 14, 28 and 90 days as setting time were used. Chemical resistance and Electrical impedance of concrete mixes were also measured. Results shows that cementitious material obtained from metakaolin exhibit the best compressive strength. On the other hand, those materials derived from bentonite, have a high electrical resistance so that, they protected reinforced concrete better that Portland does.

Avirulent Bacillus anthracis Strain with Molecular Assay Targets as Surrogate for Irradiation-Inactivated Virulent Spores.

PubMed

Plaut, Roger D; Staab, Andrea B; Munson, Mark A; Gebhardt, Joan S; Klimko, Christopher P; Quirk, Avery V; Cote, Christopher K; Buhr, Tony L; Rossmaier, Rebecca D; Bernhards, Robert C; Love, Courtney E; Berk, Kimberly L; Abshire, Teresa G; Rozak, David A; Beck, Linda C; Stibitz, Scott; Goodwin, Bruce G; Smith, Michael A; Sozhamannan, Shanmuga

2018-04-01

The revelation in May 2015 of the shipment of γ irradiation-inactivated wild-type Bacillus anthracis spore preparations containing a small number of live spores raised concern about the safety and security of these materials. The finding also raised doubts about the validity of the protocols and procedures used to prepare them. Such inactivated reference materials were used as positive controls in assays to detect suspected B. anthracis in samples because live agent cannot be shipped for use in field settings, in improvement of currently deployed detection methods or development of new methods, or for quality assurance and training activities. Hence, risk-mitigated B. anthracis strains are needed to fulfill these requirements. We constructed a genetically inactivated or attenuated strain containing relevant molecular assay targets and tested to compare assay performance using this strain to the historical data obtained using irradiation-inactivated virulent spores.

Curating NASA's Past, Present, and Future Extraterrestrial Sample Collections

NASA Technical Reports Server (NTRS)

McCubbin, F. M.; Allton, J. H.; Evans, C. A.; Fries, M. D.; Nakamura-Messenger, K.; Righter, K.; Zeigler, R. A.; Zolensky, M.; Stansbery, E. K.

2016-01-01

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10E "Curation of Extraterrestrial Materials", JSC is charged with "...curation of all extra-terrestrial material under NASA control, including future NASA missions." The Directive goes on to define Curation as including "...documentation, preservation, preparation, and distribution of samples for research, education, and public outreach." Here we describe some of the past, present, and future activities of the NASA Curation Office.

The Structure and Mechanical Properties of High-Strength Bulk Ultrafine-Grained Cobalt Prepared Using High-Energy Ball Milling in Combination with Spark Plasma Sintering

PubMed Central

Marek, Ivo; Vojtěch, Dalibor; Michalcová, Alena; Kubatík, Tomáš František

2016-01-01

In this study, bulk ultrafine-grained and micro-crystalline cobalt was prepared using a combination of high-energy ball milling and subsequent spark plasma sintering. The average grain sizes of the ultrafine-grained and micro-crystalline materials were 200 nm and 1 μm, respectively. Mechanical properties such as the compressive yield strength, the ultimate compressive strength, the maximum compressive deformation and the Vickers hardness were studied and compared with those of a coarse-grained as-cast cobalt reference sample. The bulk ultrafine-grained sample showed an ultra-high compressive yield strength that was greater than 1 GPa, which is discussed with respect to the preparation technique and a structural investigation. PMID:28773514

Development of a standard reference material for Cr(vi) in contaminated soil

USGS Publications Warehouse

Nagourney, S.J.; Wilson, S.A.; Buckley, B.; Kingston, H.M.S.; Yang, S.-Y.; Long, S.E.

2008-01-01

Over the last several decades, considerable contamination by hexavalent chromium has resulted from the land disposal of Chromite Ore Processing Residue (COPR). COPR contains a number of hexavalent chromium-bearing compounds that were produced in high temperature industrial processes. Concern over the carcinogenic potential of this chromium species, and its environmental mobility, has resulted in efforts to remediate these waste sites. To provide support to analytical measurements of hexavalent chromium, a candidate National Institute of Standards and Technology (NIST) Standard Reference Material?? (SRM 2701), having a hexavalent chromium content of approximately 500 mg kg -1, has been developed using material collected from a waste site in Hudson County, New Jersey, USA. The collection, processing, preparation and preliminary physico-chemical characterization of the material are discussed. A two-phase multi-laboratory testing study was carried out to provide data on material homogeneity and to assess the stability of the material over the duration of the study. The study was designed to incorporate several United States Environmental Protection Agency (USEPA) determinative methods for hexavalent chromium, including Method 6800 which is based on speciated isotope dilution mass spectrometry (SIDMS), an approach which can account for chromium species inter-conversion during the extraction and measurement sequence. This journal is ?? The Royal Society of Chemistry 2008.

Troubleshooting, Section One, Boilers: Correcting Oil Temperature. Part 3, Air Pollution Training Institute Self-Instructional Course SI-466.

ERIC Educational Resources Information Center

Environmental Protection Agency, Research Triangle Park, NC. Air Pollution Training Inst.

This workbook is part three of a self-instructional course prepared for the United States Environmental Protection Agency. The student proceeds at his own pace and when questions are asked, after answering, he either turns to the next page to check his response or refers to the previously covered material. The purpose of this course is to prepare…

The Basics of Boiler Operation and Maintenance. Part 2, Air Pollution Training Institute Self-Instructional Course SI-466.

ERIC Educational Resources Information Center

Environmental Protection Agency, Research Triangle Park, NC. Air Pollution Training Inst.

This workbook is part two of a self-instructional course prepared for the United States Environmental Protection Agency. The student proceeds at his own pace and when questions are asked, after answering, he either turns to the next page to check his response or refers to the previously covered material. The purpose of this course is to prepare…

The Incinerator: Section One, Basic Parts and Fundamentals. Part 5, Air Pollution Training Institute Self-Instructional Course SI-466.

ERIC Educational Resources Information Center

Environmental Protection Agency, Research Triangle Park, NC. Air Pollution Training Inst.

This workbook is part five of a self-instructional course prepared for the United States Environmental Protection Agency. The student proceeds at his own pace and when questions are asked, after answering, he either turns to the next page to check his response or refers to the previously covered material. The purpose of this course is to prepare…

The Incinerator: Section Two, Maintenance and Trobuleshooting. Part 6, Air Pollution Training Institute Self-Instructional Course SI-466.

ERIC Educational Resources Information Center

Environmental Protection Agency, Research Triangle Park, NC. Air Pollution Training Inst.

This workbook is part six of a self-instructional course prepared for the United States Environmental Protection Agency. The student proceeds at his own pace and when questions are asked, after answering, he either turns to the next page to check his response or refers to the previously covered material. The purpose of this course is to prepare…

Certified reference materials for radionuclides in Bikini Atoll sediment (IAEA-410) and Pacific Ocean sediment (IAEA-412).

PubMed

Pham, M K; van Beek, P; Carvalho, F P; Chamizo, E; Degering, D; Engeler, C; Gascó, C; Gurriaran, R; Hanley, O; Harms, A V; Herrmann, J; Hult, M; Ikeuchi, Y; Ilchmann, C; Kanisch, G; Kis-Benedek, G; Kloster, M; Laubenstein, M; Llaurado, M; Mas, J L; Nakano, M; Nielsen, S P; Osvath, I; Povinec, P P; Rieth, U; Schikowski, J; Smedley, P A; Suplinska, M; Sýkora, I; Tarjan, S; Varga, B; Vasileva, E; Zalewska, T; Zhou, W

2016-03-01

The preparation and characterization of certified reference materials (CRMs) for radionuclide content in sediments collected offshore of Bikini Atoll (IAEA-410) and in the open northwest Pacific Ocean (IAEA-412) are described and the results of the certification process are presented. The certified radionuclides include: (40)K, (210)Pb ((210)Po), (226)Ra, (228)Ra, (228)Th, (232)Th, (234)U, (238)U, (239)Pu, (239+240)Pu and (241)Am for IAEA-410 and (40)K, (137)Cs, (210)Pb ((210)Po), (226)Ra, (228)Ra, (228)Th, (232)Th, (235)U, (238)U, (239)Pu, (240)Pu and (239+240)Pu for IAEA-412. The CRMs can be used for quality assurance and quality control purposes in the analysis of radionuclides in sediments, for development and validation of analytical methods and for staff training. Copyright © 2015 Elsevier Ltd. All rights reserved.

Breckinridge Project, initial effort. Report XI, Volume V. Critical review of the design basis. [Critical review

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

None

1982-01-01

Report XI, Technical Audit, is a compendium of research material used during the Initial Effort in making engineering comparisons and decisions. Volumes 4 and 5 of Report XI present those studies which provide a Critical Review of the Design Basis. The Critical Review Report, prepared by Intercontinental Econergy Associates, Inc., summarizes findings from an extensive review of the data base for the H-Coal process design. Volume 4 presents this review and assessment, and includes supporting material; specifically, Design Data Tabulation (Appendix A), Process Flow Sheets (Appendix B), and References (Appendix C). Volume 5 is a continuation of the references ofmore » Appendix C. Studies of a proprietary nature are noted and referenced, but are not included in these volumes. They are included in the Limited Access versions of these reports and may be reviewed by properly cleared personnel in the offices of Ashland Synthetic Fuels, Inc.« less

Evolution of activities in international biological standardization since the early days of the Health Organisation of the League of Nations.

PubMed

Sizaret, P

1988-01-01

The main activities in international biological standardization during the 18 years that followed the first international biological standardization meeting in London in 1921 were concerned with expressing the potencies of test preparations in comparison with reference materials. After the Second World War, however, it became clear that the testing of biological substances against international reference materials was only one among several measures for obtaining safe and potent products. The activities in international biological standardization were therefore widened so that, by the strict observance of specific manufacturing and control requirements, it was possible to gain further in safety and efficacy. At the end of 1987, 42 international requirements for biological substances were available and were being used as national requirements, sometimes after minor modification, by the majority of WHO's Member States. This is of utmost importance for the worldwide use of safe and potent biological products, including vaccines.

The uncertainty of reference standards--a guide to understanding factors impacting uncertainty, uncertainty calculations, and vendor certifications.

PubMed

Gates, Kevin; Chang, Ning; Dilek, Isil; Jian, Huahua; Pogue, Sherri; Sreenivasan, Uma

2009-10-01

Certified solution standards are widely used in forensic toxicological, clinical/diagnostic, and environmental testing. Typically, these standards are purchased as ampouled solutions with a certified concentration. Vendors present concentration and uncertainty differently on their Certificates of Analysis. Understanding the factors that impact uncertainty and which factors have been considered in the vendor's assignment of uncertainty are critical to understanding the accuracy of the standard and the impact on testing results. Understanding these variables is also important for laboratories seeking to comply with ISO/IEC 17025 requirements and for those preparing reference solutions from neat materials at the bench. The impact of uncertainty associated with the neat material purity (including residual water, residual solvent, and inorganic content), mass measurement (weighing techniques), and solvent addition (solution density) on the overall uncertainty of the certified concentration is described along with uncertainty calculations.

Leaching behaviour and mechanical properties of copper flotation waste in stabilized/solidified products.

PubMed

Mesci, Başak; Coruh, Semra; Ergun, Osman Nuri

2009-02-01

This research describes the investigation of a cement-based solidification/stabilization process for the safe disposal of copper flotation waste and the effect on cement properties of the addition of copper flotation waste (CW) and clinoptilolite (C). In addition to the reference mixture, 17 different mixtures were prepared using different proportions of CW and C. Physical properties such as setting time, specific surface area and compressive strength were determined and compared to a reference mixture and Turkish standards (TS). Different mixtures with the copper flotation waste portion ranging from 2.5 to 12.5% by weight of the mixture were tested for copper leachability. The results show that as cement replacement materials especially clinoptilolite had clear effects on the mechanical properties. Substitution of 5% copper flotation waste for Portland cement gave a similar strength performance to the reference mixture. Higher copper flotation waste addition such as 12.5% replacement yielded lower strength values. As a result, copper flotation waste and clinoptilolite can be used as cementitious materials, and copper flotation waste also can be safely stabilized/solidified in a cement-based solidification/stabilization system.

Development of a highly precise ID-ICP-SFMS method for analysis of low concentrations of lead in rice flour reference materials.

PubMed

Zhu, Yanbei; Inagaki, Kazumi; Yarita, Takashi; Chiba, Koichi

2008-07-01

Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g(-1) after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 +/- 0.8 ng g(-1) (mean +/- expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 +/- 3 ng g(-1) and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 +/- 0.24 ng g(-1) (n = 5), 1010 +/- 10 ng g(-1) (n = 5), and 1250 +/- 20 ng g(-1) (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 +/- 0.28 ng g(-1) (n = 10 bottles).

Absolute measurements and certified reference material for iron isotopes using multiple-collector inductively coupled mass spectrometry.

PubMed

Zhou, Tao; Zhao, Motian; Wang, Jun; Lu, Hai

2008-01-01

Two enriched isotopes, 99.94 at.% 56Fe and 99.90 at.% 54Fe, were blended under gravimetric control to prepare ten synthetic isotope samples whose 56Fe isotope abundances ranged from 95% to 20%. For multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) measurements typical polyatomic interferences were removed by using Ar and H2 as collision gas and operating the MC-ICP-MS system in soft mode. Thus high-precision measurements of the Fe isotope abundance ratios were accomplished. Based on the measurement of the synthetic isotope abundance ratios by MC-ICP-MS, the correction factor for mass discrimination was calculated and the results were in agreement with results from IRMM014. The precision of all ten correction factors was 0.044%, indicating a good linearity of the MC-ICP-MS method for different isotope abundance ratio values. An isotopic reference material was certified under the same conditions as the instrument was calibrated. The uncertainties of ten correction factors K were calculated and the final extended uncertainties of the isotopic certified Fe reference material were 5.8363(37) at.% 54Fe, 91.7621(51) at.% 56Fe, 2.1219(23) at.% 57Fe, and 0.2797(32) at.% 58Fe.

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

PubMed

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

2018-04-01

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

Targeted RNA-Sequencing with Competitive Multiplex-PCR Amplicon Libraries

PubMed Central

Blomquist, Thomas M.; Crawford, Erin L.; Lovett, Jennie L.; Yeo, Jiyoun; Stanoszek, Lauren M.; Levin, Albert; Li, Jia; Lu, Mei; Shi, Leming; Muldrew, Kenneth; Willey, James C.

2013-01-01

Whole transcriptome RNA-sequencing is a powerful tool, but is costly and yields complex data sets that limit its utility in molecular diagnostic testing. A targeted quantitative RNA-sequencing method that is reproducible and reduces the number of sequencing reads required to measure transcripts over the full range of expression would be better suited to diagnostic testing. Toward this goal, we developed a competitive multiplex PCR-based amplicon sequencing library preparation method that a) targets only the sequences of interest and b) controls for inter-target variation in PCR amplification during library preparation by measuring each transcript native template relative to a known number of synthetic competitive template internal standard copies. To determine the utility of this method, we intentionally selected PCR conditions that would cause transcript amplification products (amplicons) to converge toward equimolar concentrations (normalization) during library preparation. We then tested whether this approach would enable accurate and reproducible quantification of each transcript across multiple library preparations, and at the same time reduce (through normalization) total sequencing reads required for quantification of transcript targets across a large range of expression. We demonstrate excellent reproducibility (R2 = 0.997) with 97% accuracy to detect 2-fold change using External RNA Controls Consortium (ERCC) reference materials; high inter-day, inter-site and inter-library concordance (R2 = 0.97–0.99) using FDA Sequencing Quality Control (SEQC) reference materials; and cross-platform concordance with both TaqMan qPCR (R2 = 0.96) and whole transcriptome RNA-sequencing following “traditional” library preparation using Illumina NGS kits (R2 = 0.94). Using this method, sequencing reads required to accurately quantify more than 100 targeted transcripts expressed over a 107-fold range was reduced more than 10,000-fold, from 2.3×109 to 1.4×105 sequencing reads. These studies demonstrate that the competitive multiplex-PCR amplicon library preparation method presented here provides the quality control, reproducibility, and reduced sequencing reads necessary for development and implementation of targeted quantitative RNA-sequencing biomarkers in molecular diagnostic testing. PMID:24236095

Application of inductively coupled plasma sector field mass spectrometry for low-level environmental americium-241 analysis.

PubMed

Varga, Zsolt

2007-03-28

An improved and novel sample preparation method for (241)Am analysis by inductively coupled plasma sector field mass spectrometry has been developed. The procedure involves a selective CaF(2) pre-concentration followed by an extraction chromatographic separation using TRU resin. The achieved absolute detection limit of 0.86 fg (0.11 mBq) is comparable to that of alpha spectrometry (0.1 mBq) and suitable for low-level environmental measurements. Analysis of different kinds of environmental standard reference materials (IAEA-384--Fangataufa lagoon sediment, IAEA-385--Irish Sea sediment and IAEA-308--Mixed seaweed from the Mediterranean Sea) and alpha spectrometry were used to validate the procedure. The chemical recovery of sample preparation ranged between 72 and 94%. The results obtained are in good agreement with reference values and those measured by alpha spectrometry. The proposed method offers a rapid and less labor-intensive possibility for environmental (241)Am analysis than the conventionally applied radioanalytical techniques.

[Questionnaire studies on the vital situation and nutritional habits of students].

PubMed

Przybulewska, Krystyna; Janda, Katarzyna

2004-01-01

Results of questionnaire studies carried out in 2001/2002 among 230 students of University of Agriculture in Szczecin were presented. It served for assessing their material and living situation during studying at the University. Women and people originating from cities dominated in studied group of respondents. Probably, there is a decreasing tendency referring to attending the University by country people. Residence during studying depended on the year of education and origin of respondents. Last-year students and country people were more often placed in hostel. Material help in a form of social scholarship was more often assigned to country youth, and scientific grants were more frequently given to fifth-year students. No finance help of student's families made they undertook a part-time job that was made more often by final-year students. Significant differences referring to consumption customs often depended on sex. Students themselves most often prepared meals, including dinners. Only small per cent (12%) of students went to canteens, milk bars or other restaurants. Almost one-third of respondents fed irregularly. One-dish dinners consisting most often of purchased or earlier prepared semi-products dominated. Majority of students declared feeding meat, poultry, and sweets at least once a week, as well as fish--at least once a month. Every second person declared everyday consumption of fruit and vegetables, milk and its products as well as several cups of coffee daily; it referred more often to women. Most of respondents occasionally consumed sprinkle, low-alcoholic beverages and snacks in a form of chips and nuts, but they were more often men.

A proteomics performance standard to support measurement quality in proteomics.

PubMed

Beasley-Green, Ashley; Bunk, David; Rudnick, Paul; Kilpatrick, Lisa; Phinney, Karen

2012-04-01

The emergence of MS-based proteomic platforms as a prominent technology utilized in biochemical and biomedical research has increased the need for high-quality MS measurements. To address this need, National Institute of Standards and Technology (NIST) reference material (RM) 8323 yeast protein extract is introduced as a proteomics quality control material for benchmarking the preanalytical and analytical performance of proteomics-based experimental workflows. RM 8323 yeast protein extract is based upon the well-characterized eukaryote Saccharomyces cerevisiae and can be utilized in the design and optimization of proteomics-based methodologies from sample preparation to data analysis. To demonstrate its utility as a proteomics quality control material, we coupled LC-MS/MS measurements of RM 8323 with the NIST MS Quality Control (MSQC) performance metrics to quantitatively assess the LC-MS/MS instrumentation parameters that influence measurement accuracy, repeatability, and reproducibility. Due to the complexity of the yeast proteome, we also demonstrate how NIST RM 8323, along with the NIST MSQC performance metrics, can be used in the evaluation and optimization of proteomics-based sample preparation methods. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative Technique for Comparing Simulant Materials through Figures of Merit

NASA Technical Reports Server (NTRS)

Rickman, Doug; Hoelzer, Hans; Fourroux, Kathy; Owens, Charles; McLemore, Carole; Fikes, John

2007-01-01

The 1989 workshop report entitled Workshop on Production and Uses of Simulated Lunar Materials and the Lunar Regolith Simulant Materials: Recommendations for Standardization, Production, and Usage, NASA Technical Publication both identified and reinforced a need for a set of standards and requirements for the production and usage of the Lunar simulant materials. As NASA prepares to return to the Moon, and set out to Mars, a set of early requirements have been developed for simulant materials and the initial methods to produce and measure those simulants have been defined. Addressed in the requirements document are: 1) a method for evaluating the quality of any simulant of a regolith, 2) the minimum characteristics for simulants of Lunar regolith, and 3) a method to produce simulants needed for NASA's Exploration mission. As an extension of the requirements document a method to evaluate new and current simulants has been rigorously defined through the mathematics of Figures of Merit (FoM). Requirements and techniques have been developed that allow the simulant provider to compare their product to a standard reference material through Figures of Merit. Standard reference material may be physical material such as the Apollo core samples or material properties predicted for any landing site. The simulant provider is not restricted to providing a single "high fidelity" simulant, which may be costly to produce. The provider can now develop "lower fidelity" simulants for engineering applications such as drilling and mobility applications.

Synthetic isotope mixtures for the calibration of isotope amount ratio measurements of carbon

NASA Astrophysics Data System (ADS)

Russe, K.; Valkiers, S.; Taylor, P. D. P.

2004-07-01

Synthetic isotope mixtures for the calibration of carbon isotope amount ratio measurements have been prepared by mixing carbon tetrafluoride highly enriched in 13C with carbon tetrafluoride depleted in 13C. Mixing procedures based on volumetry and gravimetry are described. The mixtures served as primary measurement standards for the calibration of isotope amount ratio measurements of the Isotopic Reference Materials PEF1, NBS22 and USGS24. Thus SI-traceable measurements of absolute carbon isotope amount ratios have been performed for the first time without any hypothesis needed for a correction of oxygen isotope abundances, such as is the case for measurements on carbon dioxide. As a result, "absolute" carbon isotope amount ratios determined via carbon tetrafluoride have smaller uncertainties than those published for carbon dioxide. From the measurements of the Reference Materials concerned, the absolute carbon isotope amount ratio of Vienna Pee Dee Belemnite (VPDB)--the hypothetical material upon which the scale for relative carbon isotope ratio measurements is based--was calculated to be R13(VPDB) = (11 101 +/- 16) × 10-6.

Collaborative study for the establishment of the Ph. Eur. Hepatitis E virus RNA for NAT testing biological reference preparation batch 1.

PubMed

Baylis, S A; Terao, E; Blümel, J; Hanschmann, K-M O

2017-01-01

A new European Pharmacopoeia (Ph. Eur.) biological reference preparation (BRP) had to be established further to the decision to include nucleic acid testing (NAT) for the detection of hepatitis E virus (HEV) RNA in the monograph Human plasma (pooled and treated for virus inactivation) (1646). To this purpose, an international collaborative study was launched in the framework of the Biological Standardisation Programme (BSP) of the European Directorate for the Quality of Medicines & HealthCare (EDQM) and the Commission of the European Union (EU). The study was run in conjunction with the establishment of the 1 st World Health Organization (WHO) international reference panel (IRP) for hepatitis E virus RNA genotypes (8578/13). Twenty-three laboratories used in-house developed and commercially available assays to calibrate a lyophilised candidate BRP prepared from a HEV 3f strain positive human plasma against the 1 st WHO International Standard (IS) for HEV RNA (6329/10). Results from quantitative and qualitative assays were in good agreement and were combined to calculate an assigned potency. Real-time stability studies indicated that the candidate BRP is very stable at lower temperatures and is thus suitable for long-term use. Based on these results, in February 2016, the Ph. Eur. Commission adopted the candidate material as the hepatitis E virus RNA for NAT testing BRP batch 1, with an assigned unitage of 2.1 × 10 4 IU/vial (4.32 log 10 IU/vial).

Documentation of Concurrent programs.

DTIC Science & Technology

1983-07-01

preparing the documentation formats, and Tom McDonald for preparing the supplemental materials and statistical analyses. 16 [ 1 -16- I j REFERENCES I Boehm...IAWb CE:~ r SET _66 (0_W3. o 40 s.~ .MCSG o-Csr-~~ to4 "LQ4 SloeuS RGJEUT P-= I -~E , t.. AcO.4JLG m*CA TI_ G.rL:m!CDP lo. ’ VS -64’ 04 l OE3 (.tt qe tso...34*h (eeeeeotop to enter h, to IAmlOCSot land ,uoMXM to R&’T- kfC ’Cod At 1*1 ,lgo: 0) 4 O ~ en ttR .I SA’ tgOhegl that ’t to 40n. .hi &ren a ~ O toll s

Guidelines for Preparation of a Scientific Paper

PubMed Central

Kosiba, Margaret M.

1988-01-01

Even the experienced scientific writer may have difficulty transferring research results to clear, concise, publishable words. To assist the beginning scientific writer, guidelines are proposed that will provide direction for determining a topic, developing protocols, collecting data, using computers for analysis and word processing, incorporating copyediting notations, consulting scientific writing manuals, and developing sound writing habits. Guidelines for writing each section of a research paper are described to help the writer prepare the title page, introduction, materials and methods, results, and discussion sections of the paper, as well as the acknowledgments and references. Procedures for writing the first draft and subsequent revisions include a checklist of structural and stylistic problems and common errors in English usage. PMID:3339646

[Current situations and problem analysis of influencing factors of traditional Chinese medicine tablets on forming quality].

PubMed

Li, Yan-Nian; Wu, Zhen-Feng; Wan, Na; Li, Yuan-Hui; Li, Hui-Ting; Yang, Ming

2018-04-01

The compressibility of tablets is the essential operating unit during the preparation of traditional Chinese medicine tablets, as well as a complicated process. Therefore, it is of great significance to comprehensively study the influencing factors on the formation process. This paper aimed to review the evaluation methods for the tablet forming quality and highlight the effects of material powder properties, excipients and preparation technology on the quality of traditional Chinese medicine tablets on the basis of relevant literatures. Furthermore, the common problems in tablet forming process are also analyzed to provide useful references for the development of tablet forming quality of traditional Chinese medicines. Copyright© by the Chinese Pharmaceutical Association.

Patent Administration by Office Computer - A Case at Mazda Motor Corporation

NASA Astrophysics Data System (ADS)

Kimura, Ikuo; Nakamura, Shinji

The needs of patent administration have been diversified reflecting R&D activities under the severe competition of technical development, and business has been increased in quantity year after year as seen in patent application. Under these circumstances it is necessary to develop business mechanization which assists manual operation as much as possible to enforce the patent administration. Introducing office computer (CPU 512 KB, external memory 128 MB) for exclusive use in this purpose, Patent Department of Mazda Motor Corporation has been constructing database of patent administration centered around patent application by their own company, and utilizes it for automatic preparation of business forms, preparation of various statistical materials, and real-time reference to the application procedures.

Development and application of a general plasmid reference material for GMO screening.

PubMed

Wu, Yuhua; Li, Jun; Wang, Yulei; Li, Xiaofei; Li, Yunjing; Zhu, Li; Li, Jun; Wu, Gang

The use of analytical controls is essential when performing GMO detection through screening tests. Additionally, the presence of taxon-specific sequences is analyzed mostly for quality control during GMO detection. In this study, 11 commonly used genetic elements involving three promoters (P-35S, P-FMV35S and P-NOS), four marker genes (Bar, NPTII, HPT and Pmi), and four terminators (T-NOS, T-35S, T-g7 and T-e9), together with the reference gene fragments from six major crops of maize, soybean, rapeseed, rice, cotton and wheat, were co-integrated into the same single plasmid to construct a general reference plasmid pBI121-Screening. The suitability test of pBI121-Screening plasmid as reference material indicated that the non-target sequence on the pBI121-Screening plasmid did not affect the PCR amplification efficiencies of screening methods and taxon-specific methods. The sensitivity of screening and taxon-specific assays ranged from 5 to 10 copies of pBI121-Screening plasmid, meeting the sensitivity requirement of GMO detection. The construction of pBI121-Screening solves the lack of a general positive control for screening tests, thereby reducing the workload and cost of preparing a plurality of the positive control. Copyright © 2016 Elsevier B.V. All rights reserved.

Crystallization processes in pharmaceutical technology and drug delivery design

NASA Astrophysics Data System (ADS)

Shekunov, B. Yu; York, P.

2000-04-01

Crystallization is a major technological process for particle formation in pharmaceutical industry and, in addition, plays an important role in defining the stability and drug release properties of the final dosage forms. Industrial and regulatory aspects of crystallization are briefly reviewed with reference to solid-state properties of pharmaceuticals. Crystallization, incorporating wider definition to include precipitation and solid-state transitions, is considered in terms of preparation of materials for direct compression, formation of amorphous, solvated and polymorphic forms, chiral separation of drugs, production of materials for inhalation drug delivery and injections. Finally, recent developments in supercritical fluid particle technology is considered in relationship to the areas discussed.

Airborne instruments to measure atmospheric aerosol particles, clouds and radiation: A cook's tour of mature and emerging technology

NASA Astrophysics Data System (ADS)

Baumgardner, D.; Brenguier, J. L.; Bucholtz, A.; Coe, H.; DeMott, P.; Garrett, T. J.; Gayet, J. F.; Hermann, M.; Heymsfield, A.; Korolev, A.; Krämer, M.; Petzold, A.; Strapp, W.; Pilewskie, P.; Taylor, J.; Twohy, C.; Wendisch, M.; Bachalo, W.; Chuang, P.

2011-10-01

An overview is presented of airborne systems for in situ measurements of aerosol particles, clouds and radiation that are currently in use on research aircraft around the world. Description of the technology is at a level sufficient for introducing the basic principles of operation and an extensive list of references for further reading is given. A number of newer instruments that implement emerging technology are described and the review concludes with a description of some of the most important measurement challenges that remain. This overview is a synthesis of material from a reference book that is currently in preparation and that will be published in 2012 by Wiley.

Identification of TL-Om1, an Adult T-Cell Leukemia (ATL) Cell Line, as Reference Material for Quantitative PCR for Human T-Lymphotropic Virus 1

PubMed Central

Okuma, Kazu; Yamagishi, Makoto; Yamochi, Tadanori; Firouzi, Sanaz; Momose, Haruka; Mizukami, Takuo; Takizawa, Kazuya; Araki, Kumiko; Sugamura, Kazuo; Yamaguchi, Kazunari; Watanabe, Toshiki

2014-01-01

Quantitative PCR (qPCR) for human T-lymphotropic virus 1 (HTLV-1) is useful for measuring the amount of integrated HTLV-1 proviral DNA in peripheral blood mononuclear cells. Many laboratories in Japan have developed different HTLV-1 qPCR methods. However, when six independent laboratories analyzed the proviral load of the same samples, there was a 5-fold difference in their results. To standardize HTLV-1 qPCR, preparation of a well-defined reference material is needed. We analyzed the integrated HTLV-1 genome and the internal control (IC) genes of TL-Om1, a cell line derived from adult T-cell leukemia, to confirm its suitability as a reference material for HTLV-1 qPCR. Fluorescent in situ hybridization (FISH) showed that HTLV-1 provirus was monoclonally integrated in chromosome 1 at the site of 1p13 in the TL-Om1 genome. HTLV-1 proviral genome was not transferred from TL-Om1 to an uninfected T-cell line, suggesting that the HTLV-1 proviral copy number in TL-Om1 cells is stable. To determine the copy number of HTLV-1 provirus and IC genes in TL-Om1 cells, we used FISH, digital PCR, and qPCR. HTLV-1 copy numbers obtained by these three methods were similar, suggesting that their results were accurate. Also, the ratio of the copy number of HTLV-1 provirus to one of the IC genes, RNase P, was consistent for all three methods. These findings indicate that TL-Om1 cells are an appropriate reference material for HTLV-1 qPCR. PMID:25502533

The determination of water in crude oil and transformer oil reference materials.

PubMed

Margolis, Sam A; Hagwood, Charles

2003-05-01

The measurement of the amount of water in oils is of significant economic importance to the industrial community, particularly to the electric power and crude oil industries. The amount of water in transformer oils is critical to their normal function and the amount of water in crude oils affects the cost of the crude oil at the well head, the pipeline, and the refinery. Water in oil Certified Reference Materials (CRM) are essential for the accurate calibration of instruments that are used by these industries. Three NIST Standard Reference Materials (SRMs) have been prepared for this purpose. The water in these oils has been measured by both coulometric and volumetric Karl Fischer methods. The compounds (such as sulfur compounds) that interfere with the Karl Fischer reaction (interfering substances) and inflate the values for water by also reacting with iodine have been measured coulometrically. The measured water content of Reference Material (RM) 8506a Transformer Oil is 12.1+/-1.9 mg kg(-1) (plus an additional 6.2+/-0.9 mg kg(-1) of interfering substances). The measured water content of SRM 2722 Sweet Crude Oil, is 99+/-6 mg kg(-1) (plus an additional 5+/-2 mg kg(-1) of interfering substances). The measured water content of SRM 2721 Sour Crude Oil, is 134+/-18 mg kg(-1) plus an additional 807+/-43 mg kg(-1) of interfering substances. Interlaboratory studies conducted with these oil samples (using SRM 2890, water saturated 1-octanol, as a calibrant) are reported. Some of the possible sources of bias in these measurements were identified, These include: improperly calibrated instruments, inability to measure the calibrant accurately, Karl Fischer reagent selection, and volatilization of the interfering substances in SRM 2721.

Stable isotope analyses of oxygen (18O:17O:16O) and chlorine (37Cl:35Cl) in perchlorate: reference materials, calibrations, methods, and interferences

USGS Publications Warehouse

Böhlke, John Karl; Mroczkowski, Stanley J.; Sturchio, Neil C.; Heraty, Linnea J.; Richman, Kent W.; Sullivan, Donald B.; Griffith, Kris N.; Gu, Baohua; Hatzinger, Paul B.

2017-01-01

RationalePerchlorate (ClO4−) is a common trace constituent of water, soils, and plants; it has both natural and synthetic sources and is subject to biodegradation. The stable isotope ratios of Cl and O provide three independent quantities for ClO4− source attribution and natural attenuation studies: δ37Cl, δ18O, and δ17O (or Δ17O or 17Δ) values. Documented reference materials, calibration schemes, methods, and interferences will improve the reliability of such studies.MethodsThree large batches of KClO4 with contrasting isotopic compositions were synthesized and analyzed against VSMOW-SLAP, atmospheric O2, and international nitrate and chloride reference materials. Three analytical methods were tested for O isotopes: conversion of ClO4− to CO for continuous-flow IRMS (CO-CFIRMS), decomposition to O2 for dual-inlet IRMS (O2-DIIRMS), and decomposition to O2 with molecular-sieve trap (O2-DIIRMS+T). For Cl isotopes, KCl produced by thermal decomposition of KClO4 was reprecipitated as AgCl and converted into CH3Cl for DIIRMS.ResultsKClO4 isotopic reference materials (USGS37, USGS38, USGS39) represent a wide range of Cl and O isotopic compositions, including non-mass-dependent O isotopic variation. Isotopic fractionation and exchange can affect O isotope analyses of ClO4− depending on the decomposition method. Routine analyses can be adjusted for such effects by normalization, using reference materials prepared and analyzed as samples. Analytical errors caused by SO42−, NO3−, ReO42−, and C-bearing contaminants include isotope mixing and fractionation effects on CO and O2, plus direct interference from CO2 in the mass spectrometer. The results highlight the importance of effective purification of ClO4− from environmental samples.ConclusionsKClO4 reference materials are available for testing methods and calibrating isotopic data for ClO4− and other substances with widely varying Cl or O isotopic compositions. Current ClO4−extraction, purification, and analysis techniques provide relative isotope-ratio measurements with uncertainties much smaller than the range of values in environmental ClO4−, permitting isotopic evaluation of environmental ClO4− sources and natural attenuation.

IFCC primary reference procedures for the measurement of catalytic activity concentrations of enzymes at 37 °C. Part 9: reference procedure for the measurement of catalytic concentration of alkaline phosphatase International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) Scientific Division, Committee on Reference Systems of Enzymes (C-RSE) (1)).

PubMed

Schumann, Gerhard; Klauke, Rainer; Canalias, Francesca; Bossert-Reuther, Steffen; Franck, Paul F H; Gella, F-Javier; Jørgensen, Poul J; Kang, Dongchon; Lessinger, Jean-Marc; Panteghini, Mauro; Ceriotti, Ferruccio

2011-09-01

Abstract This paper is the ninth in a series dealing with reference procedures for the measurement of catalytic activity concentrations of enzymes at 37 °C and the certification of reference preparations. Other parts deal with: Part 1. The concept of reference procedures for the measurement of catalytic activity concentrations of enzymes; Part 2. Reference procedure for the measurement of catalytic concentration of creatine kinase; Part 3. Reference procedure for the measurement of catalytic concentration of lactate dehydrogenase; Part 4. Reference procedure for the measurement of catalytic concentration of alanine aminotransferase; Part 5. Reference procedure for the measurement of catalytic concentration of aspartate aminotransferase; Part 6. Reference procedure for the measurement of catalytic concentration of γ-glutamyltransferase; Part 7. Certification of four reference materials for the determination of enzymatic activity of γ-glutamyltransferase, lactate dehydrogenase, alanine aminotransferase and creatine kinase at 37 °C; Part 8. Reference procedure for the measurement of catalytic concentration of α-amylase. The procedure described here is derived from the previously described 30 °C IFCC reference method. Differences are tabulated and commented on in Appendix 1.

Highly Conducting Molecular Crystals.

NASA Astrophysics Data System (ADS)

Whitehead, Roger James

Available from UMI in association with The British Library. Requires signed TDF. As the result of a wide ranging effort towards the preparation of new electrically conducting molecular crystals, high quality samples were prepared of the organic radical-ion salt (TMTSF)_2SbCl _2F_4 {bis-tetramethyltetraselenafulvalene-dichlorotetrafluoroantimonate(V) }. A collaborative effort to investigate the electronic and structural properties of this material has yielded the necessary depth of information required to give a satisfactory understanding of its rather complicated behaviour. The combination of x-ray structural studies with d.c. transport, reflectance and magnetic measurements has served to underline the importance of crystalline perfection, electronic dimensionality and conduction electron correlation in determining the materials overall behaviour. This thesis describes the method of preparation and characterization of (TMTSF)_2SbCl _2F_4 and the experimental arrangements used to determine the temperature dependence of its ambient pressure electrical conductivity, thermopower and electron spin resonance spectra. The crystal structure and optical reflectance measurements at room temperature are also presented. The results into a study of the low temperature diffraction pattern are described along with the temperature dependence in the static magnetic susceptibility and in the conductivity behaviour under elevated hydrostatic pressures. These findings are rationalized by reference to other materials which show similar behaviour in their electronic and/or structural properties, and also to the various theoretical models currently enjoying favour.

Preparation of peanut butter suspension for determination of peanuts using enzyme-linked immunoassay kits.

PubMed

Trucksess, Mary W; Brewer, Vickery A; Williams, Kristina M; Westphal, Carmen D; Heeres, James T

2004-01-01

Peanuts are one of the 8 most common allergenic foods and a large proportion of peanut-allergic individuals have severe reactions, some to minimal exposure. Specific protein constituents in the peanuts are the cause of the allergic reactions in sensitized individuals who ingest the peanuts. To avoid accidental ingestion of peanut-contaminated food, methods of analysis for the determination of the allergenic proteins in foods are important tools. Such methods could help identify foods inadvertently contaminated with peanuts, thereby reducing the incidence of allergic reactions to peanuts. Commercial immunoassay kits are available but need study for method performance, which requires reference materials for within- and between-laboratory validations. In this study, National Institute of Standards and Technology Standard Reference Material 2387 peanut butter was used. A polytron homogenizer was used to prepare a homogenous aqueous Peanut Butter suspension for the evaluation of method performance of some commercially available immunoassay kits such as Veratox for Peanut Allergen Test (Neogen Corp.), Ridascreen Peanut (R-Biopharm GmbH), and Bio-Kit Peanut Protein Assay Kit (Tepnel). Each gram of the aqueous peanut butter suspension contained 20 mg carboxymethylcellulose sodium salt, 643 microg peanut, 0.5 mg thimerosal, and 2.5 mg bovine serum albumin. The suspension was homogenous, stable, reproducible, and applicable for adding to ice cream, cookies, breakfast cereals, and chocolate for recovery studies at spike levels ranging from 12 to 90 microg/g.

High accuracy Primary Reference gas Mixtures for high-impact greenhouse gases

NASA Astrophysics Data System (ADS)

Nieuwenkamp, Gerard; Zalewska, Ewelina; Pearce-Hill, Ruth; Brewer, Paul; Resner, Kate; Mace, Tatiana; Tarhan, Tanil; Zellweger, Christophe; Mohn, Joachim

2017-04-01

Climate change, due to increased man-made emissions of greenhouse gases, poses one of the greatest risks to society worldwide. High-impact greenhouse gases (CO2, CH4 and N2O) and indirect drivers for global warming (e.g. CO) are measured by the global monitoring stations for greenhouse gases, operated and organized by the World Meteorological Organization (WMO). Reference gases for the calibration of analyzers have to meet very challenging low level of measurement uncertainty to comply with the Data Quality Objectives (DQOs) set by the WMO. Within the framework of the European Metrology Research Programme (EMRP), a project to improve the metrology for high-impact greenhouse gases was granted (HIGHGAS, June 2014-May 2017). As a result of the HIGHGAS project, primary reference gas mixtures in cylinders for ambient levels of CO2, CH4, N2O and CO in air have been prepared with unprecedented low uncertainties, typically 3-10 times lower than usually previously achieved by the NMIs. To accomplish these low uncertainties in the reference standards, a number of preparation and analysis steps have been studied and improved. The purity analysis of the parent gases had to be performed with lower detection limits than previously achievable. E.g., to achieve an uncertainty of 2•10-9 mol/mol (absolute) on the amount fraction for N2O, the detection limit for the N2O analysis in the parent gases has to be in the sub nmol/mol domain. Results of an OPO-CRDS analyzer set-up in the 5µm wavelength domain, with a 200•10-12 mol/mol detection limit for N2O, will be presented. The adsorption effects of greenhouse gas components at cylinder surfaces are critical, and have been studied for different cylinder passivation techniques. Results of a two-year stability study will be presented. The fit-for-purpose of the reference materials was studied for possible variation on isotopic composition between the reference material and the sample. Measurement results for a suit of CO2 in air mixtures with varying δ13C values (from -5‰ to -40‰) analyzed with both cavity ringdown spectroscopy (CRDS) and isotope-ratio mass spectrometry (IRMS) will be presented. Round robins were organized to assess the agreement of the new reference gas mixtures developed by different project partners and to compare the new reference gases with the reference standards currently used by the atmospheric monitoring community (NOAA and AGAGE). These results will also be presented.

I PREPARE: development and clinical utility of an environmental exposure history mnemonic.

PubMed

Paranzino, Grace K; Butterfield, Patricia; Nastoff, Teresa; Ranger, Cherryll

2005-01-01

The I PREPARE environmental exposure history mnemonic is a quick reference tool created for primary care providers. Health care providers (N = 159) were asked to evaluate a prototype mnemonic, to suggest new health history questions, and to propose the deletion of less relevant questions. The goal of this evaluation was to create a practical and clinically relevant mnemonic, rather than to obtain quantitative estimates of validity. The final I PREPARE mnemonic cues the provider to "Investigate potential exposures;" ask questions related to "Present work," "Residence," "Environmental concerns," "Past work," and "Activities;" provide "Referrals and resources;" and "Educate" the patient by reviewing a checklist of strategies to prevent or minimize exposures. The sequence of I PREPARE makes intuitive sense by cueing the provider to ask specific questions and provide educational materials to the patient. National improvements in the quality of environmental exposure history data are predicated in part on the creation of simple and convenient tools for use in clinical practice.

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

NASA Astrophysics Data System (ADS)

Sydoff, Marie; Stenström, Kristina

2010-04-01

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

Photocatalyst of Perovskite CaTiO3 Nanopowder Synthesized from CaO derived from Snail Shell in Comparison with The Use of CaO and CaCO3

NASA Astrophysics Data System (ADS)

Fatimah, I.; Rahmadianti, Y.; Pudiasari, R. A.

2018-04-01

Calcium titanate belongs to the important group of compounds with a perovskite structure having high dielectric loss for various applications including photocatalysis mechanism. Refer to the principles of green chemistry, in this work preparation of CaTiO3 was conducted by using CaO derived from snail shell. Aim of this research are to study the physicochemical character of perovskite derived from snail shell and its comparison with CaO and CaCO3 as Ca sources. Material preparation was performed by solid reaction of Ca sources with TiO2 under comparison with CaO and CaCO3 precursors. Mixture of Ca sources with TiO2 in certain proportion were ground and calcined at the temperature of 200 °C for 2 hs. Materials were characterized by using X-ray diffractometer (XRD), Fourier Transform-Infra Red (FTIR) and the photocatalytic activity was tested by using methylene blue photooxidation. Perovskite synthesized using CaO derived from snail shell exhibits the similar XRD pattern with that were prepared by using CaO and CaCO3. From the photooxidation activity test, it is proven that CaTiO3 shows similar photocatalytic activity correspond to that were prepared by CaO and CaCO3. Utilazation of shell as agricultural waste of the synthesis of CaTiO3 perovskite is the novelty of this work. Furthermore, the study on material structure and photoactivity is the main focuses for the application in industry and environment.

Methods for the preparation of protein-oligonucleotide-lipid constructs.

PubMed

Takasaki, Jennifer; Raney, Sameersingh G; Chikh, Ghania; Sekirov, Laura; Brodsky, Irina; Tam, Ying; Ansell, Steven M

2006-01-01

A mixture of ionizable cationic lipids, steric barrier lipids, and colipids is used to encapsulate oligonucleotide DNA in lipidic particles called SALP. This material is under development as an adjuvant for vaccines. Previously we have shown that coupling the antigen directly to the surface of SALP can lead to enhanced immunological responses in vivo. Two different methods for preparing ovalbumin-SALP were assessed in this work. Originally the conjugates were prepared by treating SALP containing a maleimide-derivatized lipid with thiolated ovalbumin, a method we refer to as active coupling. This reaction was found to be difficult to control and generally resulted in low coupling efficiencies. The issues relating to this approach were characterized. We have recently developed alternative techniques based on first coupling ovalbumin to a micelle and then incubating the resultant product with SALP, methods we refer to as passive coupling. We have shown that this method allows accurate control of the levels of protein associated SALP and does not suffer from surface saturation effects seen with the active coupling method that places maximum limits on the amount of protein that can be coupled to the SALP surface. The products from the passive coupling protocol are shown to have activity comparable to those derived from the active coupling protocol in investigations of in vivo immune responses.

New NIST sediment SRM for inorganic analysis.

PubMed

Zeisler, Rolf

2004-03-01

NIST maintains a portfolio of more than 1300 standard reference materials (SRM), more than a third of these relating to measurements in the biological and environmental fields. As part of the continuous renewal and replacement efforts, a set of new marine sediments has been recently developed covering organic and inorganic determinations. This paper describes the steps taken in sample preparation, homogeneity assay, and analytical characterization and certification with specific emphasis on SRM 2702 inorganics in marine sediment. Neutron activation analysis showed the SRM to be highly homogeneous, opening the possibility for use with solid sampling techniques. The certificate provides certified mass fraction values for 25 elements, reference values for eight elements, and information values for 11 elements, covering most of the priority pollutants with small uncertainties of only several percent relative. The values were obtained by combining results from different laboratories and techniques using a Bayesian statistical model. An intercomparison carried out in field laboratories with the material before certification illustrates a high commutability of this SRM.

Novel approach in k0-NAA for highly concentrated REE Samples.

PubMed

Abdollahi Neisiani, M; Latifi, M; Chaouki, J; Chilian, C

2018-04-01

The present paper presents a new approach for k 0 -NAA for accurate quantification with short turnaround analysis times for rare earth elements (REEs) in high content mineral matrices. REE k 0 and Q 0 values, spectral interferences and nuclear interferences were experimentally evaluated and improved with Alfa Aesar Specpure Plasma Standard 1000mgkg -1 mono-rare earth solutions. The new iterative gamma-ray self-attenuation and neutron self-shielding methods were investigated with powder standards prepared from 100mg of 99.9% Alfa Aesar mono rare earth oxide diluted with silica oxide. The overall performance of the new k 0 -NAA method for REEs was validated using a certified reference material (CRM) from Canadian Certified Reference Materials Project (REE-2) with REE content ranging from 7.2mgkg -1 for Yb to 9610mgkg -1 for Ce. The REE concentration was determined with uncertainty below 7% (at 95% confidence level) and proved good consistency with the CRM certified concentrations. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of fat-soluble vitamins and carotenoids in standard reference material 3280 multivitamin/multielement tablets by liquid chromatography with absorbance detection.

PubMed

Thomas, Jeanice B; Sharpless, Katherine E; Yen, James H; Rimmer, Catherine A

2011-01-01

The concentrations of selected fat-soluble vitamins and carotenoids in Standard Reference Material (SRM) 3280 Multivitamin/Multielement Tablets have been determined by two independent LC methods, with measurements performed by the National Institute of Standards and Technology (NIST). This SRM has been prepared as part of a collaborative effort between NIST and the National Institutes of Health Office of Dietary Supplements. The SRM is also intended to support the Dietary Supplement Ingredient Database that is being established by the U.S. Department of Agriculture. The methods used at NIST to determine the concentration levels of vitamins A and E, and beta-carotene in the SRM used RPLC with absorbance detection. The relative precision of these methods ranged from 2 to 8% for the analytes measured. SRM 3280 is primarily intended for use in validating analytical methods for the determination of selected vitamins, carotenoids, and elements in multivitamin/multielement tablets and similar matrixes.

Preparation and characterization of "Libby Amphibole" toxicological testing material

USGS Publications Warehouse

Lowers, Heather; Wilson, Stephen A.; Hoefen, Todd M.; Benzel, William M.; Meeker, Gregory P.

2012-01-01

The U.S. Environmental Protection Agency (USEPA) began work in Libby, Mont. in 1999 when an Emergency Response Team was sent to investigate local concern and media reports regarding asbestos-contaminated vermiculite. Since that time, the site has been granted Superfund status and site remediation to a safe level of asbestos has been ongoing. The amphibole asbestos from the Vermiculite Mountain vermiculite deposit near Libby, Mont. (Libby amphibole) is unusual in the sense that it is currently not classified as one of the regulated six asbestos minerals—chrysotile (a serpentine mineral) and the amphibole minerals amosite (asbestiform cummingtonite-grunerite), crocidolite (asbestiform riebeckite), asbestiform anthophyllite, asbestiform tremolite, and asbestiform actinolite. The amphiboles from the Vermiculite Mountain vermiculite deposit, primarily winchite and richterite, are related to tremolite and in the past have been referred to as sodium-rich tremolite or soda tremolite (Larsen, 1942; Boettcher, 1966; Wylie and Verkouteren, 2000; Gunter and others, 2003; Meeker and others, 2003). The public health issues in Libby, Mont. have brought to light many of the inconsistencies in the literature regarding fiber characteristics, nomenclature, and toxicology. To better understand the toxicological characteristics of the Libby amphibole, investigators require a sufficient quantity of material representing the range of fibrous amphiboles present in the vicinity of Vermiculite Mountain to use in toxicology studies. The material collected in 2000 (Meeker and others, 2003) has been exhausted and a second collection and preparation effort, funded by the USEPA, was conducted in 2007. Both the 2000 (LA2000) and 2007 (LA2007) materials were generated to support research needs identified by the USEPA and the National Toxicology Program, and new in-vivo and in-vitro toxicology studies are underway. This Open-File Report describes the process of preparation and summarizes the chemistry and mineralogy of the LA2007 toxicological testing material.

Development of the Quality Assurance/Quality Control Procedures for a Neutron Interrogation System

NASA Astrophysics Data System (ADS)

Obhođaš, Jasmina; Sudac, Davorin; Valković, Vladivoj

2016-06-01

In order to perform Quality Assurance/Quality Control (QA/QC) procedures for a system dedicated to the neutron interrogation of objects for the presence of threat materials one needs to perform measurements of reference materials (RM) i.e. simulants having the same (or similar) atomic ratios as real materials. It is well known that explosives, drugs, and various other benign materials, contain chemical elements such as hydrogen, oxygen, carbon and nitrogen in distinctly different quantities. For example, a high carbon-to-oxygen ratio (C/O) is characteristic of drugs. Explosives can be differentiated by measurement of both (C/O) and nitrogen-to-oxygen (N/O) ratios. The C/N ratio of the chemical warfare agents, coupled with the measurement of elements such as fluorine and phosphorus, clearly differentiate them from the conventional explosives. Here we present the RM preparation, calibration procedure and correlations attained between theoretical values and experimentally obtained results in laboratory conditions for C/O and N/C ratios of prepared hexogen (RDX), TNT, DLM2, TATP, cocaine, heroin, yperite, tetranitromethane, peroxide methylethylketone, nitromethane and ethyleneglycol dinitrate simulants. We have shown that analyses of the gamma ray spectra by using simple unfolding model developed for this purpose gave a nice agreement with the chemical formula of created simulants, thus the calibration quality was successfully tested.

Laser-induced breakdown spectroscopy (LIBS) technique for the determination of the chemical composition of complex inorganic materials

NASA Astrophysics Data System (ADS)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Kozioł, Paweł E.; Stepak, Bogusz; Abramski, Krzysztof M.

2014-08-01

Laser-induced breakdown spectroscopy (LIBS) is a fast, fully optical method, that needs little or no sample preparation. In this technique qualitative and quantitative analysis is based on comparison. The determination of composition is generally based on the construction of a calibration curve namely the LIBS signal versus the concentration of the analyte. Typically, to calibrate the system, certified reference materials with known elemental composition are used. Nevertheless, such samples due to differences in the overall composition with respect to the used complex inorganic materials can influence significantly on the accuracy. There are also some intermediate factors which can cause imprecision in measurements, such as optical absorption, surface structure, thermal conductivity etc. This paper presents the calibration procedure performed with especially prepared pellets from the tested materials, which composition was previously defined. We also proposed methods of post-processing which allowed for mitigation of the matrix effects and for a reliable and accurate analysis. This technique was implemented for determination of trace elements in industrial copper concentrates standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for contents of three elements, that is silver, cobalt and vanadium. It has been shown that the described technique can be used to qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates.

Synthetic Strategies in the Preparation of Polymer/Inorganic Hybrid Nanoparticles

PubMed Central

Hood, Matthew A.; Mari, Margherita; Muñoz-Espí, Rafael

2014-01-01

This article reviews the recent advances and challenges in the preparation of polymer/inorganic hybrid nanoparticles. We mainly focus on synthetic strategies, basing our classification on whether the inorganic and the polymer components have been formed in situ or ex situ, of the hybrid material. Accordingly, four types of strategies are identified and described, referring to recent examples: (i) ex situ formation of the components and subsequent attachment or integration, either by covalent or noncovalent bonding; (ii) in situ polymerization in the presence of ex situ formed inorganic nanoparticles; (iii) in situ precipitation of the inorganic components on or in polymer structures; and (iv) strategies in which both polymer and inorganic component are simultaneously formed in situ. PMID:28788665

UO 2 Particle Standards: Synthesis, Purification & Planchet Preparation

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

Barrett, Christopher A.; Anheier, Norman C.

2016-03-31

The IAEA has previously indicated its desire for reliable provision of suitable reference materials in support of environmental sample analysis and sustained advancement at the Department of Safeguards, as laid out in the Long Term R&D plan (LTRD 10.1 & 10.2). In a recent meeting between NPAC, the IAEA and PNNL, this pressing need was directly outlined by the IAEA as having two main objectives. The first pertains to current operations, such as instrument calibrations and evaluation of bias across the Network of Analytical Laboratories and requires particles on the order of 300-500 nm in diameter. The second need formore » particle reference material would directly support the IAEA’s ongoing R&D efforts and calls for smaller particles ranging from 50 -100 nm in size. As such, the IAEA has expressed a great deal of interest in the newly established synthesis capabilities at PNNL, initially cultivated through a PNNL LDRD project to address the particle-standards shortcomings for uranium oxide material. The joint meeting concluded with a request by the IAEA for 1-2 planchet samples containing PNNL’s UO 2 particulate material, to be delivered in the near-term. This report outlines the steps taken to meet that request and includes some basic characteristics of the samples sent to the IAEA.« less

Preparation and characterization of graphene/turbostratic carbon derived from chitosan film for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Hanappi, M. F. Y. M.; Deraman, M.; Suleman, M.; Othman, M. A. R.; Basri, N. H.; Nor, N. S. M.; Hamdan, E.; Sazali, N. E. S.; Tajuddin, N. S. M.

2018-04-01

Electrochemical capacitors or supercapacitors are the potential energy storage devices which are known for having higher specific capacitance and specific energy than electrolytic capacitors. Electric double-layer capacitors (EDLCs) also referred as ultracapacitors is a class of supercapacitors that employ different forms of carbon like activated carbon, CNT, graphene etc., as electrodes. The performance of the supercapacitors is determined by its components namely electrolyte, electrode, etc. Carbon electrodes with high surface area and desired pore size distribution are always preferred and which can be tailored by varying the precursor and method of preparation. In recent years, owing to their low cost, ease of synthesis, high stability and conductivity, the activated carbons derived from biomass precursors have been investigated as potential electrode material for the EDLCs. In this report, we present the preparation and characterization of graphene/turbostratic carbon monolith (CM) electrodes from the carbon grains (CGs) obtained by carbonization (under the flow of nitrogen, N2 gas and over a temperature range from 600 °C to 1000 °C) of biomass precursor chitosan film. The procedure to prepare the chitosan film is described elsewhere. The carbon grains are characterized using Raman spectroscopy (RS) and X-ray diffraction (XRD). We expect that the CGs would have the similar characteristics as graphene and would be a potential electrode material for EDLCs application.

Bismuth silicate glass containing heavy metal oxide as a promising radiation shielding material

NASA Astrophysics Data System (ADS)

Elalaily, Nagia A.; Abou-Hussien, Eman M.; Saad, Ebtisam A.

2016-12-01

Optical and FTIR spectroscopic measurements and electron paramagnetic resonance (EPR) properties have been utilized to investigate and characterize the given compositions of binary bismuth silicate glasses. In this work, it is aimed to study the possibility of using the prepared bismuth silicate glasses as a good shielding material for γ-rays in which adding bismuth oxide to silicate glasses causes distinguish increase in its density by an order of magnitude ranging from one to two more than mono divalent oxides. The good thermal stability and high density of the bismuth-based silicate glass encourage many studies to be undertaken to understand its radiation shielding efficiency. For this purpose a glass containing 20% bismuth oxide and 80% SiO2 was prepared using the melting-annealing technique. In addition the effects of adding some alkali heavy metal oxides to this glass, such as PbO, BaO or SrO, were also studied. EPR measurements show that the prepared glasses have good stability when exposed to γ-irradiation. The changes in the FTIR spectra due to the presence of metal oxides were referred to the different housing positions and physical properties of the respective divalent Sr2+, Ba2+ and Pb2+ ions. Calculations of optical band gap energies were presented for some selected glasses from the UV data to support the probability of using these glasses as a gamma radiation shielding material. The results showed stability of both optical and magnetic spectra of the studied glasses toward gamma irradiation, which validates their irradiation shielding behavior and suitability as the radiation shielding candidate materials.

Microwave-assisted extraction and quantitative LC/ID-MS measurement of total choline and free carnitine in food standard reference materials.

PubMed

Phillips, Melissa M; Sander, Lane C

2012-01-01

The Stakeholder Panel on Infant Formula and Adult Nutritionals of AOAC INTERNATIONAL has declared both choline and carnitine to be priority nutrients in infant formulas, and ongoing efforts exist to develop or improve Official Methods of Analysis for these nutrients. As a result, matrix-based certified reference materials are needed with assigned values for these compounds. In this work, traditional acid and enzymatic hydrolysis procedures were compared to microwave-assisted acid hydrolysis, and conditions optimized to provide complete sample hydrolysis and recovery of total choline from four food standard reference materials (SRMs): whole milk powder, whole egg powder, infant formula, and soy flour. The extracts were analyzed using LC on a mixed-mode column (simultaneous RP and ion exchange) with isotope dilution-MS detection to achieve simultaneous quantification of total choline and free carnitine. Total choline has been determined in these four food matrixes with excellent precision (0.65 to 2.60%) and accuracy, as confirmed by use of SRM 1849 Infant/Adult Nutritional Formula as a control material. Free carnitine has been determined in two of these food matrixes with excellent precision (0.69 to 2.19%) and accuracy, as confirmed by use of SRM 1849 Infant/Adult Nutritional Formula as a control material. Limitations in simultaneous determination of total choline and free carnitine resulted from extreme differences in concentration of the two components in egg powder and soy flour (at least three orders of magnitude). Samples required dilution to prevent poor LC peak shape, which caused decreased precision in the determination of low concentrations of free carnitine. Despite this limitation, the described method yields results comparable to current AOAC Official Method 999.14 Choline in Infant Formula, with a decrease of more than 2 h in sample preparation time.

HPLC-APCI-MS analysis of triacylglycerols (TAGs) in historical pharmaceutical ointments from the eighteenth century.

PubMed

Saliu, Francesco; Modugno, Francesca; Orlandi, Marco; Colombini, Maria Perla

2011-10-01

The lipid fractions of residues from historical pharmaceutical ointments were analysed by reversed-phase liquid chromatography coupled with atmospheric pressure chemical ionization and mass spectrometer detection. The residues were contained in a series of historical apothecary jars, dating from the eighteenth century and conserved at the "Aboca Museum" in Sansepolcro (Arezzo, Italy) and at the pharmacy of the "Real Cartuja de Valldemossa" in Palma de Majorca (Spain). The analytical protocol was set up using a comparative study based on the evaluation of triacylglycerol (TAG) compositions in raw natural lipid materials and in laboratory-reproduced ointments. These ointments were prepared following pharmaceutical recipes reported in historical treatises and used as reference materials. The reference materials were also subjected to stress treatments in order to evaluate the modification occurring in the TAG profiles as an effect of ageing. TAGs were successfully detected in the reproduced formulations even in mixtures of up to ten ingredients and after harsh degradative treatments, and also in real historical samples. No particular interferences were detected from other non-lipid ingredients of the formulations. The TAG compositions detected in the historical ointments indicated a predominant use of olive oil and pig adipose material as lipid ingredients. The detection of a high level of tristearine and myristyl-palmitoyl-stearyl glycerol in two of the samples suggested the presence of a fatty material of a different origin (maybe a ruminant). On the basis of the positional isomer ratio, sn-PPO/sn-POP, it was possible to hypothesize an exclusive use of pig fat in one sample. We also evaluated the application of principal component analysis of TAG profiles as an approach for the multivariate statistical comparison of the reference and historical ointments.

Propulsion Test Handbook: MSFC and SSC. Draft 01

NASA Technical Reports Server (NTRS)

Hammond, John M.

2010-01-01

This Handbook was prepared to provide Propulsion Test Personnel a central source of fundamental reference material. The Testing Process, which is a three-part process of pre-test activities, testing, and post-test activities, involves a collaborative effort from the mechanical, electrical, safety, and environmental disciplines in the test environment. Pre-test activities, testing, and post-test activities processes will vary, per test requirements; however, the content of this Handbook should cover basic procedures and standards that are shared across Centers.

National Health Care: How Can the Federal Government Increase Access to Health Care to United States Citizens? National Debate Topic for High Schools, 1993-94. 103rd Congress, 1st Session/Senate Document 103-2.

ERIC Educational Resources Information Center

1993

In compliance with government regulations, this compilation of materials and bibliographic references has been prepared by the Library of Congress to assist debaters in researching the 1993-94 national debate topic for high schools which deals with access by all U.S. citizens to health care. The compilation which was assembled after a review of a…

Interfacial Layer Effects in Ba(1-x)Sr(x)TiO3 Thick Films Prepared by Plasma Spray

DTIC Science & Technology

2003-04-01

in Materials Development for Direct Write technologies, edited by D. B. Chrisey, D. R. Gamota, H . Helvajian , and D. P. Taylor, (Mater. Res. Soc. Proc...Direct Write technologies, edited by D. B. Chrisey, D. R. Gamota, H . Helvajian , and D. P. Taylor, (Mater. Res. Soc. Proc. 624, San Francisco, CA, 2000...Research Center at Northwestern University supported by the MRSEC program under a NSF grant (DMR-0076097). REFERENCES 1. K. H . Church, C. Fore, T. Feeley

Polymer Dispersed Liquid Crystal Displays

NASA Astrophysics Data System (ADS)

Doane, J. William

The following sections are included: * INTRODUCTION AND HISTORICAL DEVELOPMENT * PDLC MATERIALS PREPARATION * Polymerization induced phase separation (PIPS) * Thermally induced phase separation (TIPS) * Solvent induced phase separation (SIPS) * Encapsulation (NCAP) * RESPONSE VOLTAGE * Dielectric and resistive effects * Radial configuration * Bipolar configuration * Other director configurations * RESPONSE TIME * DISPLAY CONTRAST * Light scattering and index matching * Incorporation of dyes * Contrast measurements * PDLC DISPLAY DEVICES AND INNOVATIONS * Reflective direct view displays * Large-scale, flexible displays * Switchable windows * Projection displays * High definition spatial light modulator * Haze-free PDLC shutters: wide angle view displays * ENVIRONMENTAL STABILITY * ACKNOWLEDGEMENTS * REFERENCES

International comparison CCQM-K111.1—propane in nitrogen

NASA Astrophysics Data System (ADS)

van der Veen, Adriaan M. H.; Wouter van der Hout, J.; Ziel, Paul R.; Jozela, Mudalo; Tshilongo, James; Ntsasa, Napo G.; Botha, Angelique

2017-01-01

This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capability of preparing Primary Standard gas Mixtures (PSMs), performing the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this subsequent key comparison is classified as a track B key comparison, which means that the results of this key comparison can be used to underpin calibration and measurement capabilities for propane under the default scheme. The artefact was a binary mixture of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The result of the participating laboratory is consistent with the key comparison reference value within the respective expanded uncertainties and deviates less than 0.1 %. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Ordered patterns and structures via interfacial self-assembly: superlattices, honeycomb structures and coffee rings.

PubMed

Ma, Hongmin; Hao, Jingcheng

2011-11-01

Self-assembly is now being intensively studied in chemistry, physics, biology, and materials engineering and has become an important "bottom-up" approach to create intriguing structures for different applications. Self-assembly is not only a practical approach for creating a variety of nanostructures, but also shows great superiority in building hierarchical structures with orders on different length scales. The early work in self-assembly focused on molecular self-assembly in bulk solution, including the resultant dye aggregates, liposomes, vesicles, liquid crystals, gels and so on. Interfacial self-assembly has been a great concern over the last two decades, largely because of the unique and ingenious roles of this method for constructing materials at interfaces, such as self-assembled monolayers, Langmuir-Blodgett films, and capsules. Nanocrystal superlattices, honeycomb films and coffee rings are intriguing structural materials with more complex features and can be prepared by interfacial self-assembly on different length scales. In this critical review, we outline the recent development in the preparation and application of colloidal nanocrystal superlattices, honeycomb-patterned macroporous structures by the breath figure method, and coffee-ring-like patterns (247 references). This journal is © The Royal Society of Chemistry 2011

Sandwich-like C@SnO2/Sn/void@C hollow spheres as improved anode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Wang, Huijun; Jiang, Xinya; Chai, Yaqin; Yang, Xia; Yuan, Ruo

2018-03-01

As lithium ion batteries (LIBs) anode, SnO2 suffers fast capacity fading due to its large volume expansion during discharge/charge process. To overcome the problem, sandwich-like C@SnO2/Sn/void@C hollow spheres (referred as C@SnO2/Sn/void@C HSs) are prepared by in-situ polymerization and carbonization, using hollow SnO2 as self-template and dopamine as carbon source. The C@SnO2/Sn/void@C HSs possesses the merits of hollow and core/void/shell structure, so that they can accommodate the volume change under discharge/charge process, shorten the transmission distance of Li ions, own more contact area for the electrolyte. Thanks to these advantages, C@SnO2/Sn/void@C HSs display excellent electrochemical performance as anode materials for LIBs, which deliver a high capacity of 786.7 mAh g-1 at the current density of 0.5 A g-1 after 60 cycles. The simple synthesis method for C@SnO2/Sn/void@C HSs with special structure will provide a promising method for preparing other anode materials for LIBs.

Curating NASA's Future Extraterrestrial Sample Collections: How Do We Achieve Maximum Proficiency?

NASA Technical Reports Server (NTRS)

McCubbin, Francis; Evans, Cynthia; Zeigler, Ryan; Allton, Judith; Fries, Marc; Righter, Kevin; Zolensky, Michael

2016-01-01

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10E "Curation of Extraterrestrial Materials", JSC is charged with "The curation of all extraterrestrial material under NASA control, including future NASA missions." The Directive goes on to define Curation as including "... documentation, preservation, preparation, and distribution of samples for research, education, and public outreach." Here we describe some of the ongoing efforts to ensure that the future activities of the NASA Curation Office are working towards a state of maximum proficiency.

Non-invasive NMR stratigraphy of a multi-layered artefact: an ancient detached mural painting.

PubMed

Di Tullio, Valeria; Capitani, Donatella; Presciutti, Federica; Gentile, Gennaro; Brunetti, Brunetto Giovanni; Proietti, Noemi

2013-10-01

NMR stratigraphy was used to investigate in situ, non-destructively and non-invasively, the stratigraphy of hydrogen-rich layers of an ancient Nubian detached mural painting. Because of the detachment procedure, a complex multi-layered artefact was obtained, where, besides layers of the original mural painting, also the materials used during the procedure all became constitutive parts of the artefact. NMR measurements in situ enabled monitoring of the state of conservation of the artefact and planning of minimum representative sampling to validate results obtained in situ by solid-state NMR analysis of the samples. This analysis enabled chemical characterization of all organic materials. Use of reference compounds and prepared specimens assisted data interpretation.

Overview of experimental preparation for the ITER-Like Wall at JET

NASA Astrophysics Data System (ADS)

Jet Efda Contributors Brezinsek, S.; Fundamenski, W.; Eich, T.; Coad, J. P.; Giroud, C.; Huber, A.; Jachmich, S.; Joffrin, E.; Krieger, K.; McCormick, K.; Lehnen, M.; Loarer, T.; de La Luna, E.; Maddison, G.; Matthews, G. F.; Mertens, Ph.; Nunes, I.; Philipps, V.; Riccardo, V.; Rubel, M.; Stamp, M. F.; Tsalas, M.

2011-08-01

Experiments in JET with carbon-based plasma-facing components have been carried out in preparation of the ITER-Like Wall with beryllium main chamber and full tungsten divertor. The preparatory work was twofold: (i) development of techniques, which ensure safe operation with the new wall and (ii) provision of reference plasmas, which allow a comparison of operation with carbon and metallic wall. (i) Compatibility with the W divertor with respect to energy loads could be achieved in N2 seeded plasmas at high densities and low temperatures, finally approaching partial detachment, with only moderate confinement reduction of 10%. Strike-point sweeping increases the operational space further by re-distributing the load over several components. (ii) Be and C migration to the divertor has been documented with spectroscopy and QMBs under different plasma conditions providing a database which will allow a comparison of the material transport to remote areas with metallic walls. Fuel retention rates of 1.0-2.0 × 1021 D s-1 were obtained as references in accompanied gas balance studies.

Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

NASA Astrophysics Data System (ADS)

López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

2007-01-01

A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

21 CFR 660.25 - Potency tests without reference preparations.

Code of Federal Regulations, 2012 CFR

2012-04-01

... manufacturer's package insert using red blood cells showing heterozygous or diminished expression of the... SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.25 Potency tests without reference preparations. Products for which Reference Blood...

21 CFR 660.25 - Potency tests without reference preparations.

Code of Federal Regulations, 2010 CFR

2010-04-01

... manufacturer's package insert using red blood cells showing heterozygous or diminished expression of the... SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.25 Potency tests without reference preparations. Products for which Reference Blood...

21 CFR 660.25 - Potency tests without reference preparations.

Code of Federal Regulations, 2014 CFR

2014-04-01

... manufacturer's package insert using red blood cells showing heterozygous or diminished expression of the... SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.25 Potency tests without reference preparations. Products for which Reference Blood...

21 CFR 660.25 - Potency tests without reference preparations.

Code of Federal Regulations, 2011 CFR

2011-04-01

... manufacturer's package insert using red blood cells showing heterozygous or diminished expression of the... SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.25 Potency tests without reference preparations. Products for which Reference Blood...

21 CFR 660.25 - Potency tests without reference preparations.

Code of Federal Regulations, 2013 CFR

2013-04-01

... manufacturer's package insert using red blood cells showing heterozygous or diminished expression of the... SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.25 Potency tests without reference preparations. Products for which Reference Blood...

[Troubleshooting of bioinequivalence of compound valsartan tablets].

PubMed

Shao, Da; Zhang, Yi-Fan; Zhan, Yan; Chen, Xiao-Yan; Zhong, Da-Fang

2014-04-01

The study aims to evaluate the bioequivalence of valsartan hydrochlorothiazide tablets, and to investigate the potential cause of bioinequivalence. This was a single-center study with an open, randomized double-way crossover design. Test and reference preparations containing 160 mg of valsartan and 25 mg of hydrochlorothiazide were given to 36 healthy male volunteers. Plasma concentrations of valsartan and hydrochlorothiazide were determined simultaneously by LC-MS/MS. The pharmacokinetic parameters and relative bioavailability were calculated, while the bioequivalence between test and reference preparations were evaluated. The dissolution profiles of test and reference preparations in four different mediums were determined via dissolution test and HPLC. The similarity was investigated according to the similarity factors (f2). The F(o-t) and F(0-infinity) were (139.4 +/- 65.2)% and (137.5 +/- 61.2)% for valsartan of test preparations. It led to get the conclusion that test and reference preparations were not bioequivalent for valsartan. A significant difference was observed between test and reference tablets in the valsartan dissolution test of pH 1.2 hydrochloric acid solution. The key factor of the bioinequivalence might be that dissolution of valsartan in acid medium has marked difference between two preparations.

[Preparation of flavonoid reference standards from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry analysis].

PubMed

Guo, Henan; Yang, Xuedong; Liu, Jun; Zheng, Wenfeng

2012-07-01

Flavonoid reference standards were targeted-prepared from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry (HPLC-MS) analysis. With HPLC-MS analysis of Scutellariae Radix, 19 flavonoid components were identified by analyzing and comparing their retention times, ultraviolet spectra, and mass spectrometry data with literature. The separation and purification protocols of all targeted flavonoid reference standards were optimally designed according to the results of HPLC-MS analysis and related literature. The ethanol extract of Scutellariae Radix was suspended in water and extracted with petroleum ether, ethyl acetate, and n-butanol successively. The ethyl acetate extract and n-butanol extract were separately subjected to primary separation by low pressure reverse phase preparative chromatography. Then the fractions containing targeted compounds were further purified by low pressure reverse and normal phases preparative chromatography. Finally, baicalin and wogonoside reference standards were obtained from n-butanol extract; baicaelin, wogonin, and oroxylin A reference standards were obtained from ethyl acetate extract. The structures of the 5 reference standards were identified by mass spectrometry (MS) and 1H nuclear magnetic resonance (1H NMR) spectroscopy. The HPLC analytical results showed that the purities of the 5 reference standards were all above 98%. It is demonstrated that the rapid targeted-preparation method under the guidance of the HPLC-MS analysis is applicable for the isolation and preparation of chemical components in traditional Chinese medicines.

21 CFR 660.52 - Reference preparations.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 7 2010-04-01 2010-04-01 false Reference preparations. 660.52 Section 660.52 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Anti-Human Globulin § 660.52 Reference...

42 CFR 7.2 - Establishment of a user charge.

Code of Federal Regulations, 2010 CFR

2010-10-01

... DISTRIBUTION OF REFERENCE BIOLOGICAL STANDARDS AND BIOLOGICAL PREPARATIONS § 7.2 Establishment of a user charge... producing and distributing reference biological standards and biological preparations. ...

A novel sample preparation method using rapid nonheated saponification method for the determination of cholesterol in emulsified foods.

PubMed

Jeong, In-Seek; Kwak, Byung-Man; Ahn, Jang-Hyuk; Leem, Donggil; Yoon, Taehyung; Yoon, Changyong; Jeong, Jayoung; Park, Jung-Min; Kim, Jin-Man

2012-10-01

In this study, nonheated saponification was employed as a novel, rapid, and easy sample preparation method for the determination of cholesterol in emulsified foods. Cholesterol content was analyzed using gas chromatography with a flame ionization detector (GC-FID). The cholesterol extraction method was optimized for maximum recovery from baby food and infant formula. Under these conditions, the optimum extraction solvent was 10 mL ethyl ether per 1 to 2 g sample, and the saponification solution was 0.2 mL KOH in methanol. The cholesterol content in the products was determined to be within the certified range of certified reference materials (CRMs), NIST SRM 1544 and SRM 1849. The results of the recovery test performed using spiked materials were in the range of 98.24% to 99.45% with an relative standard devitation (RSD) between 0.83% and 1.61%. This method could be used to reduce sample pretreatment time and is expected to provide an accurate determination of cholesterol in emulsified food matrices such as infant formula and baby food. A novel, rapid, and easy sample preparation method using nonheated saponification was developed for cholesterol detection in emulsified foods. Recovery tests of CRMs were satisfactory, and the recoveries of spiked materials were accurate and precise. This method was effective and decreased the time required for analysis by 5-fold compared to the official method. © 2012 Institute of Food Technologists®

Impact of library preparation protocols and template quantity on the metagenomic reconstruction of a mock microbial community

DOE PAGES

Bowers, Robert M.; Clum, Alicia; Tice, Hope; ...

2015-10-24

Background: The rapid development of sequencing technologies has provided access to environments that were either once thought inhospitable to life altogether or that contain too few cells to be analyzed using genomics approaches. While 16S rRNA gene microbial community sequencing has revolutionized our understanding of community composi tion and diversity over time and space, it only provides a crude estimate of microbial functional and metabolic potential. Alternatively, shotgun metagenomics allows comprehensive sampling of all genetic material in an environment, without any underlying primer biases. Until recently, one of the major bottlenecks of shotgun metagenomics has been the requirement for largemore » initial DNA template quantities during library preparation. Results: Here, we investigate the effects of varying template concentrations across three low biomass library preparation protocols on their ability to accurately reconstruct a mock microbial community of known composition. We analyze the effects of input DNA quantity and library preparation method on library insert size, GC content, community composition, assembly quality and metagenomic binning. We found that library preparation method and the amount of starting material had significant impacts on the mock community metagenomes. In particular, GC content shifted towards more GC rich sequences at the lower input quantities regardless of library prep method, the number of low quality reads that could not be mapped to the reference genomes increased with decreasing input quantities, and the different library preparation methods had an impact on overall metagenomic community composition. Conclusions: This benchmark study provides recommendations for library creation of representative and minimally biased metagenome shotgun sequencing, enabling insights into functional attributes of low biomass ecosystem microbial communities.« less

Impact of library preparation protocols and template quantity on the metagenomic reconstruction of a mock microbial community

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

Bowers, Robert M.; Clum, Alicia; Tice, Hope

Background: The rapid development of sequencing technologies has provided access to environments that were either once thought inhospitable to life altogether or that contain too few cells to be analyzed using genomics approaches. While 16S rRNA gene microbial community sequencing has revolutionized our understanding of community composi tion and diversity over time and space, it only provides a crude estimate of microbial functional and metabolic potential. Alternatively, shotgun metagenomics allows comprehensive sampling of all genetic material in an environment, without any underlying primer biases. Until recently, one of the major bottlenecks of shotgun metagenomics has been the requirement for largemore » initial DNA template quantities during library preparation. Results: Here, we investigate the effects of varying template concentrations across three low biomass library preparation protocols on their ability to accurately reconstruct a mock microbial community of known composition. We analyze the effects of input DNA quantity and library preparation method on library insert size, GC content, community composition, assembly quality and metagenomic binning. We found that library preparation method and the amount of starting material had significant impacts on the mock community metagenomes. In particular, GC content shifted towards more GC rich sequences at the lower input quantities regardless of library prep method, the number of low quality reads that could not be mapped to the reference genomes increased with decreasing input quantities, and the different library preparation methods had an impact on overall metagenomic community composition. Conclusions: This benchmark study provides recommendations for library creation of representative and minimally biased metagenome shotgun sequencing, enabling insights into functional attributes of low biomass ecosystem microbial communities.« less

Modified Graphene as Electrocatalyst towards Oxygen Reduction Reaction for Fuel Cells

NASA Astrophysics Data System (ADS)

Qazzazie, D.; Beckert, M.; Mülhaupt, R.; Yurchenko, O.; Urban, G.

2014-11-01

This paper reports modified graphene-based materials as metal-free electrocatalysts for oxygen reduction reaction (ORR) with outstanding electrocatalytic activity in alkaline conditions. Nitrogen-doped graphene samples are synthesized by a novel procedure. The defect density in the structure of the prepared materials is investigated by Raman spectroscopy. Further structural characterization by X-ray photoelectron spectroscopy reveals the successful nitrogen doping of graphene. The electrochemical characterization of graphene and nitrogen-doped graphene in 0.1 M KOH solution demonstrates the material's electrocatalytic activity towards ORR. For graphene an onset potential of - 0.175 V vs. Ag/AgCl reference electrode is determined, while for nitrogen-doped graphene the determined onset potential is - 0.160 V. Thus, the electrocatalytic activity of nitrogen-doped graphene towards ORR is enhanced which can be ascribed to the effect of nitrogen doping.

21 CFR 660.22 - Potency requirements with reference preparations.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 7 2011-04-01 2010-04-01 true Potency requirements with reference preparations. 660.22 Section 660.22 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN.... Products for which reference Blood Grouping Reagents are available shall have a potency titer value at...

21 CFR 660.22 - Potency requirements with reference preparations.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 7 2010-04-01 2010-04-01 false Potency requirements with reference preparations. 660.22 Section 660.22 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN.... Products for which reference Blood Grouping Reagents are available shall have a potency titer value at...

Determination of total arsenic in fish by hydride-generation atomic absorption spectrometry: method validation, traceability and uncertainty evaluation

NASA Astrophysics Data System (ADS)

Nugraha, W. C.; Elishian, C.; Ketrin, R.

2017-03-01

Fish containing arsenic compound is one of the important indicators of arsenic contamination in water monitoring. The high level of arsenic in fish is due to absorption through food chain and accumulated in their habitat. Hydride generation (HG) coupled with atomic absorption spectrometric (AAS) detection is one of the most popular techniques employed for arsenic determination in a variety of matrices including fish. This study aimed to develop a method for the determination of total arsenic in fish by HG-AAS. The method for sample preparation from American of Analytical Chemistry (AOAC) Method 999.10-2005 was adopted for acid digestion using microwave digestion system and AOAC Method 986.15 - 2005 for dry ashing. The method was developed and validated using Certified Reference Material DORM 3 Fish Protein for trace metals for ensuring the accuracy and the traceability of the results. The sources of uncertainty of the method were also evaluated. By using the method, it was found that the total arsenic concentration in the fish was 45.6 ± 1.22 mg.Kg-1 with a coverage factor of equal to 2 at 95% of confidence level. Evaluation of uncertainty was highly influenced by the calibration curve. This result was also traceable to International Standard System through analysis of Certified Reference Material DORM 3 with 97.5% of recovery. In summary, it showed that method of preparation and HG-AAS technique for total arsenic determination in fish were valid and reliable.

Comparative analysis on reproducibility among 5 intraoral scanners: sectional analysis according to restoration type and preparation outline form

PubMed Central

2016-01-01

PURPOSE The trueness and precision of acquired images of intraoral digital scanners could be influenced by restoration type, preparation outline form, scanning technology and the application of power. The aim of this study is to perform the comparative evaluation of the 3-dimensional reproducibility of intraoral scanners (IOSs). MATERIALS AND METHODS The phantom containing five prepared teeth was scanned by the reference scanner (Dental Wings) and 5 test IOSs (E4D dentist, Fastscan, iTero, Trios and Zfx Intrascan). The acquired images of the scanner groups were compared with the image from the reference scanner (trueness) and within each scanner groups (precision). Statistical analysis was performed using independent two-samples t-test and analysis of variance (α=.05). RESULTS The average deviations of trueness and precision of Fastscan, iTero and Trios were significantly lower than the other scanners. According to the restoration type, significantly higher trueness was observed in crown and inlay than in bridge. However, no significant difference was observed among four sites of preparation outline form. If compared by the characteristics of IOS, high trueness was observed in the group adopting the active triangulation and using powder. However, there was no significant difference between the still image acquisition and video acquisition groups. CONCLUSION Except for two intraoral scanners, Fastscan, iTero and Trios displayed comparable levels of trueness and precision values in tested phantom model. Difference in trueness was observed depending on the restoration type, the preparation outline form and characteristics of IOS, which should be taken into consideration when the intraoral scanning data are utilized. PMID:27826385

IN VIVO STUDIES AND STABILITY STUDY OF CLADOPHORA GLOMERATA EXTRACT AS A COSMETIC ACTIVE INGREDIENT.

PubMed

Fabrowska, Joanna; Kapuscinska, Alicja; Leska, Boguslawa; Feliksik-Skrobich, Katarzyna; Nowak, Izabela

2017-03-01

Marine algae are widely used as cosmetics raw materials. Likewise, freshwater alga Cladophora glomerata may be a good source of fatty acids and others bioactive agents. The aims of this study was to find out if the addition of the extract from the freshwater C. glonerata affects the stability of prepared cosmetic emulsions and to investigate in vivo effects of the extract in cosmetic formulations on hydration and elasticity of human skin. Extract from the freshwater C. glonierata was obtained using supercritical fluid extraction (SFE). Two forms of O/W emulsions were prepared: placebo and emulsion containing 0.5% of Cladophora SFE extract. The stability of obtained emulsions was investigated by using Turbiscan Lab Expert. Emulsions were applied by .volunteers daily. Corneometer was used to evaluate skin hydration and cutometer to examine skin elasticity. Measurements were conducted at reference point (week 0) and after 1st, 2nd, 3rd and 4th week of application. The addition of Cladophora extract insignificantly affected stability of the emulsion. The extract from C. glomerata in the emulsion influenced the improvement of both skin hydration and its elasticity. Thus, freshwater C. glonierata extract prepared via SFE method may be considered as an effective cosmetic raw material used as a moisturizing and firming agent.

New tool for getting data on the field for paleoclimate and paleoceanography data based on isotope 13C and 18O measurements

NASA Astrophysics Data System (ADS)

Mandic, M.; Stöbener, N.; Smajgl, D.

2017-12-01

For many decades different instrumental methods involving generations of the isotope ratio mass spectrometers with different periphery units for sample preparation, have provided scientifically required high precision, and high throughput of samples for varies application - from geological and hydrological to food and forensic. With this work we introduce automated measurement of δ13C and δ18O from solid carbonate samples, DIC and δ18O of water. We have demonstrated usage of a Thermo Scientific™ Delta Ray™ IRIS with URI Connect on certified reference materials and confirmed the high achievable accuracy and a precision better then <0.1‰ for both δ13C and δ18O, in the laboratory or the field with same precision and throughput of samples. With equilibration method for determination of δ18O in water samples, which we present in this work, achieved repeatability and accuracy are 0.12‰ and 0.68‰ respectively, which fulfill requirements of regulatory methods. The preparation of the samples for carbonate and DIC analysis on the Delta Ray IRIS with URI Connect is similar to the previously mentioned Gas Bench II methods. Samples are put into vials and phosphoric acid is added. The resulting sample-acid chemical reaction releases CO2 gas, which is then introduced into the Delta Ray IRIS via the Variable Volume. Three international standards of carbonate materials (NBS-18, NBS-19 and IAEA-CO-1) were analyzed. NBS-18 and NBS-19 were used as standards for calibration, and IAEA-CO-1 was treated as unknown. For water sample analysis equilibration method with 1% of CO2 in dry air was used. Test measurements and conformation of precision and accuracy of method determination δ18O in water samples were done with three lab standards, namely ANST, OCEAN 2 and HBW. All laboratory standards were previously calibrated with international reference material VSMOW2 and SLAP2 to assure accuracy of the isotopic values. The Principle of Identical Treatment was applied in sample and standard preparation, in measurement procedure, as well as in the evaluation of the results.

Effect of Transitioning from Standard Reference Material 2806a to Standard Reference Material 2806b for Light Obscuration Particle Countering

DTIC Science & Technology

2016-04-01

Reference Material 2806b for Light Obscuration Particle Countering April 2016 UNCLASSIFIED UNCLASSIFIED Joel Schmitigal 27809 Standard Form 298 (Rev...Standard Reference Material 2806b for Light Obscuration Particle Countering 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6...Reference Material 2806a to Standard Reference Material 2806b for Light Obscuration Particle Countering Joel Schmitigal Force Projection

Bi-Component Nanostructured Arrays of Co Dots Embedded in Ni80Fe20 Antidot Matrix: Synthesis by Self-Assembling of Polystyrene Nanospheres and Magnetic Properties.

PubMed

Coïsson, Marco; Celegato, Federica; Barrera, Gabriele; Conta, Gianluca; Magni, Alessandro; Tiberto, Paola

2017-08-23

A bi-component nanostructured system composed by a Co dot array embedded in a Ni 80 Fe 20 antidot matrix has been prepared by means of the self-assembling polystyrene nanospheres lithography technique. Reference samples constituted by the sole Co dots or Ni 80 Fe 20 antidots have also been prepared, in order to compare their properties with those of the bi-component material. The coupling between the two ferromagnetic elements has been studied by means of magnetic and magneto-transport measurements. The Ni 80 Fe 20 matrix turned out to affect the vortex nucleation field of the Co dots, which in turn modifies the magneto-resistance behaviour of the system and its spinwave properties.

Fusion Bead Procedure for Nuclear Forensics Employing Synthetic Enstatite to Dissolve Uraniferous and Other Challenging Materials Prior to Laser Ablation Inductively Coupled Plasma Mass Spectrometry.

PubMed

Reading, David G; Croudace, Ian W; Warwick, Phillip E

2017-06-06

There is an increasing demand for rapid and effective analytical tools to support nuclear forensic investigations of seized or suspect materials. Some methods are simply adapted from other scientific disciplines and can effectively be used to rapidly prepare complex materials for subsequent analysis. A novel sample fusion method is developed, tested, and validated to produce homogeneous, flux-free glass beads of geochemical reference materials (GRMs), uranium ores, and uranium ore concentrates (UOC) prior to the analysis of 14 rare earth elements (REE) via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The novelty of the procedure is the production of glass beads using 9 parts high purity synthetic enstatite (MgSiO 3 ) as the glass former with 1 part of sample (sample mass ∼1.5 mg). The beads are rapidly prepared (∼10 min overall time) by fusing the blended mixture on an iridium strip resistance heater in an argon-purged chamber. Many elements can be measured in the glass bead, but the rare earth group in particular is a valuable series in nuclear forensic studies and is well-determined using LA-ICP-MS. The REE data obtained from the GRMs, presented as chondrite normalized patterns, are in very good agreement with consensus patterns. The UOCs have comparable patterns to solution ICP-MS methods and published data. The attractions of the current development are its conservation of sample, speed of preparation, and suitability for microbeam analysis, all of which are favorable for nuclear forensics practitioners and geochemists requiring REE patterns from scarce or valuable samples.

Preparation and screening of crystalline inorganic materials

DOEpatents

Schultz, Peter G [La Jolla, CA; Xiang, Xiaodong [Danville, CA; Goldwasser, Isy [Palo Alto, CA; Brice{hacek over }o, Gabriel; Sun, Xiao-Dong [Fremont, CA; Wang, Kai-An [Cupertino, CA

2008-10-28

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Preparation and screening of crystalline zeolite and hydrothermally-synthesized materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy; Briceno, Gabriel; Sun, Xiao-Dong; Wang, Kai-An

2005-03-08

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Interaction of nanodiamonds materials with influenza viruses

NASA Astrophysics Data System (ADS)

Ivanova, V. T.; Ivanova, M. V.; Spitsyn, B. V.; Garina, K. O.; Trushakova, S. V.; Manykin, A. A.; Korzhenevsky, A. P.; Burseva, E. I.

2012-02-01

The perspectives of the application of modern materials contained nanodiamonds (ND) are considered in this study. The interaction between detonation paniculate ND, soot and influenza A and B viruses, fragments of cDNA were analyzed at the normal conditions. It was shown that these sorbents can interact with the following viruses: reference epidemic strains of influenza A(H1N1), A(H1N1)v, A(H3N2) and B viruses circulated in the word in 2000-2010. The allantoises, concentrated viruses, cDNA can be absorbed by ND sorbents and getting removed from water solutions within 20 min. ND sorbents can be used for the preparation of antivirus filters for water solution and for future diagnostic systems in virology.

European Pharmacopoeia biological reference preparation for poliomyelitis vaccine (inactivated): collaborative study for the establishment of batch No. 3.

PubMed

Martin, J; Daas, A; Milne, C

2016-01-01

Inactivated poliomyelitis vaccines are an important part of the World Health Organization (WHO) control strategy to eradicate poliomyelitis. Requirements for the quality control of poliomyelitis vaccines (inactivated) include the use of an in vitro D antigen quantification assay for potency determination on the final lot as outlined in the European Pharmacopoeia (Ph. Eur.) monograph 0214. Performance of this assay requires a reference preparation calibrated in International Units (IU). A Ph. Eur. biological reference preparation (BRP) for poliomyelitis vaccine (inactivated) calibrated in IU has been established for this purpose. Due to the dwindling stocks of batch 2 of the BRP a collaborative study was run as part of the European Directorate for the Quality of Medicines & HealthCare (EDQM) Biological Standardisation Programme to establish BRP batch 3 (BRP3). Twelve laboratories including Official Medicines Control Laboratories (OMCLs) and manufacturers participated. The candidate BRP3 (cBRP3) was from the same source and had the same characteristics as BRP batch 2 (BRP2). During the study the candidate was calibrated against the 3 rd International Standard for inactivated poliomyelitis vaccine using in-house D antigen ELISA assays in line with the Ph. Eur. monograph 0214. The candidate was also compared to BRP2 to evaluate the continuity. Based on the results of the study, values of 320 DU/mL, 78 DU/mL and 288 DU/mL (D antigen units/mL) (IU) for poliovirus type 1, 2 and 3 respectively were assigned to the candidate. In June 2016, the Ph. Eur. Commission adopted the material as Ph. Eur. BRP for poliomyelitis vaccine (inactivated) batch 3.

La–Ce isotope measurements by multicollector-ICPMS† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c7ja00256d

PubMed Central

Münker, Carsten; Strub, Erik

2017-01-01

The 138La–138Ce decay system (half-life 1.02 × 1011 years) is a potentially highly useful tool to unravel information about the timing of geological processes and about the interaction of geological reservoirs on earth, complementing information from the more popular 147Sm–143Nd and 176Lu–176Hf isotope systems. Previously published analytical protocols were limited to TIMS. Here we present for the first time an analytical protocol that employs MC-ICPMS, with an improved precision and sensitivity. To perform sufficiently accurate La–Ce measurements, an efficient ion-chromatographic procedure is required to separate Ce from the other rare earth elements (REE) and Ba quantitatively. This study presents an improved ion-chromatographic procedure that separates La and Ce from rock samples using a three-step column separation. After REE separation by cation exchange, Ce is separated employing an Ln Spec column and selective oxidation. In the last step, a cation clean-up chemistry is performed to remove all remaining interferences. Our MC-ICPMS measurement protocol includes all stable Ce isotopes (136Ce, 138Ce, 140Ce and 142Ce), by employing a 1010 ohm amplifier for the most abundant isotope 140Ce. An external reproducibility of ±0.25ε-units (2 r.s.d) has been routinely achieved for 138Ce measurements for as little as 150–600 ng Ce, depending on the sample–skimmer cone combinations being used. Because the traditionally used JMC-304 Ce reference material is not commercially available anymore, a new reference material was prepared from AMES laboratory Ce metal (Cologne-AMES). In order to compare the new material with the previously reported isotopic composition of AMES material prepared at Mainz (Mainz-AMES), Cologne-AMES and JMC-304 were measured relative to each other in the same analytical session, demonstrating isotope heterogeneity between the two AMES and different JMC-304 batches used in the literature. To enable sufficiently precise age correction of radiogenic 138Ce and to perform isochron dating, a protocol was developed where La and Ce concentrations are determined by isotope dilution (ID), using an isotope tracer enriched in 138La and 142Ce. The new protocols were applied to determine the variations of Ce isotope compositions and La–Ce concentrations of certified geochemical reference materials (CRMs): BCR-2, BCR-1, BHVO-2, JR-1, JA-2, JB-3, JG-1, JR-1, JB-1b, AGV-1 and one in-house La Palma standard. PMID:29456283

Quality control evaluation of Keshamasi, Keshanjana and Keshamasi eye ointment

PubMed Central

Dhiman, Kartar Singh; Shukla, Vinay J.; Bhalodia, Nayan R.; Sharma, Vinay R.

2014-01-01

Background: Keshanjana (collyrium) is a well known Ayurvedic preparation prepared out of Keshamasi (ash prepared by scalp hairs) mixed with Goghrita (cow's ghee). This medicine is indicated for the treatment of Shushkakshipaka (dry eye syndrome) in the classical literature of Ayurveda; hence, it was under taken for standardization and clinical evaluation in an extra-mural research project from Central Council for Research in Ayurvedic Sciences, Department of AYUSH, New Delhi. Aim: To develop standard quality parameters for the Keshamasi, Keshanjana and Keshamasi ointment. Materials and Methods: Scalp hairs of male and females collected from saloons were converted to classical Masi Kalpana and mixed with cow ghee and petrolatum in the ratio of 1:5 to prepare the Keshanjana and Keshamasi ointment respectively. Standard Operation Procedure (SOP) were adopted and recorded accordingly. The raw material, furnished products and plain Goghrita were subjected for quality control parameters i.e., physico-chemical evaluation, anti-microbial study, particle size analysis, heavy metal analysis through inductive couple plasma spectroscopy with high performance thin layer liquid chromatography fingerprints. Results: Rancidity was negative in all the samples, indicating that the physico-chemical parameters are in acceptable range. Lead and zinc were present in most of the samples; while all samples are were free from microbial contamination. Conclusion: As no standards are available to compare the results of the current study, the observations cannot be compared. Thus the profile generated in the current study can be considered as standard to refer in future studies. PMID:25364202

Nano Traditional Chinese Medicine: Current Progresses and Future Challenges.

PubMed

Huang, Yi; Zhao, Yinglan; Liu, Fang; Liu, Songqing

2015-01-01

Nano traditional Chinese medicine (nano TCM) refers to bioactive ingredients, bioactive parts, medicinal materials or complex prescription, being approximately 100 nm in size, which are processed by nanotechnology. Nano TCM is a product of the TCM modernization, and is an application of nanotechnology in the field of TCM. This article reviews literatures on researches of nano TCM, which were published in the past 15 years. Different nanotechnologies have been used in preparation of Nano TCM in view of the varying aims of the study. The mechanical crushing technology is the main approach for nanolization of TCM material and complex prescription, and nanoparticulate drug delivery systems is the main approach for nanolization of bioactive ingredients or bioactive parts in TCM. Nano TCM has a number of advantages, for example, enhancing the bioavailability of TCM, reducing the adverse effects of TCM, achieving sustained release, attaining targeted delivery, enhancing pharmacological effects and improving the administration route of TCM. However, there are still many problems that must be resolved in nano TCM research. The main challenges to nano TCM include the theory system of TCM modernization, preparation technology, safety and stability, etc.

River sediment (S-37)--a new analytical quality control material ensuring comparability of chlorinated hydrocarbon analysis during an international environmental study in China.

PubMed

Gawlik, B M; Martens, D; Henkelmann, B; Schramm, K W; Kettrup, A; Muntau, H

2000-06-01

A sediment reference material (S-37) was prepared as analytical quality control material to be used within an international project on polychlorinated hydrocarbon analysis in two Chinese rivers. The raw material was sampled during a cruise on Yangtse River and transported afterwards to the JRC Ispra for further processing. The material was treated according to the general principles applicable for candidate reference material production. After a thorough homogeneity study of the bulk the material was bottled. A total of 1,080 bottles each containing 50 g of dry sediment powder was obtained. Final homogeneity and stability testing proved the material to be fit for the purpose. Isotope dilution GC/MS was used to establish target values for pentachlorobenzene (1.17 +/- 0.08 ng/g), hexachlorobenzene (3.60 +/- 0.17 ng/g), octachlorostyrene (0.19 +/- 0.01 ng/g), pentachloroanisole (0.52 +/- 0.02 ng/g), alpha-HCH (0.70 +/- 0.05 ng/g), beta-HCH (1.38 +/- 0.18 ng/g), gamma-HCH (0.83 +/- 038 ng/g), 2,4'-DDT (0.36 +/- 0.04 ng/g), 2,4'-DDE (0.29 +/- 0.02 ng/g), 2,4'-DDD (0.49 +/- 0.02), 4,4'-DDT (3.42 +/- 0.47 ng/g), 4,4'-DDD (1.29 +/- 0.17 ng/g), PCB 28 (0.11 +/- 0.01 ng/g), PCB 52 (0.09 +/- 0.003 ng/g), PCB 101 (0.07 +/- 0.003 ng/g), PCB 138 (0.06 +/- 0.003 ng/g) and PCB 153 (0.06 +/- 0.003 ng/g). Furthermore, indicative values for major and minor constituents as well as for polychlorinated dibenzodioxines and -furanes were measured.

Recent developments in the field of environmental reference materials at the JRC Ispra.

PubMed

Muntau, H

2001-06-01

The production of reference materials for environmental analysis started in the Joint Research Centre at Ispra/Italy in 1972 with the objective of later certification by the BCR, but for obvious budget reasons only a fraction of the total production achieved at Ispra ever reached certification level, although all materials were produced according to the severe quality requirements requested for certified reference materials. Therefore, the materials not destinated to certification are in growing demand as inter-laboratory test materials and as laboratory reference materials, for internal quality control, e.g., by control charts. The history of reference material production within the Joint Research Centre is briefly reviewed and the latest additions described. New developments such as micro-scale reference materials intended for analytical methods requiring sample intakes at milligram or sub-milligram level and therefor not finding supply on the reference material market, and "wet" environmental reference materials, which meet more precisely the "real-world" environmental analysis conditions, are presented and the state-of-the-art discussed.

Fast and accurate preparation fatty acid methyl esters by microwave-assisted derivatization in the yeast Saccharomyces cerevisiae.

PubMed

Khoomrung, Sakda; Chumnanpuen, Pramote; Jansa-ard, Suwanee; Nookaew, Intawat; Nielsen, Jens

2012-06-01

We present a fast and accurate method for preparation of fatty acid methyl esters (FAMEs) using microwave-assisted derivatization of fatty acids present in yeast samples. The esterification of free/bound fatty acids to FAMEs was completed within 5 min, which is 24 times faster than with conventional heating methods. The developed method was validated in two ways: (1) through comparison with a conventional method (hot plate) and (2) through validation with the standard reference material (SRM) 3275-2 omega-3 and omega-6 fatty acids in fish oil (from the Nation Institute of Standards and Technology, USA). There were no significant differences (P>0.05) in yields of FAMEs with both validations. By performing a simple modification of closed-vessel microwave heating, it was possible to carry out the esterification in Pyrex glass tubes kept inside the closed vessel. Hereby, we are able to increase the number of sample preparations to several hundred samples per day as the time for preparation of reused vessels was eliminated. Pretreated cell disruption steps are not required, since the direct FAME preparation provides equally quantitative results. The new microwave-assisted derivatization method facilitates the preparation of FAMEs directly from yeast cells, but the method is likely to also be applicable for other biological samples.

Integrated Data Collection Analysis (IDCA) Program - RDX Type II Class 5 Standard, Data Set 1

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

Sandstrom, Mary M.; Brown, Geoffrey W.; Preston, Daniel N.

This document describes the results of the first reference sample material—RDX Type II Class 5—examined in the proficiency study for small-scale safety and thermal (SSST) testing of explosive materials for the Integrated Data Collection Analysis (IDCA) Program. The IDCA program is conducting proficiency testing on homemade explosives (HMEs). The reference sample materials are being studied to establish the accuracy of traditional explosives safety testing for each performing laboratory. These results will be used for comparison to results from testing HMEs. This effort, funded by the Department of Homeland Security (DHS), ultimately will put the issues of safe handling of thesemore » materials in perspective with standard military explosives. The results of the study will add SSST testing results for a broad suite of different HMEs to the literature, potentially suggest new guidelines and methods for HME testing, and possibly establish what are the needed accuracies in SSST testing to develop safe handling practices. Described here are the results for impact, friction, electrostatic discharge, and scanning calorimetry analysis of a reference sample of RDX Type II Class 5. The results from each participating testing laboratory are compared using identical test material and preparation methods wherever possible. Note, however, the test procedures differ among the laboratories. These results are then compared to historical data from various sources. The performers involved are Lawrence Livermore National Laboratory (LLNL), Los Alamos National Laboratory (LANL), Air Force Research Laboratory/ RXQL (AFRL), Indian Head Division, Naval Surface Warfare Center, (IHD-NSWC), and Sandia National Laboratories (SNL). These tests are conducted as a proficiency study in order to establish some consistency in test protocols, procedures, and experiments and to understand how to compare results when test protocols are not identical.« less

Hydrologic almanac of Florida

USGS Publications Warehouse

Heath, Richard C.; Conover, Clyde Stuart

1981-01-01

This first edition is a ready reference source of information on various facts and features about water in Florida. It is aimed primarily to help bust politicians, writers, agency officials, water managers, planners, consultants, educators, hydrologists, engineers, scientists, and the general public answer questions that arise on comparative and statistical aspects on the hydrology of Florida. It contains statistical comparative data, much of which was especially prepared for the almanac, a glossary of technical terms, tabular material, and conversion factors. Also included is a selective bibliography of 174 reports on water in Florida. (USGS)

Transparent Tube Studies of Burning to Detonation Transition in Granular Explosives 1: Preliminary Framing Camera Studies

DTIC Science & Technology

1980-10-27

Reference 13. The 94/6 RDX/ wax (X893) and 97/3 RDX/ wax (X758) were mechanical mixtures prepared from Class A RDX (X597) and carnauba wax (N134). The...UKLAS9*TE SE,’CRITY CLASSIFICATION OF THIS PAGE (When Data Entered) ionization probes in previous steel tube studies. In charges of 94/6 RDX/ wax ...explosives (picric acid, tetryl, and RDX/ wax ) were among those materials in previous steel tube studies at NSWC which achieved deflagration to

[The overview of research on toxicological (forensic) chemistry based on the materials of the abstracts of dissertation theses. The forms and modes of information].

PubMed

Gorbacheva, N A; Orlova, A M

2012-01-01

The authors discuss the system of information about investigations on toxicological (forensic) chemistry carried out for obtaining the scientific degree as it has formed in this country. They present a review and a list of theses and their abstracts in this discipline defended during the period from 1936 to 2010. The analysis of the themes of the studies is performed with reference to the dynamics of preparation of the theses in the Soviet and post-Soviet periods.

Stable isotope quality assurance using the 'calibrated IRMS' strategy.

PubMed

Meijer, Harro A J

2009-06-01

Procedures in our laboratory have always been directed towards complete understanding of all processes involved and corrections needed etc., instead of relying fully on laboratory reference materials. This rather principal strategy (or attitude) is probably not optimal in the economic sense, and is not necessarily more accurate either. Still, it has proven to be very rewarding in its capability to detect caveats that go undiscovered in the standard way of measurement, but that do influence the accuracy or reliability of the measurement procedure. An additional benefit of our laboratory procedures is that it makes us capable of assisting the International Atomic Energy Agency (IAEA) with primary questions like mutual scale assignments and comparison of isotope ratios of the same isotope in different matrices (like delta(18)O in water, carbonates and atmospheric CO(2)), establishment of the (17)O-(18)O relation, and the replenishment of the calibration standards. Finally, for manual preparation systems with a low sample throughput (and thus only few reference materials analysed) it may well be the only way to produce reliable results.

Determination of arsenic in traditional Chinese medicine by microwave digestion with flow injection-inductively coupled plasma mass spectrometry (FI-ICP-MS).

PubMed

Ong, E S; Yong, Y L; Woo, S O

1999-01-01

A simple, rapid, and sensitive method with high sample throughput was developed for determining arsenic in traditional Chinese medicine (TCM) in the form of uncoated tablets, sugar-coated tablets, black pills, capsules, powders, and syrups. The method involves microwave digestion with flow injection-inductively coupled plasma mass spectrometry (FI-ICP-MS). Method precision was 2.7-10.1% (relative standard deviation, n = 6) for different concentrations of arsenic in different TCM samples analyzed by different analysts on different days. Method accuracy was checked with a certified reference material (sea lettuce, Ulva lactuca, BCR CRM 279) for external calibration and by spiking arsenic standard into different TCMs. Recoveries of 89-92% were obtained for the certified reference material and higher than 95% for spiked TCMs. Matrix interference was insignificant for samples analyzed by the method of standard addition. Hence, no correction equation was used in the analysis of arsenic in the samples studied. Sample preparation using microwave digestion gave results that were very similar to those obtained by conventional wet acid digestion using nitric acid.

Rapid and simple determination of selenium in blood serum by inductively coupled plasma-mass spectrometry (ICP-MS).

PubMed

Labat, L; Dehon, B; Lhermitte, M

2003-05-01

An inductively coupled plasma mass spectrometer (ICP-MS) with a rapid sample-preparative procedure was used for the determination of selenium in blood serum. Blood serum was prepared by dilution in an acidic solution consisting of nitric acid (1%), X-triton (0.1%) and 1-butanol (0.8%). A calibration curve was established for 1-40 microg mL(-1) (r(2)>0.99). The limit of detection was 0.5 microg mL(-1). Repeatability and intermediate precision were satisfactory with relative standard deviations (RSD) of 2.0% and 3.2%, respectively. This method was easily applied to reference materials with satisfactory accuracy. Good correlation (r(2)=0.96) was observed between ICP-MS and atomic absorption spectrometry (AAS) for the determination of (82)Se in blood serum from 23 patients. These results suggest that the sample preparative procedure coupled with ICP-MS can be used for the routine determination of (82)Se in human blood serum.

Optical method for determining the mechanical properties of a material

DOEpatents

Maris, H.J.; Stoner, R.J.

1998-12-01

Disclosed is a method for characterizing a sample, comprising the steps of: (a) acquiring data from the sample using at least one probe beam wavelength to measure, for times less than a few nanoseconds, a change in the reflectivity of the sample induced by a pump beam; (b) analyzing the data to determine at least one material property by comparing a background signal component of the data with data obtained for a similar delay time range from one or more samples prepared under conditions known to give rise to certain physical and chemical material properties; and (c) analyzing a component of the measured time dependent reflectivity caused by ultrasonic waves generated by the pump beam using the at least one determined material property. The first step of analyzing may include a step of interpolating between reference samples to obtain an intermediate set of material properties. The material properties may include sound velocity, density, and optical constants. In one embodiment, only a correlation is made with the background signal, and at least one of the structural phase, grain orientation, and stoichiometry is determined. 14 figs.

Method of making a layered composite electrode/electrolyte

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2005-01-25

An electrode/electrolyte structure is prepared by a plurality of methods. An unsintered (possibly bisque fired) moderately catalytic electronically-conductive or homogeneous mixed ionic electronic conductive electrode material is deposited on a layer composed of a sintered or unsintered ionically-conductive electrolyte material prior to being sintered. A layer of particulate electrode material is deposited on an unsintered ("green") layer of electrolyte material and the electrode and electrolyte layers are sintered simultaneously, sometimes referred to as "co-firing," under conditions suitable to fully densify the electrolyte while the electrode retains porosity. Or, the layer of particulate electrode material is deposited on a previously sintered layer of electrolyte, and then sintered. Subsequently, a catalytic material is added to the electrode structure by infiltration of an electrolcatalyst precursor (e.g., a metal salt such as a transition metal nitrate). This may be followed by low temperature firing to convert the precursor to catalyst. The invention allows for an electrode with high electronic conductivity and sufficient catalytic activity to achieve high power density in an ionic (electrochemical) device such as fuel cells and electrolytic gas separation systems.

Optical method for determining the mechanical properties of a material

DOEpatents

Maris, Humphrey J.; Stoner, Robert J.

1998-01-01

Disclosed is a method for characterizing a sample, comprising the steps of: (a) acquiring data from the sample using at least one probe beam wavelength to measure, for times less than a few nanoseconds, a change in the reflectivity of the sample induced by a pump beam; (b) analyzing the data to determine at least one material property by comparing a background signal component of the data with data obtained for a similar delay time range from one or more samples prepared under conditions known to give rise to certain physical and chemical material properties; and (c) analyzing a component of the measured time dependent reflectivity caused by ultrasonic waves generated by the pump beam using the at least one determined material property. The first step of analyzing may include a step of interpolating between reference samples to obtain an intermediate set of material properties. The material properties may include sound velocity, density, and optical constants. In one embodiment, only a correlation is made with the background signal, and at least one of the structural phase, grain orientation, and stoichiometry is determined.

Performance of Commercial Enzyme-Linked Immunosorbent Assays for Detection of Antibodies to Bordetella pertussis▿

PubMed Central

Riffelmann, M.; Thiel, K.; Schmetz, J.; Wirsing von Koenig, C. H.

2010-01-01

Measuring antibodies to Bordetella pertussis antigens is mostly done by enzyme-linked immunosorbent assays (ELISAs). We compared the performance of ELISA kits that were commercially available in Germany. Eleven measured IgG antibodies, and nine measured IgA antibodies. An in-house ELISA with purified antigens served as a reference method. Samples included two WHO reference preparations, the former Food and Drug Administration (FDA)/Center for Biologics Evaluation and Research (CBER) reference preparations, serum samples from patients with clinically suspected pertussis, and serum samples from patients having received a combined tetanus, diphtheria, and pertussis (Tdap) vaccination. Kits using pertussis toxin (PT) as an antigen showed linearity compared to the WHO Reference preparation (r2 between 0.82 and 0.99), and these kits could quantify antibodies according to the reference preparation. ELISA kits using mixed antigens showed no linear correlation to the reference preparations. Patient results were compared to results of in-house ELISAs using a dual cutoff of either ≥100 IU/ml anti-PT IgG or ≥40 IU/ml anti-PT IgG together with ≥12 IU/ml anti-PT IgA. The sensitivities of kits measuring IgG antibodies ranged between 0.84 and 1.00. The specificities of kits using PT as an antigen were between 0.81 and 0.93. The specificities of kits using mixed antigens were between 0.51 and 0.59 and were thus not acceptable. The sensitivities of kits measuring IgA antibodies ranged between 0.53 and 0.73, and the specificities were between 0.67 and 0.94, indicating that IgA antibodies may be of limited diagnostic value. Our data suggest that ELISAs should use purified PT as an antigen and be standardized to the 1st International Reference preparation. PMID:20943873

Identification of Metal Oxide Nanoparticles in Histological Samples by Enhanced Darkfield Microscopy and Hyperspectral Mapping.

PubMed

Roth, Gary A; Sosa Peña, Maria del Pilar; Neu-Baker, Nicole M; Tahiliani, Sahil; Brenner, Sara A

2015-12-08

Nanomaterials are increasingly prevalent throughout industry, manufacturing, and biomedical research. The need for tools and techniques that aid in the identification, localization, and characterization of nanoscale materials in biological samples is on the rise. Currently available methods, such as electron microscopy, tend to be resource-intensive, making their use prohibitive for much of the research community. Enhanced darkfield microscopy complemented with a hyperspectral imaging system may provide a solution to this bottleneck by enabling rapid and less expensive characterization of nanoparticles in histological samples. This method allows for high-contrast nanoscale imaging as well as nanomaterial identification. For this technique, histological tissue samples are prepared as they would be for light-based microscopy. First, positive control samples are analyzed to generate the reference spectra that will enable the detection of a material of interest in the sample. Negative controls without the material of interest are also analyzed in order to improve specificity (reduce false positives). Samples can then be imaged and analyzed using methods and software for hyperspectral microscopy or matched against these reference spectra in order to provide maps of the location of materials of interest in a sample. The technique is particularly well-suited for materials with highly unique reflectance spectra, such as noble metals, but is also applicable to other materials, such as semi-metallic oxides. This technique provides information that is difficult to acquire from histological samples without the use of electron microscopy techniques, which may provide higher sensitivity and resolution, but are vastly more resource-intensive and time-consuming than light microscopy.

Decommissioning Handbook

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

Not Available

1994-03-01

The Decommissioning Handbook is a technical guide for the decommissioning of nuclear facilities. The decommissioning of a nuclear facility involves the removal of the radioactive and, for practical reasons, hazardous materials to enable the facility to be released and not represent a further risk to human health and the environment. This handbook identifies and technologies and techniques that will accomplish these objectives. The emphasis in this handbook is on characterization; waste treatment; decontamination; dismantling, segmenting, demolition; and remote technologies. Other aspects that are discussed in some detail include the regulations governing decommissioning, worker and environmental protection, and packaging and transportationmore » of the waste materials. The handbook describes in general terms the overall decommissioning project, including planning, cost estimating, and operating practices that would ease preparation of the Decommissioning Plan and the decommissioning itself. The reader is referred to other documents for more detailed information. This Decommissioning Handbook has been prepared by Enserch Environmental Corporation for the US Department of Energy and is a complete restructuring of the original handbook developed in 1980 by Nuclear Energy Services. The significant changes between the two documents are the addition of current and the deletion of obsolete technologies and the addition of chapters on project planning and the Decommissioning Plan, regulatory requirements, characterization, remote technology, and packaging and transportation of the waste materials.« less

Performance of Bi2O3/TiO2 prepared by sol-gel on p-Cresol degradation under solar and visible light.

PubMed

Vigil-Castillo, Héctor H; Hernández-Ramírez, Aracely; Guzmán-Mar, Jorge L; Ramos-Delgado, Norma A; Villanueva-Rodríguez, Minerva

2018-05-21

Photocatalytic degradation of p-Cresol was evaluated using the mixed oxide Bi 2 O 3 /TiO 2 (containing 2 and 20% wt. Bi 2 O 3 referred as TB2 and TB20) and was compared with bare TiO 2 under simulated solar radiation. Materials were prepared by the classic sol-gel method. All solids exhibited the anatase phase by X-ray diffraction (XRD) and Raman spectroscopy. The synthesized materials presented lower crystallite size and Eg value, and also higher surface area as Bi 2 O 3 amount was increased. Bi content was quantified showing near to 70% of theoretical values in TB2 and TB20. Bi 2 O 3 incorporation also was demonstrated by X-ray photoelectron spectroscopy (XPS). Characterization of mixed oxides suggests a homogeneous distribution of Bi 2 O 3 on TiO 2 surface. Photocatalytic tests were carried out using a catalyst loading of 1 g L -1 under simulated solar light and visible light. The incorporation of Bi 2 O 3 in TiO 2 improved the photocatalytic properties of the synthesized materials obtaining better results with TB20 than the unmodified TiO 2 under both radiation sources.

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

Eppich, Gary R.; Williams, Ross W.; Gaffney, Amy M.

Here, age dating of nuclear material can provide insight into source and suspected use in nuclear forensic investigations. We report here a method for the determination of the date of most recent chemical purification for uranium materials using the 235U- 231Pa chronometer. Protactinium is separated from uranium and neptunium matrices using anion exchange resin, followed by sorption of Pa to an SiO 2 medium. The concentration of 231Pa is measured by isotope dilution mass spectrometry using 233Pa spikes prepared from an aliquot of 237Np and calibrated in-house using the rock standard Table Mountain Latite and the uranium isotopic standard U100.more » Combined uncertainties of age dates using this method are 1.5 to 3.5 %, an improvement over alpha spectrometry measurement methods. Model ages of five uranium standard reference materials are presented; all standards have concordant 235U- 231Pa and 234U- 230Th model ages.« less

Environmental test program for superconducting materials and devices

NASA Technical Reports Server (NTRS)

Haertling, Gene; Randolph, Henry; Hsi, Chi-Shiung; Verbelyi, Darren

1992-01-01

A systematic approach to obtaining real time, superconducting YBa2Cu30(7-x) materials is presented. The work was carried out under the overall direction of Clemson University with tasks being performed at both Clemson and Westinghouse (Aiken, SC). Clemson prepared the tapecast superconducting 123 material and fabricated in into substrate-supported, environmentally-protected conducting links. Following this, all of the elements were individually tested for resistance vs. temperature and Tc; and then a portion of them were kept at Clemson for further testing while a randomly selected group was delivered to Westinghouse for specialized testing and evaluation in their low temperature/high vacuum and radiation facilities. In addition, a number of control samples (12 ea.) were put on the shelf at Clemson for further reference at the end of the testing period. The specific tests conducted at Clemson and Westinghouse/SRC are presented with a summary of the results.

Polymerase chain reaction technology as analytical tool in agricultural biotechnology.

PubMed

Lipp, Markus; Shillito, Raymond; Giroux, Randal; Spiegelhalter, Frank; Charlton, Stacy; Pinero, David; Song, Ping

2005-01-01

The agricultural biotechnology industry applies polymerase chain reaction (PCR) technology at numerous points in product development. Commodity and food companies as well as third-party diagnostic testing companies also rely on PCR technology for a number of purposes. The primary use of the technology is to verify the presence or absence of genetically modified (GM) material in a product or to quantify the amount of GM material present in a product. This article describes the fundamental elements of PCR analysis and its application to the testing of grains. The document highlights the many areas to which attention must be paid in order to produce reliable test results. These include sample preparation, method validation, choice of appropriate reference materials, and biological and instrumental sources of error. The article also discusses issues related to the analysis of different matrixes and the effect they may have on the accuracy of the PCR analytical results.

Development of near-zero water consumption cement materials via the geopolymerization of tektites and its implication for lunar construction

PubMed Central

Wang, Kai-tuo; Tang, Qing; Cui, Xue-min; He, Yan; Liu, Le-ping

2016-01-01

The environment on the lunar surface poses some difficult challenges to building long-term lunar bases; therefore, scientists and engineers have proposed the creation of habitats using lunar building materials. These materials must meet the following conditions: be resistant to severe lunar temperature cycles, be stable in a vacuum environment, have minimal water requirements, and be sourced from local Moon materials. Therefore, the preparation of lunar building materials that use lunar resources is preferred. Here, we present a potential lunar cement material that was fabricated using tektite powder and a sodium hydroxide activator and is based on geopolymer technology. Geopolymer materials have the following properties: approximately zero water consumption, resistance to high- and low-temperature cycling, vacuum stability and good mechanical properties. Although the tektite powder is not equivalent to lunar soil, we speculate that the alkali activated activity of lunar soil will be higher than that of tektite because of its low Si/Al composition ratio. This assumption is based on the tektite geopolymerization research and associated references. In summary, this study provides a feasible approach for developing lunar cement materials using a possible water recycling system based on geopolymer technology. PMID:27406467

Development of near-zero water consumption cement materials via the geopolymerization of tektites and its implication for lunar construction.

PubMed

Wang, Kai-Tuo; Tang, Qing; Cui, Xue-Min; He, Yan; Liu, Le-Ping

2016-07-13

The environment on the lunar surface poses some difficult challenges to building long-term lunar bases; therefore, scientists and engineers have proposed the creation of habitats using lunar building materials. These materials must meet the following conditions: be resistant to severe lunar temperature cycles, be stable in a vacuum environment, have minimal water requirements, and be sourced from local Moon materials. Therefore, the preparation of lunar building materials that use lunar resources is preferred. Here, we present a potential lunar cement material that was fabricated using tektite powder and a sodium hydroxide activator and is based on geopolymer technology. Geopolymer materials have the following properties: approximately zero water consumption, resistance to high- and low-temperature cycling, vacuum stability and good mechanical properties. Although the tektite powder is not equivalent to lunar soil, we speculate that the alkali activated activity of lunar soil will be higher than that of tektite because of its low Si/Al composition ratio. This assumption is based on the tektite geopolymerization research and associated references. In summary, this study provides a feasible approach for developing lunar cement materials using a possible water recycling system based on geopolymer technology.

Experimental Study on Reaction Characteristics of PTFE/Ti/W Energetic Materials under Explosive Loading

PubMed Central

Li, Yan; Jiang, Chunlan; Wang, Zaicheng; Luo, Puguang

2016-01-01

Metal/fluoropolymer composites represent a new category of energetic structural materials that release energy through exothermic chemical reactions initiated under shock loading conditions. This paper describes an experiment designed to study the reaction characteristics of energetic materials with low porosity under explosive loading. Three PTFE (polytetrafluoroethylene)/Ti/W mixtures with different W contents are processed through pressing and sintering. An inert PTFE/W mixture without reactive Ti particles is also prepared to serve as a reference. Shock-induced chemical reactions are recorded by high-speed video through a narrow observation window. Related shock parameters are calculated based on experimental data, and differences in energy release are discussed. The results show that the reaction propagation of PTFE/Ti/W energetic materials with low porosity under explosive loading is not self-sustained. As propagation distance increases, the energy release gradually decreases. In addition, reaction failure distance in PTFE/Ti/W composites is inversely proportional to the W content. Porosity increased the failure distance due to higher shock temperature. PMID:28774056

Effects of materials containing antimicrobial compounds on food hygiene.

PubMed

Møretrø, Trond; Langsrud, Solveig

2011-07-01

Surfaces with microorganisms may transfer unwanted microorganisms to food through cross-contamination during processing and preparation. A high hygienic status of surfaces that come in contact with food is important in order to reduce the risk of cross-contamination. During the last decade, products containing antimicrobial compounds, such as cutting boards, knives, countertops, kitchen utensils, refrigerators, and conveyor belts, have been introduced to the market, claiming hygienic effects. Such products are often referred to as "treated articles." Here we review various aspects related to treated articles intended for use during preparation and processing of food. Regulatory issues and methods to assess antibacterial effects are covered. Different concepts for treated articles as well as their antibacterial activity are reviewed. The effects of products with antimicrobials on food hygiene and safety are discussed. Copyright ©, International Association for Food Protection

Setting maximum limits for trace elements in baby food in European legislation: the outcome of International Measurement Evaluation Programme®-33.

PubMed

Cordeiro, F; Baer, I; Robouch, P; Emteborg, H; Can, S Z; Krata, A; Zampella, M; Quétel, C R; Hearn, R; De la Calle, B

2013-01-01

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme® (IMEP). It organises various types of inter-laboratory comparisons in support of European Union policies. This paper presents the results of a proficiency testing exercise (PT) focusing on the determination of total cadmium (Cd) and total lead (Pb) mass fractions in baby food in support to Commission Regulation (EC) 1881/2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs. The test material used in this exercise was soya-based baby food formula purchased in a local pharmacy and prepared by the Reference Materials Unit of the IRMM for this exercise. Sixty-six laboratories from 23 countries registered to the exercise and 61 of them reported results. Each participant received one bottle containing approximately 15 g of test material. Participants were asked to quantify the measurands in the powder and in the reconstituted formula. Reference values independent from the participants' results were established using isotope dilution inductively coupled plasma mass spectrometry. The total Cd mass fraction was determined by IRMM and LGC Ltd (UK), while the total Pb was determined by IRMM. The standard deviation for proficiency assessment σ^ was set at 22% of the assigned value for all measurands. Laboratories were rated with z- and ζ- (zeta) scores in accordance with ISO 13528. The outcome of this exercise is clearly influenced by the very low level of Cd and Pb content in the test material which triggered: a high number of 'less than' values; overestimated values especially for Pb very likely due to contamination; and a visible method influence in the case of Pb (methods based on atomic absorption were not sensitive enough to attain such low limits of detection). The results were also evaluated with regard to the reported limit of detection and some incoherencies were observed.

The processing and collaborative assay of a reference endotoxin.

PubMed

Hochstein, H D; Mills, D F; Outschoorn, A S; Rastogi, S C

1983-10-01

A preparation of Escherichia coli bacterial endotoxin, the latest of successive lots drawn from bulk material which has been studied in laboratory tests and in animals and humans for suitability as a reference endotoxin, has been filled and lyophilized in a large number of vials. Details of its characterization, including stability studies, are given. A collaborative assay was conducted by 14 laboratories using gelation end-points with Limulus amebocyte lysates. Approximate continuity of the unit of potency with the existing national unit was achieved. The lot was made from the single final bulk but had to be freeze-dried in five sublimators. An assessment was therefore made for possible heterogeneity. The results indicate that the lot can be used as a large homogeneous quantity. The advantages of using it widely as a standard for endotoxins are discussed.

Screening combinatorial arrays of inorganic materials with spectroscopy or microscopy

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2004-02-03

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial synthesis of novel materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

1999-01-01

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial sythesis of organometallic materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2002-07-16

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Polymer arrays from the combinatorial synthesis of novel materials

DOEpatents

Schultz, Peter G.; Xiang, Xiao-Dong; Goldwasser, Isy; Briceno, Gabriel; Sun, Xiao-Dong

2004-09-21

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial synthesis of novel materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2002-02-12

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial synthesis of novel materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

1999-12-21

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial synthesis of novel materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2001-01-01

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Combinatorial screening of inorganic and organometallic materials

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2002-01-01

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Development of references of anomalies detection on P91 material using Self-Magnetic Leakage Field (SMLF) technique

NASA Astrophysics Data System (ADS)

Husin, Shuib; Afiq Pauzi, Ahmad; Yunus, Salmi Mohd; Ghafar, Mohd Hafiz Abdul; Adilin Sekari, Saiful

2017-10-01

This technical paper demonstrates the successful of the application of self-magnetic leakage field (SMLF) technique in detecting anomalies in weldment of a thick P91 materials joint (1 inch thickness). Boiler components such as boiler tubes, stub boiler at penthouse and energy piping such as hot reheat pipe (HRP) and H-balance energy piping to turbine are made of P91 material. P91 is ferromagnetic material, therefore the technique of self-magnetic leakage field (SMLF) is applicable for P91 in detecting anomalies within material (internal defects). The technique is categorized under non-destructive technique (NDT). It is the second passive method after acoustic emission (AE), at which the information on structures radiation (magnetic field and energy waves) is used. The measured magnetic leakage field of a product or component is a magnetic leakage field occurring on the component’s surface in the zone of dislocation stable slipbands under the influence of operational (in-service) or residual stresses or in zones of maximum inhomogeneity of metal structure in new products or components. Inter-granular and trans-granular cracks, inclusion, void, cavity and corrosion are considered types of inhomogeneity and discontinuity in material where obviously the output of magnetic leakage field will be shown when using this technique. The technique does not required surface preparation for the component to be inspected. This technique is contact-type inspection, which means the sensor has to touch or in-contact to the component’s surface during inspection. The results of application of SMLF technique on the developed P91 reference blocks have demonstrated that the technique is practical to be used for anomaly inspection and detection as well as identification of anomalies’ location. The evaluation of this passive self-magnetic leakage field (SMLF) technique has been verified by other conventional non-destructive tests (NDTs) on the reference blocks where simulated defects/anomalies have been developed inside at the weldment. The results from the inspection test showed that the signatures of magnetic leakage field gradient distribution prove that the peak is found on the location of defect/anomaly in the reference block. It is in agreement with the evidence of anomaly that seen in the radiography test film (RT).

Flame resistant cellulose fiber insulation and process of preparing it

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

Quinto, M.J.

1979-11-06

This invention produces flame resistant cellulose fiber insulation, which will be referred to as CFI. The best flameproofing agents which have been used in the past are mixtures of boric acid and borax as the major portion of the mix and have been applied both as dry powders and sprayed from water dispersions. Boric acid is quite expensive as it is prepared from borax by the addition of acid and purification of the boric acid. In the present invention lower cost materials and process are obtained by applying a mixture of boric acid and borax which has been prepared bymore » adding acid, such as sulfuric acid, a mixture of sulfuric and phosphoric acid, and the like, to borax to transform a portion of the borax into boric acid. The reaction products, sodium sulfate, or a mixture of sodium sulfate and sodium phosphate in the case both acids are used, remain in the material applied to CFI. While they are not by themselves highly effective flameproofing agents, particularly sodium sulfate is not, they do add somewhat to flame resistance. In other words, wht elimination of the step of separating and/or purifying boric acid is eliminated without, however, eliminating its function. The product produced is as good a flame retarder when applied to CFI; in fact it is slightly better. Additionally there are great savings in cost.« less

The establishment of a WHO Reference Reagent for anti-malaria (Plasmodium falciparum) human serum.

PubMed

Bryan, Donna; Silva, Nilupa; Rigsby, Peter; Dougall, Thomas; Corran, Patrick; Bowyer, Paul W; Ho, Mei Mei

2017-08-05

At a World Health Organization (WHO) sponsored meeting it was concluded that there is an urgent need for a reference preparation that contains antibodies against malaria antigens in order to support serology studies and vaccine development. It was proposed that this reference would take the form of a lyophilized serum or plasma pool from a malaria-endemic area. In response, an immunoassay standard, comprising defibrinated human plasma has been prepared and evaluated in a collaborative study. A pool of human plasma from a malaria endemic region was collected from 140 single plasma donations selected for reactivity to Plasmodium falciparum apical membrane antigen-1 (AMA-1) and merozoite surface proteins (MSP-1 19 , MSP-1 42 , MSP-2 and MSP-3). This pool was defibrinated, filled and freeze dried into a single batch of ampoules to yield a stable source of naturally occurring antibodies to P. falciparum. The preparation was evaluated by an enzyme-linked immunosorbent assay (ELISA) in a collaborative study with sixteen participants from twelve different countries. This anti-malaria human serum preparation (NIBSC Code: 10/198) was adopted by the WHO Expert Committee on Biological Standardization (ECBS) in October 2014, as the first WHO reference reagent for anti-malaria (Plasmodium falciparum) human serum with an assigned arbitrary unitage of 100 units (U) per ampoule. Analysis of the reference reagent in a collaborative study has demonstrated the benefit of this preparation for the reduction in inter- and intra-laboratory variability in ELISA. Whilst locally sourced pools are regularly use for harmonization both within and between a few laboratories, the presence of a WHO-endorsed reference reagent should enable optimal harmonization of malaria serological assays either by direct use of the reference reagent or calibration of local standards against this WHO reference. The intended uses of this reference reagent, a multivalent preparation, are (1) to allow cross-comparisons of results of vaccine trials performed in different centres/with different products; (2) to facilitate standardization and harmonization of immunological assays used in epidemiology research; and (3) to allow optimization and validation of immunological assays used in malaria vaccine development.

Preparation of pyrolysis reference samples: evaluation of a standard method using a tube furnace.

PubMed

Sandercock, P Mark L

2012-05-01

A new, simple method for the reproducible creation of pyrolysis products from different materials that may be found at a fire scene is described. A temperature programmable steady-state tube furnace was used to generate pyrolysis products from different substrates, including softwoods, paper, vinyl sheet flooring, and carpet. The temperature profile of the tube furnace was characterized, and the suitability of the method to reproducibly create pyrolysates similar to those found in real fire debris was assessed. The use of this method to create proficiency tests to realistically test an examiner's ability to interpret complex gas chromatograph-mass spectrometric fire debris data, and to create a library of pyrolsates generated from materials commonly found at a fire scene, is demonstrated. © 2011 American Academy of Forensic Sciences.

Combinatorial synthesis and screening of non-biological polymers

DOEpatents

Schultz, Peter G.; Xiang, Xiao-Dong; Goldwasser, Isy; Briceno, Gabriel; Sun, Xiao-Dong; Wang, Kai-An

2006-04-25

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Giant magnetoresistive cobalt oxide compounds

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

1998-01-01

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Giant magnetoresistive cobalt oxide compounds

DOEpatents

Schultz, P.G.; Xiang, X.; Goldwasser, I.

1998-07-07

Methods and apparatus are disclosed for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties. 58 figs.

Synthesis and screening combinatorial arrays of zeolites

DOEpatents

Schultz, Peter G.; Xiang, Xiaodong; Goldwasser, Isy

2003-11-18

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, non-biological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

Radiopacity of different resin-based and conventional luting cements compared to human and bovine teeth.

PubMed

Pekkan, Gürel; Ozcan, Mutlu

2012-02-03

This study evaluated the radiopacity of different resin-based luting materials and compared the results to human and bovine dental hard tissues. Disc specimens (N=130, n=10 per group) (diameter: 6 mm, thickness: 1 mm) were prepared from 10 resin-based and 3 conventional luting cements. Human canine dentin (n=10), bovine enamel (n=10), bovine dentin (n=10) and Aluminium (Al) step wedge were used as references. The optical density values of each material were measured from radiographic images using a transmission densitometer. Al step wedge thickness and optical density values were plotted and equivalent Al thickness values were determined for radiopacity measurements of each material. The radiopacity values of conventional cements and two resin luting materials (Rely X Unicem and Variolink II), were significantly higher than that of bovine enamel that could be preferred for restorations cemented on enamel. Since all examined resin-based luting materials showed radiopacity values equivalent to or greater than that of human and bovine dentin, they could be considered suitable for the restorations cemented on dentin.

[Evidential value of dental materials identification by infrared spectroscopy in forensic medicine opinionating].

PubMed

Wachowiak, Roman; Strach, Bogna

2007-01-01

The potential for a release of dental restoration material or a spontaneous loss of a tooth structure fragment in the course of mastication frequently requires a reliable identification of the lost fragment in order to confirm its origin. The consequences of incidental mechanical injuries -- in view of the presence of dangerous solid fragments -- become particularly important in cases of using a chewing gum. The problem involves distinguishing between the structure of a fragment of restoration or a broken tooth structure and incidental contaminants of chewing gum produced in the process of gum manufacturing. The consequences of mechanical injuries or exposure to potential structural tooth damage in the course of gum chewing provide a subject for numerous litigations against manufacturer of chewing gum and require appropriate identification of the material. The studies were conducted using solid phase infrared spectroscopy in the range of 500-4000 wavelength (cm(-1)) for a quick identification of dental materials used in the dental practice. A database of infrared transmission spectra characteristic of commonly employed dental filling materials was prepared to provide a systemic reference system, useful in controversial interpretation cases.

Recommendations for reference method for haemoglobinometry in human blood (ICSH standard 1986) and specifications for international haemiglobincyanide reference preparation (3rd edition). International Committee for Standardization in Haematology; Expert Panel on Haemoglobinometry.

PubMed

1987-01-01

Scientific symposia on haemoglobinometry were held at the 9th Congress of the European Society of Haematology, Lisbon, 1963 (ESH 1964) and the 10th Congress of the International Society of Haematology (ISH), Stockholm, 1964 (ISH 1965). The International Committee for Standardization in Haematology (ICSH) made recommendations endorsed by the General Assembly of ICSH in Sydney on 23 August 1966 (ICSH 1967), for a reference method for haemoglobinometry and for the manufacture and distribution of an international reference preparation. Further symposia were held at the 12th Congress of the ISH, New York, 1968 (Astaldi, Sirtori & Vanzetti 1979) and at the 13th Congress of ISH, Munich, 1970 (Izak & Lewis 1972). The recommendations were reissued in 1978 (ISH 1978). On the basis of continuing experimental studies, the reference method and the specifications for the international reference preparation have been modified. The revised recommendations are described in this document.

Validation of a dilute and shoot method for quantification of 12 elements by inductively coupled plasma tandem mass spectrometry in human milk and in cow milk preparations.

PubMed

Dubascoux, Stéphane; Andrey, Daniel; Vigo, Mario; Kastenmayer, Peter; Poitevin, Eric

2018-09-01

Nutritional information about human milk is essential as early human growth and development have been closely linked to the status and requirements of several macro- and micro-elements. However, methods addressing whole mineral profiling in human milk have been scarce due in part to their technical complexities to accurately and simultaneously measure the concentration of micro- and macro-trace elements in low volume of human milk. In the present study, a single laboratory validation has been performed using a "dilute and shoot" approach for the quantification of sodium (Na), magnesium (Mg), phosphorus (P), potassium (K), calcium (Ca), manganese (Mn), iron (Fe), copper (Cu), zinc (Zn), selenium (Se), molybdenum (Mo) and iodine (I), in both human milk and milk preparations. Performances in terms of limits of detection and quantification, of repeatability, reproducibility and trueness have been assessed and verified using various reference or certified materials. For certified human milk sample (NIST 1953), recoveries obtained for reference or spiked values are ranged from 93% to 108% (except for Mn at 151%). This robust method using new technology ICP-MS/MS without high pressure digestion is adapted to both routinely and rapidly analyze human milk micro-sample (i.e. less than 250 μL) in the frame of clinical trials but also to be extended to the mineral profiling of milk preparations like infant formula and adult nutritionals. Copyright © 2018 Elsevier GmbH. All rights reserved.

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

PubMed

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

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

Nuclear reference materials to meet the changing needs of the global nuclear community

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

Martin, H.R.; Gradle, C.G.; Narayanan, U.I.

New Brunswick Laboratory (NBL) serves as the U.S. Government`s certifying authority for nuclear reference materials and measurement calibration standards. In this role, NBL provides nuclear reference materials certified for chemical and/or isotopic compositions traceable to a nationally accepted, internationally compatible reference base. Emphasis is now changing as to the types of traceable nuclear reference materials needed as operations change within the Department of Energy complex and at nuclear facilities around the world. New challenges include: environmental and waste minimization issues, facilities and materials transitioning from processing to storage modes with corresponding changes in the types of measurements being performed, emphasismore » on requirements for characterization of waste materials, and difficulties in transporting nuclear materials and international factors, including IAEA influences. During these changing times, it is critical that traceable reference materials be provided for calibration or validation of the performance of measurement systems. This paper will describe actions taken and planned to meet the changing reference material needs of the global nuclear community.« less

Final report on CCQM-K80: Comparison of value-assigned CRMs and PT materials: Creatinine in human serum

NASA Astrophysics Data System (ADS)

Camara, Johanna E.; Duewer, David L.; Gasca Aragon, Hugo; Lippa, Katrice A.; Toman, Blaza

2013-01-01

The 2009 CCQM-K80 'Comparison of value-assigned CRMs and PT materials: creatinine in human serum' is the first in a series of key comparisons directly testing the chemical measurement services provided to customers by National Metrology Institutes (NMIs) and Designated Institutes. CCQM-K80 compared the assigned serum creatinine values of certified reference materials (CRMs) using measurements made on these materials under repeatability conditions. Six NMIs submitted 17 CRM materials for evaluation, all intended for sale to customers. These materials represent nearly all of the higher-order CRMs then available for this clinically important measurand. The certified creatinine mass fraction in the materials ranged from 3 mg/kg to 57 mg/kg. All materials were stored and prepared according the specifications provided by each NMI. Samples were processed and analyzed under repeatability conditions by one analyst using isotope dilution liquid chromatography-mass spectrometry. The instrumental repeatability imprecision, expressed as a percent relative standard deviation, was 1.2%. Given the number of materials and the time required for each analysis, the measurements were made in two measurement campaigns ('runs'). In both campaigns, replicate analyses (two injections of one preparation separated in time) were made on each of two or three independently prepared aliquots from one randomly selected unit of each of the 17 materials. The mean value, between-campaign, between-aliquot and between-replicate variance components, standard uncertainty of the mean value, and the number of degrees of freedom associated with the standard uncertainty were estimated using a linear mixed model. Since several of the uncertainties estimated using this traditional frequentist approach were associated with a single degree of freedom, Markov Chain Monte Carlo Bayesian analysis was used to estimate 95% level-of-confidence coverage intervals, U95. Uncertainty-weighted generalized distance regression was used to establish the key comparison reference function (KCRF) relating the assigned values to the repeatability measurements. Parametric bootstrap Monte Carlo was used to estimate 95% level-of-confidence coverage intervals for the degrees of equivalence of materials, d +/- U95(d), and of the participating NMIs, D +/- U95(D). Because of the wide range of creatinine mass fraction in the materials, these degrees of equivalence are expressed in percent relative form: %d +/- U95(%d) and %D +/- U95(%D). On the basis of leave-one-out cross-validation, the assigned values for 16 of the 17 materials were deemed equivalent at the 95% level of confidence. These materials were used to define the KCRF. The excluded material was identified as having a marginally underestimated assigned uncertainty, giving it large and potentially anomalous influence on the KCRF. However, this material's %d of 1.4 +/- 1.5 indicates that it is equivalent with the other materials at the 95% level of confidence. The median |%d| for all 17 of the materials is 0.3 with a median U95(%d) of 1.9. All of these higher-order CRMs for creatinine in human serum are equivalent within their assigned uncertainties. The median |%D| for the participating NMIs is 0.3 with a median U95(%D) of 2.1. These results demonstrate that all participating NMIs have the ability to correctly value-assign CRMs and proficiency test materials for creatinine in human serum and similar measurands. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

PA01.34. Catagorical interpretation in Microsoft excel of jangam dravya database from Bruhat-Trayi & Laghu-Trayi

PubMed Central

Saraf, Abhijeet

2012-01-01

Purpose: Not a single drug in Ayurveda has been termed as non-medicinal. This means every Dravya has medicinal value in this world. Jangam dravya is an animal sourced medicine. In samhita Jangam Dravya are described first. So as per Krama Varnan Vichar, Jangam Dravyas are significant in this type. In Ayurvedic literature there is more literature on Audbhid & Parthiva Dravyas. I Total available nighantu: more than 25. Total available Rasa Grantha: about 145. There is no one Grantha on Jangam Dravya which describes their whole information. Jangam Dravyas are described in Ayurvedic literature in different views and in different branches. Gross description is available in Samhitas. But they aren’t in format. They are not compiled according to their Guna Karma, Upayogitwa, Vyadhiharatwa, and Kalpa etc. Their use in Chikitsa is minimal as their ready references are not available, though very much effective. So due to sheer need of compilation of these references this topic was selected for study. The basic need for study of Jangam Dravya is to prepare its whole DATABASE. So through this study Database of Jangam Dravya can be available like Jangam Dravya. Method: Selection of topic this is a fundamental & literary study, Selection of material, Selection of Database software & font, Collection of data & preparation of Master Chart, Preparation of Database, Interpretation & summarization of data. Result: So in this paper, we are going to focus on literature availability of jangam dravya with the help of modern technique like Microsoft Excel. And also how we can prepare and use the categorical interpretation of jangam dravya with help of database Conclusion: Jangam Dravyas are described in Ayurvedic literature in different views and in different branches. Importances of these dravyas are the main key point of this study.

Electric Utility Rate Design Study: reference manual and procedures for implementing PURPA

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

Not Available

State regulatory commissions will be assisted by using this manual in carrying out their responsibilities under the National Energy Act, specifically under the Public Utilities Regulatory Policies Act (PURPA). The research and materials of the Rate Design Study are basically applicable to Title I of PURPA, and the Manual covers only that part of the Act. The Rate Design Study covers a wide scope of research and professional opinions and are a major reference source for data, information, and divergent views on practically every aspect of electric utility rate design. The introductory part calls attention to particularly important aspects ofmore » responsibilities, authority, and procedures. The second part outlines the specific responsibilities placed by Title I of PURPA on the State commissions. Part 3 discusses some of the procedural and substantive requirements and options of PURPA with particular emphasis on their relation to the Rate Design Study, State law, and State regulatory policies. Part 4 is an independent analysis that includes cross-indexed references to the more than 60 reports prepared by the Rate Design Study and also to other pertinent sources of information and data. Part 5 summarizes a survey conducted in January 1979 of State commission actions related to the matters contained in Title I of PURPA. Part 6 presents the text of the law. Part 7 is the request from NARUC that prompted the preparation of the Manual. (MCW)« less

Experimental verification of stopping-power prediction from single- and dual-energy computed tomography in biological tissues

NASA Astrophysics Data System (ADS)

Möhler, Christian; Russ, Tom; Wohlfahrt, Patrick; Elter, Alina; Runz, Armin; Richter, Christian; Greilich, Steffen

2018-01-01

An experimental setup for consecutive measurement of ion and x-ray absorption in tissue or other materials is introduced. With this setup using a 3D-printed sample container, the reference stopping-power ratio (SPR) of materials can be measured with an uncertainty of below 0.1%. A total of 65 porcine and bovine tissue samples were prepared for measurement, comprising five samples each of 13 tissue types representing about 80% of the total body mass (three different muscle and fatty tissues, liver, kidney, brain, heart, blood, lung and bone). Using a standard stoichiometric calibration for single-energy CT (SECT) as well as a state-of-the-art dual-energy CT (DECT) approach, SPR was predicted for all tissues and then compared to the measured reference. With the SECT approach, the SPRs of all tissues were predicted with a mean error of (-0.84  ±  0.12)% and a mean absolute error of (1.27  ±  0.12)%. In contrast, the DECT-based SPR predictions were overall consistent with the measured reference with a mean error of (-0.02  ±  0.15)% and a mean absolute error of (0.10  ±  0.15)%. Thus, in this study, the potential of DECT to decrease range uncertainty could be confirmed in biological tissue.

40 CFR 1068.95 - What materials does this part reference?

Code of Federal Regulations, 2011 CFR

2011-07-01

... material from the Society of Automotive Engineers that we have incorporated by reference. The first column... reference it. Anyone may purchase copies of these materials from the Society of Automotive Engineers, 400... Materials Document number and name Part 1068reference SAE J1930, Electrical/Electronic Systems Diagnostic...

40 CFR 1068.95 - What materials does this part reference?

Code of Federal Regulations, 2010 CFR

2010-07-01

... material from the Society of Automotive Engineers that we have incorporated by reference. The first column... reference it. Anyone may purchase copies of these materials from the Society of Automotive Engineers, 400... Materials Document number and name Part 1068reference SAE J1930, Electrical/Electronic Systems Diagnostic...

40 CFR 1042.910 - Reference materials.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Reference materials. 1042.910 Section... Other Reference Information § 1042.910 Reference materials. Documents listed in this section have been... information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov...

40 CFR 1042.910 - Reference materials.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Reference materials. 1042.910 Section... Other Reference Information § 1042.910 Reference materials. Documents listed in this section have been... information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov...

40 CFR 1043.100 - Reference materials.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Reference materials. 1043.100 Section... § 1043.100 Reference materials. Documents listed in this section have been incorporated by reference into... the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov...

Combinatorial synthesis of inorganic or composite materials

DOEpatents

Goldwasser, Isy; Ross, Debra A.; Schultz, Peter G.; Xiang, Xiao-Dong; Briceno, Gabriel; Sun, Xian-Dong; Wang, Kai-An

2010-08-03

Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials or, alternatively, allowing the components to interact to form at least two different materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, nonbiological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

An improved reference measurement procedure for triglycerides and total glycerides in human serum by isotope dilution gas chromatography-mass spectrometry.

PubMed

Chen, Yizhao; Liu, Qinde; Yong, Sharon; Teo, Hui Ling; Lee, Tong Kooi

2014-01-20

Triglycerides are widely tested in clinical laboratories using enzymatic methods for lipid profiling. As enzymatic methods can be affected by interferences from biological samples, this together with the non-specific nature of triglycerides measurement makes it necessary to verify the accuracy of the test results with a reference measurement procedure. Several such measurement procedures had been published. These procedures generally involved lengthy and laborious sample preparation steps. In this paper, an improved reference measurement procedure for triglycerides and total glycerides was reported which simplifies the sample preparation steps and greatly shortens the time taken. The procedure was based on isotope dilution gas chromatography-mass spectrometry (IDGC-MS)with tripalmitin as the calibration standard. Serum samples were first spiked with isotope-labeled tripalmitin. For the measurement of triglycerides, the serum samples were subjected to lipid extraction followed by separation of triglycerides from diglycerides and monoglycerides. Triglycerides were then hydrolyzed to glycerol, derivatized and injected into the GC–MS for quantification. For the measurement of total glycerides, the serum samples were hydrolyzed directly and derivatized before injection into the GC-MS for quantification. All measurement results showed good precision with CV <1%. A certified reference material (CRM) of lipids in frozen human serum was used to verify the accuracy of the measurement. The obtained values for both triglycerides and total glycerides were well within the certified ranges of the CRM, with deviation <0.4% from the certified values. The relative expanded uncertainties were also comparable with the uncertainties associated with the certified values of the CRM. The validated procedure was used in an External Quality Assessment (EQA) Program organized by our laboratory to establish the assigned values for triglycerides and total glycerides.

Dynamic-gravimetric preparation of metrologically traceable primary calibration standards for halogenated greenhouse gases

NASA Astrophysics Data System (ADS)

Guillevic, Myriam; Vollmer, Martin K.; Wyss, Simon A.; Leuenberger, Daiana; Ackermann, Andreas; Pascale, Céline; Niederhauser, Bernhard; Reimann, Stefan

2018-06-01

For many years, the comparability of measurements obtained with various instruments within a global-scale air quality monitoring network has been ensured by anchoring all results to a unique suite of reference gas mixtures, also called a primary calibration scale. Such suites of reference gas mixtures are usually prepared and then stored over decades in pressurised cylinders by a designated laboratory. For the halogenated gases which have been measured over the last 40 years, this anchoring method is highly relevant as measurement reproducibility is currently much better ( < 1 %, k = 2 or 95 % confidence interval) than the expanded uncertainty of a reference gas mixture (usually > 2 %). Meanwhile, newly emitted halogenated gases are already measured in the atmosphere at pmol mol-1 levels, while still lacking an established reference standard. For compounds prone to adsorption on material surfaces, it is difficult to evaluate mixture stability and thus variations in the molar fractions over time in cylinders at pmol mol-1 levels.To support atmospheric monitoring of halogenated gases, we create new primary calibration scales for SF6 (sulfur hexafluoride), HFC-125 (pentafluoroethane), HFO-1234yf (or HFC-1234yf, 2,3,3,3-tetrafluoroprop-1-ene), HCFC-132b (1,2-dichloro-1,1-difluoroethane) and CFC-13 (chlorotrifluoromethane). The preparation method, newly applied to halocarbons, is dynamic and gravimetric: it is based on the permeation principle followed by dynamic dilution and cryo-filling of the mixture in cylinders. The obtained METAS-2017 primary calibration scales are made of 11 cylinders containing these five substances at near-ambient and slightly varying molar fractions. Each prepared molar fraction is traceable to the realisation of SI units (International System of Units) and is assigned an uncertainty estimate following international guidelines (JCGM, 2008), ranging from 0.6 % for SF6 to 1.3 % (k = 2) for all other substances. The smallest uncertainty obtained for SF6 is mostly explained by the high substance purity level in the permeator and the low SF6 contamination of the matrix gas. The measured internal consistency of the suite ranges from 0.23 % for SF6 to 1.1 % for HFO-1234yf (k = 1). The expanded uncertainty after verification (i.e. measurement of the cylinders vs. each others) ranges from 1 to 2 % (k = 2).This work combines the advantages of SI-traceable reference gas mixture preparation with a calibration scale system for its use as anchor by a monitoring network. Such a combined system supports maximising compatibility within the network while linking all reference values to the SI and assigning carefully estimated uncertainties.For SF6, comparison of the METAS-2017 calibration scale with the scale prepared by SIO (Scripps Institution of Oceanography, SIO-05) shows excellent concordance, the ratio METAS-2017 / SIO-05 being 1.002. For HFC-125, the METAS-2017 calibration scale is measured as 7 % lower than SIO-14; for HFO-1234yf, it is 9 % lower than Empa-2013. No other scale for HCFC-132b was available for comparison. Finally, for CFC-13 the METAS-2017 primary calibration scale is 5 % higher than the interim calibration scale (Interim-98) that was in use within the Advanced Global Atmospheric Gases Experiment (AGAGE) network before adopting the scale established in the present work.

Nuclear reference materials to meet the changing needs of the global nuclear community

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

Martin, H.R.; Gradle, C.G.; Narayanan, U.I.

New Brunswick Laboratory (NBL) serves as the US Government`s Certifying Authority for nuclear reference materials and measurement calibration standards. In this role, NBL provides nuclear reference materials certified for chemical and/or isotopic compositions traceable to a nationally accepted, internationally compatible reference base. Emphasis is now changing as to the types of traceable nuclear reference materials needed as operations change within the Department of Energy (DOE) complex and at nuclear facilities around the world. Environmental and waste minimization issues, facilities and materials transitioning from processing to storage modes with corresponding changes in the types of measurements being performed, emphasis on requirementsmore » for characterization of waste materials, difficulties in transporting nuclear materials, and International factors, including International Atomic Energy Agency (IAEA) inspection of excess US nuclear materials, are all contributing influences. During these changing times, ft is critical that traceable reference materials be provided for calibration or validation of the performance of measurement systems. This paper will describe actions taken and planned to meet the changing reference material needs of the global nuclear community.« less

Substance and materiality? The archaeology of Talensi medicine shrines and medicinal practices.

PubMed

Insoll, Timothy

2011-08-01

Talensi materia medica is varied, encompassing plant, mineral, and animal substances. Healing, medicines, and medicinal practices and knowledge can be shrine-based and linked with ritual practices. This is explored utilising ethnographic data and from an archaeological perspective with reference to future possibilities for research both on Talensi medicine and, by implication, more generally through considering the archaeology of Talensi medicine preparation, use, storage, spread, and disposal. It is suggested that configuring the archaeology of medicine shrines and practices more broadly in terms of health would increase archaeological visibility and research potential.

Towards standardized testing methodologies for optical properties of components in concentrating solar thermal power plants

NASA Astrophysics Data System (ADS)

Sallaberry, Fabienne; Fernández-García, Aránzazu; Lüpfert, Eckhard; Morales, Angel; Vicente, Gema San; Sutter, Florian

2017-06-01

Precise knowledge of the optical properties of the components used in the solar field of concentrating solar thermal power plants is primordial to ensure their optimum power production. Those properties are measured and evaluated by different techniques and equipment, in laboratory conditions and/or in the field. Standards for such measurements and international consensus for the appropriate techniques are in preparation. The reference materials used as a standard for the calibration of the equipment are under discussion. This paper summarizes current testing methodologies and guidelines for the characterization of optical properties of solar mirrors and absorbers.

Substance and materiality? The archaeology of Talensi medicine shrines and medicinal practices

PubMed Central

Insoll, Timothy

2011-01-01

Talensi materia medica is varied, encompassing plant, mineral, and animal substances. Healing, medicines, and medicinal practices and knowledge can be shrine-based and linked with ritual practices. This is explored utilising ethnographic data and from an archaeological perspective with reference to future possibilities for research both on Talensi medicine and, by implication, more generally through considering the archaeology of Talensi medicine preparation, use, storage, spread, and disposal. It is suggested that configuring the archaeology of medicine shrines and practices more broadly in terms of health would increase archaeological visibility and research potential. PMID:21810036

NASA EPSCoR Nebraska Preparation Grant: Year 1

NASA Technical Reports Server (NTRS)

Bowen, Brent D.; Holmes, Bruce J.; Bartle, John R.; Gogos, George; Hinton, David W.; Lehrer, Henry R.; Moussavi, Massoum; Reed, B. J.; Schaaf, Michaela M.; Smith, Russell L.;

Analysis of Rare Earth Elements in Geologic Samples using Inductively Coupled Plasma Mass Spectrometry; US DOE Topical Report - DOE/NETL-2016/1794

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

Bank, Tracy L.; Roth, Elliot A.; Tinker, Phillip

2016-04-17

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used to measure the concentrations of rare earth elements (REE) in certified standard reference materials including shale and coal. The instrument used in this study is a Perkin Elmer Nexion 300D ICP-MS. The goal of the study is to identify sample preparation and operating conditions that optimized recovery of each element of concern. Additionally, the precision and accuracy of the technique are summarized and the drawbacks and limitations of the method are outlined.

A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis (by V. E. Buhrke, R. Jenkins, and D. K. Smith)

NASA Astrophysics Data System (ADS)

Rudman, Reuben

1999-06-01

Wiley-VCH: New York, 1998. xxiv + 333 pp. ISBN 0-471-19458-1. $79.95. I would have subtitled this book "All You Ever Wanted To Know about ...Sample Preparation". Although its principal thrust is geared towards the analytical chemist in an X-ray diffraction (XRD) or X-ray fluorescence (XRF) service laboratory, this text will be of use primarily as a reference source in all milieus dealing with undergraduate research projects and advanced laboratory courses in physical and analytical chemistry. It contains dozens of suggestions for preparing randomly oriented small samples of nearly anything. For example, rocks and minerals, soft organics and hard ceramics, radioactive and liquid materials, metals and oils are all treated. As the availability of XRD and XRF equipment has increased, so has the use of these techniques in the teaching schedule. Many undergraduate laboratory and research projects utilizing these methods have been described in the literature and are found in laboratory textbooks. Very often, especially with the increasingly common use of automated computer-controlled instrumentation, sample preparation has become the key experimental technique required for successful data collection. However, it is not always easy to prepare the statistically random distribution of small particles (crystallites) that is required by these methods. A multitude of techniques have been developed over the past 70 years, but many of them have been handed down by word of mouth or are scattered throughout the literature. This book represents an attempt to systematically describe the theory and practice of sample preparation. This excellent guide to the intricacies of sample preparation begins with a description of statistical sampling methods and the principles of grinding techniques. After a discussion of XRF specimen preparation, which includes pressing pellets, fusion methods, crucible selection and handling very small samples, detailed descriptions for handling rocks, minerals, cements, metals, oils, and vegetation [sic] are given. The preparation of XRD samples is described for various diffraction equipment geometries (utilizing both counter and film detectors), including specific information regarding the use of flat specimens and slurries, the use of internal standards, and the effects of crystallite size on the diffraction pattern. Methods for handling ceramics, clays, zeolites, air-sensitive samples, thin films, and plastics are described, along with the special handling requirements for materials to be studied by high-pressure, high-temperature, or low-temperature techniques. One whole chapter is devoted to the equipment used in specimen preparation, including grinders, pulverizers, presses, specimen holders, repair of platinumware, and sources of all types of special equipment. Did you ever want to know where to get a Plattner steel mortar or a micronizing mill or soft-glass capillary tubes with 0.01-mm wall thickness? It's all here in this monograph. The book ends with a good glossary of terms, a general bibliography in addition to the extensive list of references following each of its 9 chapters, and an index. It will be of help in many areas of spectroscopy and analytical chemistry, as well as in XRD and XRF analyses.

[Guide for the publication of written materials].

PubMed

Garcia Campos, M G

1987-01-01

Tips for writing and editing population education or other materials and descriptions of the process of printing a text and of available types of print media are provided. Written materials should be brief and concise, and should avoid bombarding the reader with too many figures or references. Ideas of others must always be acknowledged. Adjectives and metaphors should be used in moderation. The first person and obscure words should both be avoided. Acronyms and abbreviations should be defined at their 1st use. Ideas should be presented in a logical sequence. Illustrations and tables may facilitate comprehension, but only if they are clearly presented and printed. Materials should be adapted to their audiences. In a country with the cultural, racial, and social diversity of Peru, it is impossible to refer to a general audience. Population communication which wishes to influence people must be based on a clear knowledge of the level of information, habits, linguistic practices, and other traits of the intended audience. Once the audience has been characterized, the objectives of the publication should be clearly defined. The technical characteristics of the publication are then selected. The format should be a standard size so that all the available paper can be used. The number of pages is often determined by the funds available although ideally it should be decided in accordance with the information to be presented. The color, type of lettering and spacing, paper, number of copies to be printed, and frequency of appearance are influenced by budgetary considerations, but the letter size and spacing should be generous enough to allow easy reading. The layout, style, and sections of the work must then be determined. A bulletin for example could have an editorial, a central article, reportage, an in-depth interview, correspondence, book reviews, and other regular features. The contents should be carefully checked for accuracy and grammaticality, and each step of technical preparation and printing must be carefully monitored. Among available printed media, most require literate audiences and trained personnel to prepare them. Production costs are relatively high and good distribution networks are needed. Traditional media such as dances or festivals avoid some of these requirements but can only reach limited audiences.

78 FR 47319 - Fee Schedule for Reference Biological Standards and Biological Preparations

Federal Register 2010, 2011, 2012, 2013, 2014

2013-08-05

... DEPARTMENT OF HEALTH AND HUMAN SERVICES Centers for Disease Control and Prevention Fee Schedule for Reference Biological Standards and Biological Preparations AGENCY: Centers for Disease Control and Prevention (CDC), Department of Health and Human Services (HHS). ACTION: General notice. SUMMARY: The Centers...

JADOPPT: java based AutoDock preparing and processing tool.

PubMed

García-Pérez, Carlos; Peláez, Rafael; Therón, Roberto; Luis López-Pérez, José

2017-02-15

AutoDock is a very popular software package for docking and virtual screening. However, currently it is hard work to visualize more than one result from the virtual screening at a time. To overcome this limitation we have designed JADOPPT, a tool for automatically preparing and processing multiple ligand-protein docked poses obtained from AutoDock. It allows the simultaneous visual assessment and comparison of multiple poses through clustering methods. Moreover, it permits the representation of reference ligands with known binding modes, binding site residues, highly scoring regions for the ligand, and the calculated binding energy of the best ranked results. JADOPPT, supplementary material (Case Studies 1 and 2) and video tutorials are available at http://visualanalytics.land/cgarcia/JADOPPT.html. carlosgarcia@usal.es or pelaez@usal.es. Supplementary data are available at Bioinformatics online. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

High-precision determination of 18O/16O ratios of silver phosphate by EA-pyrolysis-IRMS continuous flow technique.

PubMed

Lécuyer, Christophe; Fourel, François; Martineau, François; Amiot, Romain; Bernard, Aurélien; Daux, Valérie; Escarguel, Gilles; Morrison, John

2007-01-01

A high-precision, and rapid on-line method for oxygen isotope analysis of silver phosphate is presented. The technique uses high-temperature elemental analyzer (EA)-pyrolysis interfaced in continuous flow (CF) mode to an isotopic ratio mass spectrometer (IRMS). Calibration curves were generated by synthesizing silver phosphate with a 13 per thousand spread in delta(18)O values. Calibration materials were obtained by reacting dissolved potassium dihydrogen phosphate (KH(2)PO(4)) with water samples of various oxygen isotope compositions at 373 K. Validity of the method was tested by comparing the on-line results with those obtained by classical off-line sample preparation and dual inlet isotope measurement. In addition, silver phosphate precipitates were prepared from a collection of biogenic apatites with known delta(18)O values ranging from 12.8 to 29.9 per thousand (V-SMOW). Reproducibility of +/- 0.2 per thousand was obtained by the EA-Py-CF-IRMS method for sample sizes in the range 400-500 microg. Both natural and synthetic samples are remarkably well correlated with conventional (18)O/(16)O determinations. Silver phosphate is a very stable material and easy to degas and, thus, could be considered as a good candidate to become a reference material for the determination of (18)O/(16)O ratios of phosphate by high-temperature pyrolysis. Copyright 2006 John Wiley & Sons, Ltd.

Expression and purification of a functional recombinant aspartate aminotransferase (AST) from Escherichia coli.

PubMed

Zou, Lihui; Zhao, Haijian; Wang, Daguang; Wang, Meng; Zhang, Chuanbao; Xiao, Fei

2014-07-01

Aspartate aminotransferase (AST; E.C. 2.6.1.1), a vitamin B6-dependent enzyme, preferentially promotes the mutual transformation of aspartate and α-ketoglutarate to oxaloacetate and glutamate. It plays a key role in amino acid metabolism and has been widely recommended as a biomarker of liver and heart damage. Our study aimed to evaluate the extensive preparation of AST and its application in quality control in clinical laboratories. We describe a scheme to express and purify the 6His-AST fusion protein. An optimized sequence coding AST was synthesized and transformed into Escherichia coli BL21 (DE3) strain for protein expression. Ideally, the fusion protein has a volumetric productivity achieving 900 mg/l cultures. After affinity chromatography, the enzyme activity of purified AST reached 150,000 U/L. Commutability assessment between the engineered AST and standard AST from Roche suggested that the engineered AST was the better candidate for the reference material. Moreover, the AST showed high stability during long-term storage at -20ºC. In conclusion, the highly soluble 6His-tagged AST can become a convenient tool for supplying a much better and cheaper standard or reference material for the clinical laboratory.

Graphene Oxide from Carbon Rod Waste

NASA Astrophysics Data System (ADS)

Rahmawati, F.; Prasasti, B. L. W.; Mudjijono, M.

2018-03-01

Carbon rods extracted from Zn-C primary battery waste was used as raw material for graphene oxide (GO) synthesis. The synthesis used a modified Hummers method by providing potassium permanganate-sulfuric acid as the oxidizing agent. XRD analysis confirms a significant change between the graphite waste pattern and the produced graphene oxide pattern. A major peak at 2θ 27 ° which present in the graphite waste pattern is disappeared after it converts to the product, as well as a broad peak under 25 ° referring the presence of amorphous carbon. A broad peak at low angle of 12.02 ° dominantly present in the prepared GO pattern as a characteristic peak of GO. Meanwhile, some small peaks at 2θ of 17.76 °, 28.58 °, and 37.28 ° confirming the presence of manganese oxide which was used as oxidizing agent. A sharp peak at 1700 – 1500 cm-1 in the FT-IR spectrum indicates the presence of –C=O group, and at 1600 cm-1 refers to –C=C group. It confirms that this research has produced the targeted GO. Even though, the purity is need to be enhanced by removing the rest of oxidizing agent that still exist in the material.

Determination of As, Cd, Hg and Pb in herbs using slurry sampling electrothermal vaporisation inductively coupled plasma mass spectrometry.

PubMed

Lin, Mei-Ling; Jiang, Shiuh-Jen

2013-12-01

Inductively coupled plasma mass spectrometry coupled with ultrasonic slurry sampling electrothermal vaporisation (USS-ETV-ICP-MS) has been applied to determine As, Cd, Hg and Pb in 0.5% m/v slurries of several herb samples. 1% m/v 8-Hydroxyquinoline was used as the modifier to enhance the ion signals. The influences of instrument operating conditions, slurry preparation and interferences on the ion signals were reported. This method has been applied to the determination of As, Cd, Hg and Pb in NIST SRM 1547 peach leaves and SRM 1573a tomato leaves reference materials and three herb samples purchased from the local market and ground to 150 μm. The analysis results of the standard reference materials agreed with the certified values which are at sub μg g(-1) levels. Precision between sample replicates was better than 4% for all the determinations. The method detection limits estimated from standard addition curves were about 0.3, 0.1, 0.1 and 0.2 ng g(-1) for As, Cd, Hg and Pb, respectively, in original herb samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

The importance of reference materials in doping-control analysis.

PubMed

Mackay, Lindsey G; Kazlauskas, Rymantas

2011-08-01

Currently a large range of pure substance reference materials are available for calibration of doping-control methods. These materials enable traceability to the International System of Units (SI) for the results generated by World Anti-Doping Agency (WADA)-accredited laboratories. Only a small number of prohibited substances have threshold limits for which quantification is highly important. For these analytes only the highest quality reference materials that are available should be used. Many prohibited substances have no threshold limits and reference materials provide essential identity confirmation. For these reference materials the correct identity is critical and the methods used to assess identity in these cases should be critically evaluated. There is still a lack of certified matrix reference materials to support many aspects of doping analysis. However, in key areas a range of urine matrix materials have been produced for substances with threshold limits, for example 19-norandrosterone and testosterone/epitestosterone (T/E) ratio. These matrix-certified reference materials (CRMs) are an excellent independent means of checking method recovery and bias and will typically be used in method validation and then regularly as quality-control checks. They can be particularly important in the analysis of samples close to threshold limits, in which measurement accuracy becomes critical. Some reference materials for isotope ratio mass spectrometry (IRMS) analysis are available and a matrix material certified for steroid delta values is currently under production. In other new areas, for example the Athlete Biological Passport, peptide hormone testing, designer steroids, and gene doping, reference material needs still need to be thoroughly assessed and prioritised.

78 FR 57293 - Distribution of Reference Biological Standards and Biological Preparations

Federal Register 2010, 2011, 2012, 2013, 2014

2013-09-18

... DEPARTMENT OF HEALTH AND HUMAN SERVICES 42 CFR Part 7 [Docket No. CDC-2013-0013] RIN 0920-AA52 Distribution of Reference Biological Standards and Biological Preparations AGENCY: Centers for Disease Control and Prevention (HHS/CDC), Department of Health and Human Services (HHS). ACTION: Confirmation of...

Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

PubMed

Muller, Edson I; Souza, Juliana P; Muller, Cristiano C; Muller, Aline L H; Mello, Paola A; Bizzi, Cezar A

2016-08-15

In this work a green digestion method which only used H2O2 as an oxidant and high temperature and pressure in the single reaction chamber system (SRC-UltraWave™) was applied for subsequent elemental determination by inductively coupled plasma-based techniques. Milk powder was chosen to demonstrate the feasibility and advantages of the proposed method. Samples masses up to 500mg were efficiently digested, and the determination of Ca, Fe, K, Mg and Na was performed by inductively coupled plasma optical emission spectrometry (ICP-OES), while trace elements (B, Ba, Cd, Cu, Mn, Mo, Pb, Sr and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). Residual carbon (RC) lower than 918mgL(-1) of C was obtained for digests which contributed to minimizing interferences in determination by ICP-OES and ICP-MS. Accuracy was evaluated using certified reference materials NIST 1549 (non-fat milk powder certified reference material) and NIST 8435 (whole milk powder reference material). The results obtained by the proposed method were in agreement with the certified reference values (t-test, 95% confidence level). In addition, no significant difference was observed between results obtained by the proposed method and conventional wet digestion using concentrated HNO3. As digestion was performed without using any kind of acid, the characteristics of final digests were in agreement with green chemistry principles when compared to digests obtained using conventional wet digestion method with concentrated HNO3. Additionally, H2O2 digests were more suitable for subsequent analysis by ICP-based techniques due to of water being the main product of organic matrix oxidation. The proposed method was suitable for quality control of major components and trace elements present in milk powder in consonance with green sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of mass measurement equipment using an electronic mass-comparator for gravimetric preparation of reference gas mixtures

NASA Astrophysics Data System (ADS)

Matsumoto, Nobuhiro; Watanabe, Takuro; Maruyama, Masaaki; Horimoto, Yoshiyuki; Maeda, Tsuneaki; Kato, Kenji

2004-06-01

The gravimetric method is the most popular method for preparing reference gas mixtures with high accuracy. We have designed and manufactured novel mass measurement equipment for gravimetric preparation of reference gas mixtures. This equipment consists of an electronic mass-comparator with a maximum capacity of 15 kg and readability of 1 mg and an automatic cylinder exchanger. The structure of this equipment is simpler and the cost is much lower than a conventional mechanical knife-edge type large balance used for gravimetric preparation of primary gas mixtures in Japan. This cylinder exchanger can mount two cylinders alternatively on the weighing pan of the comparator. In this study, the performance of the equipment has been evaluated. At first, the linearity and repeatability of the mass measurement were evaluated using standard mass pieces. Then, binary gas mixtures of propane and nitrogen were prepared and compared with those prepared with the conventional knife-edge type balance. The comparison resulted in good consistency at the compatibility criterion described in ISO6143:2001.

Environmentally-Friendly Dense and Porous Geopolymers Using Fly Ash and Rice Husk Ash as Raw Materials

PubMed Central

Ziegler, Daniele; Formia, Alessandra; Tulliani, Jean-Marc; Palmero, Paola

2016-01-01

This paper assesses the feasibility of two industrial wastes, fly ash (FA) and rice husk ash (RHA), as raw materials for the production of geopolymeric pastes. Three typologies of samples were thus produced: (i) halloysite activated with potassium hydroxide and nanosilica, used as the reference sample (HL-S); (ii) halloysite activated with rice husk ash dissolved into KOH solution (HL-R); (iii) FA activated with the alkaline solution realized with the rice husk ash (FA-R). Dense and porous samples were produced and characterized in terms of mechanical properties and environmental impact. The flexural and compressive strength of HL-R reached about 9 and 43 MPa, respectively. On the contrary, the compressive strength of FA-R is significantly lower than the HL-R one, in spite of a comparable flexural strength being reached. However, when porous samples are concerned, FA-R shows comparable or even higher strength than HL-R. Thus, the current results show that RHA is a valuable alternative to silica nanopowder to prepare the activator solution, to be used either with calcined clay and fly ash feedstock materials. Finally, a preliminary evaluation of the global warming potential (GWP) was performed for the three investigated formulations. With the mix containing FA and RHA-based silica solution, a reduction of about 90% of GWP was achieved with respect to the values obtained for the reference formulation. PMID:28773587

Preparation of electromechanically active silicone composites and some evaluations of their suitability for biomedical applications.

PubMed

Iacob, Mihail; Bele, Adrian; Patras, Xenia; Pasca, Sorin; Butnaru, Maria; Alexandru, Mihaela; Ovezea, Dragos; Cazacu, Maria

2014-10-01

Some films based on electromechanically active polymer composites have been prepared. Polydimethylsiloxane-α,ω-diols (PDMSs) having different molecular masses (Mv=60 700 and Mv=44 200) were used as matrix in which two different active fillers were incorporated: titanium dioxide in situ generated from its titanium isopropoxide precursor and silica particles functionalized with polar aminopropyl groups on surface. A reference sample based on simple crosslinked PDMS was also prepared. The composites processed as films were investigated to evaluate their ability to act as efficient electromechanical actuators for potential biomedical application. Thus, the surface morphology of interest for electrodes compliance was analysed by atomic force microscopy. Mechanical and dielectric characteristics were evaluated by tensile tests and dielectric spectroscopy, respectively. Electromechanical actuation responses were measured by interferometry. The biocompatibility of the obtained materials has been verified through tests in vitro and, for valuable films, in vivo. The experimental, clinical and anatomopathological evaluation of the in vivo tested samples did not reveal significant pathological modifications. Copyright © 2014 Elsevier B.V. All rights reserved.

Extraction and derivatization of polar herbicides for GC-MS analyses.

PubMed

Ranz, Andreas; Maier, Eveline; Motter, Herbert; Lankmayr, Ernst

2008-09-01

A sample preparation procedure including a simultaneous microwave-assisted (MA) extraction and derivatization for the determination of chlorophenoxy acids in soil samples is presented. For a selective and sensitive measurement, an analytical technique such as GC coupled with MS needs to be adopted. For GC analyses, chlorophenoxy acids have to be converted into more volatile and thermally stable derivatives. Derivatization by means of microwave radiation offers new alternatives in terms of shorter derivatization time and reduces susceptibility for the formation of artefacts. Extraction and derivatization into methyl esters (ME) were performed with sulphuric acid and methanol. Due to the novelty of the simultaneous extraction and derivatization assisted by means of microwave radiation, a careful investigation and optimization of influential reaction parameters was necessary. It could be shown that the combination of sulphuric acid and methanol provides a fast sample preparation including an efficient clean up procedure. The data obtained by the described method are in good agreement with those published for the reference material. Finally, compared to conventional heating and also to the standard procedure of the EPA, the sample preparation time could be considerably shortened.

Publications of the Fossil Energy Advanced Research and Technology Development Materials Program: April 1, 1993-March 31, 1995

NASA Astrophysics Data System (ADS)

Carlson, Paul T.

1995-04-01

The objective of the Fossil Energy Advanced Research and Technology Development (AR and TD) Materials Program is to conduct research and development on materials for fossil energy applications, with a focus on the longer-term needs for materials with general applicability to the various fossil fuel technologies. The Program includes research aimed at a better understanding of materials behavior in fossil energy environments and on the development of new materials capable of substantial improvement in plant operations and reliability. The scope of the Program addresses materials requirements for all fossil energy systems, including materials for coal preparation, coal liquefaction, coal gasification, heat engines and heat recovery, combustion systems, and fuel cells. Work on the Program is conducted at national and government laboratories, universities, and industrial research facilities. This bibliography covers the period of April 1, 1993, through March 31, 1995, and is a supplement to previous bibliographies in this series. It is the intent of this series of bibliographies to list only those publications that can be conveniently obtained by a researcher through relatively normal channels. The publications listed in this document have been limited to topical reports, open literature publications in referred journals, full-length papers in published proceedings of conferences, full-length papers in unreferred journals, and books and book articles.

Studies on wettability of polypropylene/methyl-silicone composite film and polypropylene monolithic material.

PubMed

Hou, Weixin; Mu, Bo; Wang, Qihua

2008-11-01

A polypropylene/methyl-silicone superhydrophobic surface was prepared using a simple casting method. Varying the ratio of polypropylene and methyl-silicone results in different surface microstructure. The wetting behavior of the as-prepared surface was investigated. A polypropylene monolithic material was also prepared. Its superhydrophobicity still retains when the material was cut or abraded. The as-prepared material can also be used to separate some organic solvents from water.

Mineral oil certified reference materials for the determination of polychlorinated biphenyls from the National Metrology Institute of Japan (NMIJ)

PubMed Central

Aoyagi, Yoshie; Matsuo, Mayumi; Ishikawa, Keiichiro; Hanari, Nobuyasu; Otsuka, Satoko; Tsuda, Yoko; Yarita, Takashi

2008-01-01

Four mineral oil certified reference materials (CRMs), NMIJ CRM 7902-a, CRM 7903-a, CRM 7904-a, and CRM 7905-a, have been issued by the National Metrology Institute of Japan, which is part of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST), for the determination of polychlorinated biphenyls (PCBs). The raw materials for the CRMs were an insulation oil (CRM 7902-a and CRM 7903-a) and a fuel oil (CRM7904-a and CRM 7905-a). A solution of PCB3, PCB8, and technical PCB products, comprising four types of Kaneclor, was added to the oil matrices. The total PCB concentrations in the PCB-fortified oils (CRM 7902-a and CRM 7904-a) are approximately 6 mg kg−1. In addition, the mineral oils which were not fortified with PCBs were also distributed as CRMs (CRM 7903-a and CRM 7905-a). Characterization of these CRMs was conducted by the NMIJ/AIST, where the mineral oils and the PCB solution were analyzed using multiple analytical methods such as dimethylsulfoxide extraction, normal-phase liquid chromatography, gel permeation chromatography, reversed-phase liquid chromatography, and chromatography using sulfoxide-bonded silica; and/or various capillary columns for gas chromatography, and two ionization modes for mass spectrometry. The target compounds in the mineral oils and those in the PCB solution were determined by one of the primary methods of measurement, isotope dilution–mass spectrometry (ID-MS). Certified values have been provided for 11 PCB congeners (PCB3, 8, 28, 52, 101, 118, 138, 153, 180, 194, and 206) in the CRMs. These CRMs have information values for PCB homologue concentrations determined by using a Japanese official method for determination of PCBs in wastes and densities determined with an oscillational density meter. Because oil samples having arbitrary PCB concentrations between respective property values of the PCB-fortified and nonfortified CRMs can be prepared by gravimetric mixing of the CRM pairs, these CRMs can be used for validation of PCB analyses using various instruments which have different sensitivities. Figure Preparation and certification processes of the mineral oil CRMs (example shown is polychlorinated biphenyls in insulation oil, high/low concentrations) Electronic supplementary material The online version of this article (doi:10.1007/s00216-008-2010-3) contains supplementary material, which is available to authorized users. PMID:18415091

Deriving proper measurement uncertainty from Internal Quality Control data: An impossible mission?

PubMed

Ceriotti, Ferruccio

2018-03-30

Measurement uncertainty (MU) is a "non-negative parameter characterizing the dispersion of the quantity values being attributed to a measurand, based on the information used". In the clinical laboratory the most convenient way to calculate MU is the "top down" approach based on the use of Internal Quality Control data. As indicated in the definition, MU depends on the information used for its calculation and so different estimates of MU can be obtained. The most problematic aspect is how to deal with bias. In fact bias is difficult to detect and quantify and it should be corrected including only the uncertainty derived from this correction. Several approaches to calculate MU starting from Internal Quality Control data are presented. The minimum requirement is to use only the intermediate precision data, provided to include 6 months of results obtained with a commutable quality control material at a concentration close to the clinical decision limit. This approach is the minimal requirement and it is convenient for all those measurands that are especially used for monitoring or where a reference measurement system does not exist and so a reference for calculating the bias is lacking. Other formulas including the uncertainty of the value of the calibrator, including the bias from a commutable certified reference material or from a material specifically prepared for trueness verification, including the bias derived from External Quality Assessment schemes or from historical mean of the laboratory are presented and commented. MU is an important parameter, but a single, agreed upon way to calculate it in a clinical laboratory is not yet available. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Determination of δ18O and δ15N in Nitrate

USGS Publications Warehouse

Revesz, K.; Böhlke, J.K.; Yoshinari, T.

1997-01-01

The analyses of both O and N isotopic compositions of nitrate have many potential applications in studies of nitrate sources and reactions in hydrology, oceanography, and atmospheric chemistry, but simple and precise methods for these analyses have yet to be developed. Testing of a new method involving reaction of potassium nitrate with catalyzed graphite (C + Pd + Au) at 520 °C resulted in quantitative recovery of N and O from nitrate as free CO2, K2CO3, and N2. The δ18O values of nitrate reference materials were obtained by analyzing both the CO2 and K2CO3 from catalyzed graphite combustion. Provisional values of δ18OVSMOW for the internationally distributed KNO3 reference materials IAEA-N3 and USGS-32 were both equal to +22.7 ± 0.5‰. Because the fraction of free CO2 and the isotopic fractionation factor between CO2 and K2CO3 were constant in the combustion products, the δ18O value of KNO3 could be calculated from measurements of the δ18O of free CO2. Thus, δ18OKNO3 = aδ18Ofree CO2 − b, where a and b were equal to 0.9967 and 3.3, respectively, for the specific conditions of the experiments. The catalyzed graphite combustion method can be used to determine δ18O of KNO3 from measurements of δ18O of free CO2 with reproducibility on the order of ±0.2‰ or better if local reference materials are prepared and analyzed with the samples. Reproducibility of δ15N was ±0.1‰ after trace amounts of CO were removed.

Distortion of genetically modified organism quantification in processed foods: influence of particle size compositions and heat-induced DNA degradation.

PubMed

Moreano, Francisco; Busch, Ulrich; Engel, Karl-Heinz

2005-12-28

Milling fractions from conventional and transgenic corn were prepared at laboratory scale and used to study the influence of sample composition and heat-induced DNA degradation on the relative quantification of genetically modified organisms (GMO) in food products. Particle size distributions of the obtained fractions (coarse grits, regular grits, meal, and flour) were characterized using a laser diffraction system. The application of two DNA isolation protocols revealed a strong correlation between the degree of comminution of the milling fractions and the DNA yield in the extracts. Mixtures of milling fractions from conventional and transgenic material (1%) were prepared and analyzed via real-time polymerase chain reaction. Accurate quantification of the adjusted GMO content was only possible in mixtures containing conventional and transgenic material in the form of analogous milling fractions, whereas mixtures of fractions exhibiting different particle size distributions delivered significantly over- and underestimated GMO contents depending on their compositions. The process of heat-induced nucleic acid degradation was followed by applying two established quantitative assays showing differences between the lengths of the recombinant and reference target sequences (A, deltal(A) = -25 bp; B, deltal(B) = +16 bp; values related to the amplicon length of the reference gene). Data obtained by the application of method A resulted in underestimated recoveries of GMO contents in the samples of heat-treated products, reflecting the favored degradation of the longer target sequence used for the detection of the transgene. In contrast, data yielded by the application of method B resulted in increasingly overestimated recoveries of GMO contents. The results show how commonly used food technological processes may lead to distortions in the results of quantitative GMO analyses.

Steroid isotopic standards for gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS).

PubMed

Zhang, Ying; Tobias, Herbert J; Brenna, J Thomas

2009-03-01

Carbon isotope ratio (CIR) analysis of urinary steroids using gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS) is a recognized test to detect illicit doping with synthetic testosterone. There are currently no universally used steroid isotopic standards (SIS). We adapted a protocol to prepare isotopically uniform steroids for use as a calibrant in GCC-IRMS that can be analyzed under the same conditions as used for steroids extracted from urine. Two separate SIS containing a mixture of steroids were created and coded CU/USADA 33-1 and CU/USADA 34-1, containing acetates and native steroids, respectively. CU/USADA 33-1 contains 5alpha-androstan-3beta-ol acetate (5alpha-A-AC), 5alpha-androstan-3alpha-ol-17-one acetate (androsterone acetate, A-AC), 5beta-androstan-3alpha-ol-11, 17-dione acetate (11-ketoetiocholanolone acetate, 11k-AC) and 5alpha-cholestane (Cne). CU/USADA 34-1 contains 5beta-androstan-3alpha-ol-17-one (etiocholanolone, E), 5alpha-androstan-3alpha-ol-17-one (androsterone, A), and 5beta-pregnane-3alpha, 20alpha-diol (5betaP). Each mixture was prepared and dispensed into a set of about 100 ampoules using a protocol carefully designed to minimize isotopic fractionation and contamination. A natural gas reference material, NIST RM 8559, traceable to the international standard Vienna PeeDee Belemnite (VPDB) was used to calibrate the SIS. Absolute delta(13)C(VPDB) and Deltadelta(13)C(VPDB) values from randomly selected ampoules from both SIS indicate uniformity of steroid isotopic composition within measurement reproducibility, SD(delta(13)C)<0.2 per thousand. This procedure for creation of isotopic steroid mixtures results in consistent standards with isotope ratios traceable to the relevant international reference material.

Shrinkage stress compensation in composite-restored teeth: relaxation or hygroscopic expansion?

PubMed

Meriwether, Laurel A; Blen, Bernard J; Benson, Jarred H; Hatch, Robert H; Tantbirojn, Daranee; Versluis, Antheunis

2013-05-01

Polymerization of composite restorations causes shrinkage, which deforms and thus stresses restored teeth. This shrinkage deformation, however, has been shown to decrease over time. The objective was to investigate whether this reduction was caused by hygroscopic expansion or stress relaxation of the composite/tooth complex. Extracted molars were mounted in rigid stainless steel rings with four spherical reference areas. Twelve molars were prepared with large mesioocclusodistal slots, etched, bonded, and restored with a composite material (Filtek Supreme, 3M ESPE) in two horizontal layers. Ten intact molars were the controls. The teeth were stored either in deionized water or silicone oil. They were scanned after preparation (baseline), restoration (0-week), and after 1, 2, and 4 weeks storage. Scanned tooth surfaces were aligned with the baseline using the unchanged reference areas. Cuspal flexure was calculated from lingual and buccal surface deformation. To verify that the restorations had remained bonded, dye penetration at the interfaces was assessed using basic fuchsin dye. Statistical assessment was done by ANOVA followed by Student-Newman-Keuls post hoc test (p=0.05). Substantial cuspal contraction was found for restored teeth after the composite was cured (13-14 μm cuspal flexure). After 4 weeks cuspal contraction decreased significantly for restored teeth stored in water (7.3 ± 3.2) but not for those stored in silicone oil (11.4 ± 5.0). Dye penetration of the occlusal interface was minimal in both groups (106 ± 87 and 21 ± 28 μm in water and silicone oil, respectively). The results suggest that hygroscopic expansion was the main mechanism for shrinkage stress compensation. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

PubMed

Krawczyk-Coda, Magdalena; Stanisz, Ewa

2017-11-01

This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

Establishment of the 2nd Korean national biological reference standard for blood coagulation factor VIII:C concentrate.

PubMed

Lee, Naery; Seo, Ji Suk; Kim, Jae Ok; Ban, Sang Ja

2017-05-01

Since the 1st Korean national biological reference standard for factor (F)VIII concentrate, established in 2001, has shown declining potency, we conducted this study to replace this standard with a 2nd Korean national biological reference standard for blood coagulation FVIII concentrate. The candidate materials for the 2nd standard were prepared in 8000 vials with 10 IU/ml of target potency, according to the approved manufacturing process of blood coagulation Factor VIII:C Monoclonal Antibody-purified, Freeze-dried Human Blood Coagulation Factor VIII:C. Potency was evaluated by one-stage clotting and chromogenic methods and the stability was confirmed to meet the specifications during a period of 73 months. Since the potencies obtained by the two methods differed significantly (P < 0.015), the values were determined separately according to the geometric means (8.9 and 7.4 IU/vial, respectively). The geometric coefficients of interlaboratory variability were 3.4% and 7.6% by the one-stage clotting and chromogenic assays, respectively. Copyright © 2017 International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

Chapter 23: International Standard reagents for harmonization of HPV serology and DNA assays--an update.

PubMed

Pagliusi, Sonia R; Dillner, Joakim; Pawlita, Michael; Quint, Wim G V; Wheeler, Cosette M; Ferguson, M

2006-08-31

International reference materials such as International Standard reagents facilitate quality assurance of essential biopharmaceutical products and related in vitro diagnostic tests. Standardization of antibody and DNA measurements and harmonization of laboratory procedures are key to the success of cancer prevention strategies through screening methods as well as for development and implementation of vaccination against the human papillomavirus (HPV). The WHO supported the preparation and initial analysis of a panel of candidate serological and DNA reference reagents aimed at facilitating inter-laboratory comparisons and detection of HPV worldwide. Two international collaborative studies assessed the performance of various HPV antibody and HPV-DNA detection assays and examined the feasibility of generating HPV antibody and DNA standard reagents. These studies showed that improvement in performance and comparability of assays is urgently needed and that the use of the same International Standard reference reagent could significantly improve performance and comparability. It is hoped that the establishment of International Units and International Standards for HPV antibody and DNA analysis will be pursued with high priority.

Iodine Standard Materials: Preparation and Inter-Laboratory Comparisons

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

D D Jenson; M L Adamic; J E Olson

The Idaho National Laboratory is preparing to enter the community of AMS practioners who analyze for 129Iodine. We expect to take delivery of a 0.5 MV compact accelerator mass spectrometry system, built by NEC, in the early summer of 2014. The primary mission for this instrument is iodine; it is designed to analyze iodine in the +3 charge state. As part of the acceptance testing for this instrument, both at NEC and on-site in our laboratory, some sort of standard or reference material is needed to verify performance. Appropriate standard materials are not readily available in the commercial marketplace. Smallmore » quantities can sometimes be acquired from other laboratories already engaged in iodine analyses. In the longer-term, meaningful quantities of standard materials are needed for routine use in analyses, and for quality control functions1. We have prepared some standard materials, starting with elemental Woodward iodine and NIST SRM 3231 [Iodine-129 Isotopic Standard (high level)] 10-6 solution. The goal was to make mixtures at the 5x10-10, 5x10-11, 5x10-12 ratio levels, along with some unmodified Woodward, in the chemical form of silver iodide. Approximately twenty grams of each of these mixtures were prepared. The elemental Woodward iodine was dissolved in chloroform, then reduced to iodide using sodium bisulfite in water. At this point the NIST spike material was added, in the form of sodium iodide. The mixed iodides were oxidized back to iodine in chloroform using hydrogen peroxide. This oxidation step was essential for isotopic equilibration of the 127 and 129 atoms. The iodine was reduced to iodide using sodium bisulfite as before. Excess sulfites and sulfates were precipitated with barium nitrate. After decanting, silver nitrate was used to precipitate the desired silver iodide. Once the silver iodide was produced, the material was kept in darkness as much as possible to minimize photo-oxidation. The various mixtures were synthesized independently of each other; there were no serial dilutions involved. Aliquots of these four materials have been submitted to five established AMS laboratories where iodine analyses are routinely performed: ETH (Zurich), CNA (Seville), PRIME (Purdue), LLNL (California), and Isotrace (Toronto.) Results from four of these laboratories have been received; in general they indicate that the desired 129/127 ratios have been achieved. We will discuss the results of this informal round-robin exercise. If the installation of the instrument in Idaho goes well, we may have some very preliminary results from the new system. An integral part of data reporting is the approach to data reduction. Accordingly, there will also be some discussion of various philosophies of data handling in regard to the use of standards to adjust data, and background subtraction.« less

Determination of the rare-earth elements in geological materials by inductively coupled plasma mass spectrometry

USGS Publications Warehouse

Lichte, F.E.; Meier, A.L.; Crock, J.G.

1987-01-01

A method of analysis of geological materials for the determination of the rare-earth elements using the Inductively coupled plasma mass spectrometric technique (ICP-MS) has been developed. Instrumental parameters and factors affecting analytical results have been first studied and then optimized. Samples are analyzed directly following an acid digestion, without the need for separation or preconcentration with limits of detection of 2-11 ng/g, precision of ?? 2.5% relative standard deviation, and accuracy comparable to inductively coupled plasma emission spectrometry and instrumental neutron activation analysis. A commercially available ICP-MS instrument is used with modifications to the sample introduction system, torch, and sampler orifice to reduce the effects of high salt content of sample solutions prepared from geologic materials. Corrections for isobaric interferences from oxide ions and other diatomic and triatomic ions are made mathematically. Special internal standard procedures are used to compensate for drift in metahmetal oxide ratios and sensitivity. Reference standard values are used to verify the accuracy and utility of the method.

Neutron resonance spectroscopy for the characterization of materials and objects

NASA Astrophysics Data System (ADS)

Schillebeeckx, P.; Borella, A.; Emiliani, F.; Gorini, G.; Kockelmann, W.; Kopecky, S.; Lampoudis, C.; Moxon, M.; Perelli Cippo, E.; Postma, H.; Rhodes, N. J.; Schooneveld, E. M.; Van Beveren, C.

2012-03-01

The resonance structure in neutron induced reaction cross sections can be used to determine the elemental compositions of materials or objects. The occurrence of resonances is the basis of neutron resonance capture analysis (NRCA) and neutron resonance transmission analysis (NRTA). NRCA and NRTA are fully non-destructive methods to determine the bulk elemental composition without the need of any sample preparation and resulting in a negligible residual activity. They have been applied to determine the elemental composition of archaeological objects and to characterize reference materials used for cross section measurements. For imaging applications a position sensitive neutron detector has been developed within the ANCIENT CHARM project. The detector is based on a 10 × 10 array of 6Li-glass scintillators mounted on a pitch of 2.5 mm, resulting in a 25 × 25 mm2 active area. The detector has been tested at the time-of-flight facility GELINA and used at the ISIS spallation source to study cultural heritage objects.

WHO Expert Committee on Specifications for Pharmaceutical Preparations.

PubMed

2005-01-01

This report presents the recommendations of an international group of experts convened by the World Health Organization to consider matters concerning the quality assurance of pharmaceuticals and specifications for drug substances and dosage forms. Of particular relevance to drug regulatory authorities and pharmaceutical manufacturers, this report discusses the monographs on antiretrovirals proposed for inclusion in The International Pharmacopoeia and specifications for radiopharmaceuticals, quality specifications for antituberculosis drugs and the revision of the monograph on artemisinin derivatives, as well as quality control of reference materials, good manufacturing practices (GMP), inspection, distribution and trade and other aspects of quality assurance of pharmaceuticals, and regulatory issues. The report is complemented by a number of annexes, including an amendment to good manufacturing practices: main principles regarding the requirement for the sampling of starting materials, guidelines on good manufacturing practices regarding water for pharmaceutical use, guidelines on the sampling of pharmaceutical products and related materials and draft guidelines for registration of fixed-dose combination medicinal products.

Nanocrystalline hydroxyapatite enriched in selenite and manganese ions: physicochemical and antibacterial properties

NASA Astrophysics Data System (ADS)

Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

2015-07-01

In this work, we used the co-precipitation method to synthesize hydroxyapatite (Mn-SeO3-HA) containing both selenium IV (approximately 3.60 wt.%) and manganese II (approximately 0.29 wt.%). Pure hydroxyapatite (HA), hydroxyapatite-containing manganese (II) ions (Mn-HA), and hydroxyapatite-containing selenite ions alone (SeO3-HA), prepared with the same method, were used as reference materials. The structures and physicochemical properties of all the obtained samples were investigated. PXRD studies showed that the obtained materials were homogeneous and consisted of apatite phase. Introducing selenites into the hydroxyapatite crystals considerably affects the size and degree of ordering. Experiments with transmission electron microscopy (TEM) showed that Mn-SeO3-HA crystals are very small, needle-like, and tend to form agglomerates. Fourier transform infrared spectroscopy (FT-IR) and solid-state nuclear magnetic resonance (ssNMR) were used to analyze the structure of the obtained material. Preliminary microbiological tests showed that the material demonstrated antibacterial activity against Staphylococcus aureus, yet such properties were not confirmed regarding Escherichia coli. PACS codes: 61, 76, 81

Sol-Gel Derived Active Material for Yb Thin-Disk Lasers

PubMed Central

Almeida, Rui M.; Ribeiro, Tiago

2017-01-01

A ytterbium doped active material for thin-disk laser was developed based on aluminosilicate and phosphosilicate glass matrices containing up to 30 mol% YbO1.5. Thick films and bulk samples were prepared by sol-gel processing. The structural nature of the base material was assessed by X-ray diffraction and Raman spectroscopy and the film morphology was evidenced by scanning electron microscopy. The photoluminescence (PL) properties of different compositions, including emission spectra and lifetimes, were also studied. Er3+ was used as an internal reference to compare the intensities of the Yb3+ PL peaks at ~ 1020 nm. The Yb3+ PL lifetimes were found to vary between 1.0 and 0.5 ms when the Yb concentration increased from 3 to 30 mol%. Based on a figure of merit, the best active material selected was the aluminosilicate glass composition 71 SiO2-14 AlO1.5-15 YbO1.5 (in mol%). An active disk, ~ 36 μm thick, consisting of a Bragg mirror, an aluminosilicate layer doped with 15 mol% Yb and an anti-reflective coating, was fabricated. PMID:28869488

Tribological Performance of Ni3Al Matrix Self-Lubricating Composites Containing Multilayer Graphene Prepared by Additive Manufacturing

NASA Astrophysics Data System (ADS)

Yan, Zhao; Shi, Xiaoliang; Huang, Yuchun; Deng, Xiaobin; Liu, Xiyao; Yang, Kang

2018-01-01

In order to improve tribological performance of Ni3Al-based alloy, Ni3Al matrix composites containing 1.5 wt.% multilayer graphene (MLG) are prepared through additive manufacturing (AM) and spark plasma sintering (SPS), which are denoted as NMAM and NMSPS, respectively. Tribological behaviors of NMAM and NMSPS against Si3N4 balls are researched under constant speed (0.2 m/s) and varied loads (from 4 to 16 N) for evaluating the tribological properties of NMAM and NMSPS. The results present that NMAM exhibits the excellent tribological properties [low friction coefficients (0.26-0.40) and considerable wear resistance (2.8-4.6 × 10-5 mm3 N-1 m-1)] as compared to NMSPS, which attributes to the uniform enrichment of MLG with properties of high tensile strength and being easily sheared off on the worn surfaces. Owing to the use of spherical prealloyed powder containing multilayer graphene and the characteristics of layer by layer depositing in the AM process, NMAM has a more compact and uniform substrate, which persistently provides a source of the formation of continuous and stable frictional layer. Due to the characteristics of AM rapid solidification, NMAM has the small grain size and well-compacted microstructure, which can effectively reduce the probability of spalling wear and lead to the increase in wear resistance of materials. The research can offer the reference for self-lubricating materials prepared by AM technology.

Bisphenol A polycarbonate as a reference material

NASA Technical Reports Server (NTRS)

Hilado, C. J.; Cumming, H. J.; Williams, J. B.

1977-01-01

Test methods require reference materials to standardize and maintain quality control. Various materials have been evaluated as possible reference materials, including a sample of bisphenol A polycarbonate without additives. Screening tests for relative toxicity under various experimental conditions were performed using male mice exposed to pyrolysis effluents over a 200-800 C temperature range. It was found that the bisphenol A polycarbonate served as a suitable reference material as it is available in large quantities, and does not significantly change with time.

Consumer’s Perception on Design and Layout of Consumer Medical Information Leaflets on Obesity and Lipid Lowering Drugs

PubMed Central

Mathew, Elizabeth M.; Rajiah, Kingston; Sharma, Krishana Kumar

2013-01-01

Background: Printed education materials are often used to augment healthcare professional’s verbal information to consumers so it serves as an important component of symptom management. They also enhance the teaching process and can be used by consumers as a home reference. Objective: This study was aimed to interpret consumers’ perception on Consumer Medical Information Leaflets (CMILs) on obesity and lipid lowering drugs, on design and layout using the standard method such as Baker Able Leaflet Design (BALD). Material and Methods: Convenience sampling was done. The study was conducted over a period of 3 years in community pharmacy settings in Tamil Nadu, India. The Consumer Medical Information Leaflets (CMILs) were randomly collected from different community pharmacies. Total of 19 CMILs which are commonly used by the consumers were collected and CMILs were assessed using BALD assessment tool Results: According to BALD assessment (46.28%) leaflets were rated as ‘above standard’ and (53.72) leaflets were rated as ‘standard or poor’ in layout and design since their scores were less than 25. This shows that this issue may be important from the patient’s perspective, which may discourage patient from actually reading the CMILs. Conclusion: In India, generally CMILs are continued to be prepared in English and with higher proportion of consumers with English illiteracy. CMILs, which are prepared without taking consideration of reading level of consumers and proper layout and design, may not achieve the intended purpose. This is an important aspect that any company has to reckon while preparing leaflets and at least in some major local languages in which CMILs have to be prepared. PMID:24551641

Theophylline-nicotinamide cocrystal formation in physical mixture during storage.

PubMed

Ervasti, Tuomas; Aaltonen, Jaakko; Ketolainen, Jarkko

2015-01-01

Pharmaceutically relevant properties, such as solubility and dissolution rate, of active pharmaceutical ingredients can be enhanced by cocrystal formation. Theophylline and nicotinamide are known to form cocrystals, for example if subjected to solid-state grinding. However, under appropriate conditions, cocrystals can also form in physical mixtures without any mechanical activation. The purpose of this work was to study whether theophylline and nicotinamide could form cocrystals spontaneously, without mechanical activation. Crystalline theophylline and nicotinamide powders were gently mixed manually in a 1:1 molar ratio and stored at different relative humidity and temperature conditions. The solid state of the samples was analyzed by differential scanning calorimetry, Raman spectroscopy and X-ray powder diffractometry. Three different variations of theophylline were used as starting materials, e.g., two size fractions of theophylline anhydrate (large 710 μm-1 mm and small 180-355 μm), and monohydrate (recrystallized from water). As a reference, anhydrous theophylline-nicotinamide cocrystals were prepared by solid-state grinding. The results of this study indicate that theophylline-nicotinamide cocrystals can form without any mechanical activation from physical mixtures of theophylline and nicotinamide during storage. For anhydrous samples, storage humidity was found to be a critical parameter for cocrystal formation. Increasing temperature was also found to have an accelerating effect on the transformation. The effect of particle size of anhydrous theophylline on the transformation rate could not be completely resolved; DSC and Raman indicated slightly faster transformation with a physical mixture prepared from large size fraction of anhydrous theophylline, but the differences were only minor. Cocrystal formation was also observed in the physical mixture prepared from theophylline monohydrate, but the rate was not as high as with samples prepared from anhydrous material. Copyright © 2015 Elsevier B.V. All rights reserved.

40 CFR 1045.810 - What materials does this part reference?

Code of Federal Regulations, 2010 CFR

2010-07-01

... Definitions and Other Reference Information § 1045.810 What materials does this part reference? Documents... material. Table 1 to this section lists material from the Society of Automotive Engineers that we have... the Society of Automotive Engineers, 400 Commonwealth Drive, Warrendale, PA 15096 or http://www.sae...

Method and apparatus for assessing material properties of sheet-like materials

DOEpatents

Telschow, Kenneth L.; Deason, Vance A.

2002-01-01

Apparatus for producing an indication of a material property of a sheet-like material according to the present invention may comprise an excitation source for vibrating the sheet-like material to produce at least one traveling wave therein. A light source configured to produce an object wavefront and a reference wavefront directs the object wavefront toward the sheet-like material to produce a modulated object wavefront. A modulator operatively associated with the reference wavefront modulates the reference wavefront in synchronization with the traveling wave on the sheet-like material to produce a modulated reference wavefront. A sensing medium positioned to receive the modulated object wavefront and the modulated reference wavefront produces an image of the traveling wave in the sheet-like material, the image of the anti-symmetric traveling wave being related to a displacement amplitude of the anti-symmetric traveling wave over a two-dimensional area of the vibrating sheet-like material. A detector detects the image of the traveling wave in the sheet-like material.

10 CFR 1016.33 - External transmission of documents and material.

Code of Federal Regulations, 2011 CFR

2011-01-01

... authorization of DOE. (b) Preparation of documents. Documents containing Restricted Data shall be prepared for... transferred. (c) Preparation of material. Material, other than documents, containing Restricted Data shall be... Section 1016.33 Energy DEPARTMENT OF ENERGY (GENERAL PROVISIONS) SAFEGUARDING OF RESTRICTED DATA Control...

Rheological behaviour, mechanical properties and morphological aspects of thermoplastic polyurethane reinforced with multiwalled carbon nanotubes

NASA Astrophysics Data System (ADS)

Russo, Pietro; Acierno, Domenico; Spena, Paola

2010-06-01

Melt blended compounds based on a film grade thermoplastic polyurethane resin filled with relatively low contents of multiwalled carbon nanotubes have been investigated. Materials, prepared through the production of a masterbatch containing 3 wt% of nanotubes and subsequent dilution of the same by addition of matrix pellets, were analyzed in the form of tapes and films always taking the neat matrix, processed in the same conditions, as the reference. Improvements of the matrix extrudability and mechanical benefits showed for all investigated composite samples have been satisfactorily interpreted by morphological observations carried out in both transmission and scanning electron microscopy.

Advanced methods for preparation and characterization of infrared detector materials. [crystallization and phase diagrams of Hg sub 1-x Cd sub x Te

NASA Technical Reports Server (NTRS)

Lehoczy, S. L.

1979-01-01

Crystal growth of Hg sub 1-x Cd sub x Te and density measurements of ingot slices are discussed. Radial compositional variations are evaluated from the results of infrared transmission edge mapping. The pseudo-binary HgTe-CdTe phase diagram is examined with reference to differential thermal analysis measurements. The phase equilibria calculations, based on the 'regular association solution' theory (R.A.S.) are explained and, using the obtained R.A.S. parameters, the activities of Hg, Cd, and Te vapors and their partial pressures over the pseudo-binary melt are calculated.

An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

PubMed

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

International comparison Euramet.QM-K111—propane in nitrogen

NASA Astrophysics Data System (ADS)

Wouter van der Hout, J.; van der Veen, Adriaan M. H.; Ziel, Paul R.; Kipphardt, Heinrich; Tuma, Dirk; Maiwald, Michael; Fernández, Teresa E.; Gómez, Concepción; Cieciora, Dariusz; Ochman, Grzegorz; Dias, Florbela; Silvino, Victor; Macé, Tatiana; Sutour, Christophe; Marioni, Fabrice; Ackermann, Andreas; Niederhauser, Bernhard; Fükő, Judit; Büki, Tamás; Nagyné Szilágyi, Zsófia; Tarhan, Tanıl; Engin, Erinç

2017-01-01

This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison. The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within +/- 1 % of the KCRV. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Exploratory sensory profiling of three culinary preparations of potatoes (Solanum tuberosum L.).

PubMed

Seefeldt, Helene F; Tønning, Erik; Thybo, Anette K

2011-01-15

A consumer-oriented description of potato quality with regard to culinary preparation could increase potato consumption. The aim of this study was to investigate the sensory attributes in 11 potato varieties grown at two locations and used for three culinary preparations. Sensory evaluation of the potatoes served either as boiled, oven-fried or mashed were performed using 15-19 descriptors for appearance, flavour and texture attributes. A principal component analysis revealed that 45% of the variation in the sensory data was related to variety differences, which was ascribed to variation in appearance, dry matter content and texture. Growing location also significantly affected appearance and texture. The sensory panel judged the sensory attributes 'yellowness', 'hardness', 'adhesiveness' and 'moistness' to be important quality descriptors in all three culinary preparations. Internal references showed the high reproducibility of the sensory evaluations. The potatoes grown in a sandy location had higher content of dry matter compared to those grown in a clay location, affecting the quality. This study showed that it was possible to do reliable and reproducible sensory profiles in a potato material with a large span in quality. Sensory information based on few attributes can be used to describe culinary quality of potato varieties. Copyright © 2010 Society of Chemical Industry.

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

PubMed

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

2015-05-13

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

A comparative study of ChIP-seq sequencing library preparation methods.

PubMed

Sundaram, Arvind Y M; Hughes, Timothy; Biondi, Shea; Bolduc, Nathalie; Bowman, Sarah K; Camilli, Andrew; Chew, Yap C; Couture, Catherine; Farmer, Andrew; Jerome, John P; Lazinski, David W; McUsic, Andrew; Peng, Xu; Shazand, Kamran; Xu, Feng; Lyle, Robert; Gilfillan, Gregor D

2016-10-21

ChIP-seq is the primary technique used to investigate genome-wide protein-DNA interactions. As part of this procedure, immunoprecipitated DNA must undergo "library preparation" to enable subsequent high-throughput sequencing. To facilitate the analysis of biopsy samples and rare cell populations, there has been a recent proliferation of methods allowing sequencing library preparation from low-input DNA amounts. However, little information exists on the relative merits, performance, comparability and biases inherent to these procedures. Notably, recently developed single-cell ChIP procedures employing microfluidics must also employ library preparation reagents to allow downstream sequencing. In this study, seven methods designed for low-input DNA/ChIP-seq sample preparation (Accel-NGS® 2S, Bowman-method, HTML-PCR, SeqPlex™, DNA SMART™, TELP and ThruPLEX®) were performed on five replicates of 1 ng and 0.1 ng input H3K4me3 ChIP material, and compared to a "gold standard" reference PCR-free dataset. The performance of each method was examined for the prevalence of unmappable reads, amplification-derived duplicate reads, reproducibility, and for the sensitivity and specificity of peak calling. We identified consistent high performance in a subset of the tested reagents, which should aid researchers in choosing the most appropriate reagents for their studies. Furthermore, we expect this work to drive future advances by identifying and encouraging use of the most promising methods and reagents. The results may also aid judgements on how comparable are existing datasets that have been prepared with different sample library preparation reagents.

Development of C-reactive protein certified reference material NMIJ CRM 6201-b: optimization of a hydrolysis process to improve the accuracy of amino acid analysis.

PubMed

Kato, Megumi; Kinumi, Tomoya; Yoshioka, Mariko; Goto, Mari; Fujii, Shin-Ichiro; Takatsu, Akiko

2015-04-01

To standardize C-reactive protein (CRP) assays, the National Metrology Institute of Japan (NMIJ) has developed a C-reactive protein solution certified reference material, CRM 6201-b, which is intended for use as a primary reference material to enable the SI-traceable measurement of CRP. This study describes the development process of CRM 6201-b. As a candidate material of the CRM, recombinant human CRP solution was selected because of its higher purity and homogeneity than the purified material from human serum. Gel filtration chromatography was used to examine the homogeneity and stability of the present CRM. The total protein concentration of CRP in the present CRM was determined by amino acid analysis coupled to isotope-dilution mass spectrometry (IDMS-AAA). To improve the accuracy of IDMS-AAA, we optimized the hydrolysis process by examining the effect of parameters such as the volume of protein samples taken for hydrolysis, the procedure of sample preparation prior to the hydrolysis, hydrolysis temperature, and hydrolysis time. Under optimized conditions, we conducted two independent approaches in which the following independent hydrolysis and liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) were combined: one was vapor-phase acid hydrolysis (130 °C, 24 h) and hydrophilic interaction liquid chromatography-mass spectrometry (HILIC-MS) method, and the other was microwave-assisted liquid-phase acid hydrolysis (150 °C, 3 h) and pre-column derivatization liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. The quantitative values of the two different amino acid analyses were in agreement within their uncertainties. The certified value was the weighted mean of the results of the two methods. Uncertainties from the value-assignment method, between-method variance, homogeneity, long-term stability, and short-term stability were taken into account in evaluating the uncertainty for a certified value. The certified value and the expanded uncertainty (k = 2) of CRM 6201-b are (40.0 ± 1.6) μmol kg(-1).

Reproducibility of polycarbonate reference material in toxicity evaluation

NASA Technical Reports Server (NTRS)

Hilado, C. J.; Huttlinger, P. A.

1981-01-01

A specific lot of bisphenol A polycarbonate has been used for almost four years as the reference material for the NASA-USF-PSC toxicity screening test method. The reproducibility of the test results over this period of time indicate that certain plastics may be more suitable reference materials than the more traditional cellulosic materials.

Starting and Operating Live Virtual Reference Services: A How-To-Do-It Manual for Librarians. How-To-Do-It Manuals for Librarians, Number 118.

ERIC Educational Resources Information Center

Meola, Marc; Stormont, Sam

This guide discusses the essentials of live virtual reference, preparing for virtual reference, and implementing and incorporating virtual reference. Chapter 1, "Understanding Live Virtual Reference," lays out what virtual reference is and how it compares to other forms of reference. Chapter 2, "Offering Live Virtual Reference," presents ten…

[Reference values for the blood coagulation tests in Mexico: usefulness of the pooled plasma from blood donors].

PubMed

Calzada-Contreras, Adriana; Moreno-Hernández, Manuel; Castillo-Torres, Noemi Patricia; Souto-Rosillo, Guadalupe; Hernández-Juárez, Jesús; Ricardo-Moreno, María Tania; Sánchez-Fernández, Maria Guadalupe de Jesús; García-González, América; Majluf-Cruz, Abraham

2012-01-01

The blood coagulation system maintains the blood in a liquid state and bleeding and thrombosis are the manifestations of its malfunction. Blood coagulation laboratory evaluates the physiology of this system. To establish both, the reference values for several tests performed at the blood coagulation laboratory as well as the utility of the pooled plasma to perform these assays. MATERIAL AND: In this descriptive, cross-sectional, randomized study, we collected plasma from Mexican Mestizos. Each pooled plasma was prepared with the plasma from at least 20 blood donors. We performed screening and special tests and the Levey-Jennings graphs were built and interpreted after each pass. Results of the tests were analyzed and their distribution was established using the Kolmogorov-Smirnov test. To establish the reference values we used 95% confidence intervals. We collected 72 pooled plasmas. The distribution for PT, APTT, and TT tests was abnormal. Although the PT test showed a bimodal distribution it was normal for factor VII. The reference values for the hemostatic, anticoagulant, and fibrinolytic factors were different from those suggested by the manufacturers. We established the reference values for the blood coagulation tests in the adult Mexican population. We have shown that the pooled plasma must be used for the screening tests. We suggest that each clinical laboratory should establish its own reference values (at least for the screening tests). To reach this objective, we encourage the use of the pooled plasma.

Nicotine, acetanilide and urea multi-level2H-,13C- and15N-abundance reference materials for continuous-flow isotope ratio mass spectrometry

USGS Publications Warehouse

Schimmelmann, A.; Albertino, A.; Sauer, P.E.; Qi, H.; Molinie, R.; Mesnard, F.

2009-01-01

Accurate determinations of stable isotope ratios require a calibration using at least two reference materials with different isotopic compositions to anchor the isotopic scale and compensate for differences in machine slope. Ideally, the S values of these reference materials should bracket the isotopic range of samples with unknown S values. While the practice of analyzing two isotopically distinct reference materials is common for water (VSMOW-SLAP) and carbonates (NBS 19 and L-SVEC), the lack of widely available organic reference materials with distinct isotopic composition has hindered the practice when analyzing organic materials by elemental analysis/isotope ratio mass spectrometry (EA-IRMS). At present only L-glutamic acids USGS40 and USGS41 satisfy these requirements for ??13C and ??13N, with the limitation that L-glutamic acid is not suitable for analysis by gas chromatography (GC). We describe the development and quality testing of (i) four nicotine laboratory reference materials for on-line (i.e. continuous flow) hydrogen reductive gas chromatography-isotope ratio mass-spectrometry (GC-IRMS), (ii) five nicotines for oxidative C, N gas chromatography-combustion-isotope ratio mass-spectrometry (GC-C-IRMS, or GC-IRMS), and (iii) also three acetanilide and three urea reference materials for on-line oxidative EA-IRMS for C and N. Isotopic off-line calibration against international stable isotope measurement standards at Indiana University adhered to the 'principle of identical treatment'. The new reference materials cover the following isotopic ranges: ??2Hnicotine -162 to -45%o, ??13Cnicotine -30.05 to +7.72%, ?? 15Nnicotine -6.03 to +33.62%; ??15N acetanilide +1-18 to +40.57%; ??13Curea -34.13 to +11.71%, ??15Nurea +0.26 to +40.61% (recommended ?? values refer to calibration with NBS 19, L-SVEC, IAEA-N-1, and IAEA-N-2). Nicotines fill a gap as the first organic nitrogen stable isotope reference materials for GC-IRMS that are available with different ??13N values. Comparative ??13C and ??15N on-line EA-IRMS data from 14 volunteering laboratories document the usefulness and reliability of acetanilides and ureas as EA-IRMS reference materials.

Fabrication of PVDF-TrFE based bilayered PbTiO3/PVDF-TrFE films capacitor

NASA Astrophysics Data System (ADS)

Nurbaya, Z.; Wahid, M. H.; Rozana, M. D.; Annuar, I.; Alrokayan, S. A. H.; Khan, H. A.; Rusop, M.

2016-07-01

Development of high performance capacitor is reaching towards new generation where the ferroelectric materials take places as the active dielectric layer. The motivation of this study is to produce high capacitance device with long life cycle. This was configured by preparing bilayered films where lead titanate as an active dielectric layer and stacked with the top dielectric layer, poly(vinyledenefluoride-trifluoroethylene). Both of them are being referred that have one in common which is ferroelectric behavior. Therefore the combination of ceramic and polymer ferroelectric material could perform optimum dielectric characteristic for capacitor applications. The fabrication was done by simple sol-gel spin coating method that being varied at spinning speed property for polymer layers, whereas maintaining the ceramic layer. The characterization of PVDF-TrFE/PbTiO3 was performed according to metal-insulator-metal stacked capacitor measurement which includes structural, dielectric, and ferroelectric measurement.

Friction and Wear Behavior of Selected Dental Ceramics

NASA Astrophysics Data System (ADS)

Park, Jongee; Pekkan, Gurel; Ozturk, Abdullah

The purpose of this study was to determine the friction coefficients and wear rates of six commercially available dental ceramics including IPS Empress 2 (E2), Cergo Pressable Ceramic (CPC), Cercon Ceram (CCS) and Super porcelain EX-3 (SPE). Bovine enamel (BE) was also tested as a reference material for comparison purposes. Samples of the dental ceramics were prepared according to the instructions described by the manufacturers in disk-shape with nominal dimensions of 12 mm × 2 mm. The wear tests were performed by means of a pin-on-disk type tribometer. The friction coefficients and specific wear rates of the materials were determined at a load of 10 N and rotating speed of 0.25 cm/s without lubrication. Surface morphology of the wear tracks was examined using a scanning electron microscope. Statistical analyses were made using one-way ANOVA and Turkey's HSD (P < 0.05).

Development of deep eutectic solvents applied in extraction and separation.

PubMed

Li, Xiaoxia; Row, Kyung Ho

2016-09-01

Deep eutectic solvents, as an alternative to ionic liquids, have greener credentials than ionic liquids, and have attracted considerable attention in related chemical research. Deep eutectic solvents have attracted increasing attention in chemistry for the extraction and separation of various target compounds from natural products. This review highlights the preparation of deep eutectic solvents, unique properties of deep eutectic solvents, and synthesis of deep-eutectic-solvent-based materials. On the other hand, application in the extraction and separation of deep eutectic solvents is also included in this report. In this paper, the available data and references in this field are reviewed to summarize the applications and developments of deep eutectic solvents. Based on the development of deep eutectic solvents, an exploitation of new deep eutectic solvents and deep eutectic solvents-based materials is expected to diversify into extraction and separation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Degradation of strength properties of epoxy resin filled with natural-based particles

NASA Astrophysics Data System (ADS)

Valášek, Petr; Habrová, Karolína; Müller, Miroslav

2018-05-01

Degradation of polymeric materials can be considered as a limiting factor for their use. Mechanical characteristics of epoxy resins are reduced, for example, by the action and changes of temperature or humidity. Degradation also occurs in composite systems where the epoxy resins function as matrices, i.e. in polymer composite materials. If a natural filler is used together with the epoxy resin, we refer to these materials as biocomposites, where also the natural character of the filler material greatly affects the degradation process. The paper focuses on the description of the shear strength of the resin filled with particles prepared from the seeds of dates of Phoenix Dactylifera plant. The degradation was evaluated experimentally in laboratory conditions via the climatic chamber. The experiment describes composites with a particle size of filler 100-200 μm with a concentration of 5 - 10 wt%. As the number of degradation cycles increased, the tensile strength of both the unfilled and the filled epoxy resin decreased. After 5 weeks, the drop was up to 50%. The presence of the particles did not significantly affect the shear strength compared to the non-filled resin. The described way of utilization of the natural-based particles is the possibility of material utilization of secondary natural materials.

Fracture resistance of five pin-retained core build-up materials on teeth with and without extracoronal preparation.

PubMed

Burke, F J; Shaglouf, A G; Combe, E C; Wilson, N H

2000-01-01

Core build-ups should provide satisfactory strength and resistance to fracture both before and after crown preparation. This paper examines the resistance to fracture of core build-ups in different materials and the fracture resistance of core build-ups when these have been reduced for full crown preparation. Standardized core build-ups were made on groups of extracted molar teeth of similar size, with 10 teeth per group. Three resin-composite (prisma APH: Dentsply, Weybridge, UK; Ti-Core, Essential Dental Systems, NJ, US and Coradent, Vivadent, Liechtenstein), one cermet (Ketac-Silver, ESPE GmbH, Seefeld, Germany) and one amalgam material (Duralloy, Degussa Ltd, Cheshire, UK). These specimens were subjected to compressive force on a universal testing machine and the force at fracture noted. Standardized full crown preparations were made on a further five groups of core build-up specimens using the same materials as above. These prepared specimens were subjected to compressive force on a universal testing machine and the force to fracture noted. The results indicated that amalgam core build-ups demonstrated higher fracture resistance than the other materials examined. There was a general decrease in the fracture strength of the specimens following crown preparation, with the teeth restored with the amalgam core build-ups showing a greater percentage reduction in fracture strength than the other materials tested. Prepared core build-ups in a hybrid composite material provided the highest fracture resistance. The cermet material used provided the lowest resistance to fracture in both the core build-up and crown preparation specimens. In terms of fracture resistance, no advantage was apparent in using the two composite materials designated as being specifically appropriate for core build-ups.

Application of an ETV-ICP system for the determination of elements in human hair*1

NASA Astrophysics Data System (ADS)

Plantikow-Voβgätter, F.; Denkhaus, E.

1996-01-01

When determining element contents in hair samples without sample digestion it is necessary to analyze large sample volumes in order to minimize problems of inhomogeneity of biological sample materials. Therefore an electrothermal vaporization system (ETV) is used for solid sample introduction into an inductively coupled plasma (ICP) for the determination of matrix and trace elements in hair. This paper concentrates on the instrumental aspects without time consuming sample preparation. The results obtained for optimization tests, ETV operating parameters and ICP operating parameters, are shown and discussed. Standard additions are used for calibration for the determination of Zn, Mg, and Mn in human hair. Studies including reproducibility and detection limits for chosen elements have been carried out on certified reference materials (CRMs). The determination of reproducibility (relative standard deviation (RSD) of n = 10) and detection limits (DLs) of Zn (RSD < 8.5%, DL < 0.8 μ g -1), Mn (RSD < 14.1%, DL < 0.3 μ g -1), and Mg (RSD < 7.4%, DL < 6.6 μ g -1) are satisfactory. The concentration values found show good agreement with the corresponding certified values. Further sample preparation steps, including hair sampling, washing procedure and homogenization for hair, relating to measurements of real hair samples are described.

Cryomilled and spark plasma sintered titanium: the evolution of microstructure

NASA Astrophysics Data System (ADS)

Kozlík, Jiří; Becker, Hanka; Harcuba, Petr; Stráský, Josef; Janeček, Milos

2017-05-01

Bulk ultra-fine grained (UFG) commercially pure Ti was prepared by cryogenic milling in liquid argon and subsequent spark plasma sintering (SPS). During cryogenic milling, individual powder particles are repetitively severely deformed by attrition forces. Powder particles were not significantly refined, but due to severe repetitive plastic deformation, ultra-fine grained microstructure emerges within each powder particle. Cryogenic milling can be therefore considered as a specific severe plastic deformation (SPD) method. Compactization of cryomilled powder by SPS technique (also referred to as field assisted sintering technique - FAST) requires significantly lower sintering temperatures and shorter sintering times for successful compaction when compared to any other sintering technique. This is crucial for maintaining the UFG microstructure due to its limited thermal stability. Several specimens were prepared by varying processing parameters, in particular the sintering temperature. The microstructure of powders and compacted samples was observed by scanning electron microscopy (SEM). Increased sintering temperature results in recrystallization and grain growth. A trade-off relationship between the density of compacted material and grain size was identified. Microhardness of the material was found to depend on residual porosity rather than grain size. This contribution presents cryogenic milling and spark plasma sintering as a viable alternative for achieving UFG microstructure in commercially pure Ti.

Forensic determination of ricin and the alkaloid marker ricinine from castor bean extracts.

PubMed

Darby, S M; Miller, M L; Allen, R O

2001-09-01

Liquid chromatography/mass spectrometry (LC/ MS) and matrix assisted laser desorption/ionization time-of-flight (MALDI-TOF) MS methods were developed for the presumptive identification of ricin toxin and the alkaloid marker ricinine from crude plant materials. Ricin is an extremely potent poison, which is of forensic interest due to its appearance in terrorism literature and its potential for use as a homicide agent. Difficulties arise in attempting to analyze ricin because it is a large heterogeneous protein with glycosylation. The general protein identification scheme developed uses LC/MS or MALDI-TOF for size classification followed by the use of the same instrumentation for the analysis of the tryptic digest. Fragments of the digest can be searched in an online database for tentative identification of the unknown protein and then followed by comparison to authentic reference materials. LC fractionation or molecular weight cutoff filtration was used for preparation of the intact toxin before analysis. Extracts from two types of castor beans were prepared using a terrorist handbook procedure and determined to contain 1% ricin. Additionally, a forensic sample suspected to contain ricin was analyzed using the presented identification scheme (data not shown). The identification of the alkaloid ricinine by GC/MS and LC/MS was shown to be a complementary technique for the determination of castor bean extracts.

A facile method to prepare a versatile surface coating with fibrinolytic activity, vascular cell selectivity and antibacterial properties.

PubMed

Jin, Sheng; Gu, Hao; Chen, Xianshuang; Liu, Xiaoli; Zhan, Wenjun; Wei, Ting; Sun, Xuebo; Ren, Chuanlu; Chen, Hong

2018-07-01

Clot and thrombus formation on surfaces that come into contact with blood is still the most serious problem for blood contacting devices. Despite many years of continuous efforts in developing hemocompatible materials, it is still of great interest to develop multifunctional materials to enable vascular cell selectivity (to favor rapid endothelialization while inhibiting smooth muscle cell proliferation) and improve hemocompatibility. In addition, biomaterial-associated infections also cause the failure of biomedical implants and devices. However, it remains a challenging task to design materials that are multifunctional, since one of their functions will usually be compromised by the introduction of another function. In the present work, the gold substrate was first layer-by-layer (LbL) deposited with a multilayered polyelectrolyte film containing chitosan (positively charged) and a copolymer of sodium 4-vinylbenzenesulfonate (SS) and the "guest" adamantane monomer 1-adamantan-1-ylmethyl methacrylate (P(SS-co-Ada), negatively charged) via electro-static interactions, referred to as Au-LbL. The chitosan and P(SS-co-Ada) were intended to provide, respectively, resistance to bacteria and heparin-like properties. Then, "host" β-cyclodextrin derivatives bearing seven lysine ligands (CD-L) were immobilized on the Au-LbL surface by host-guest interactions between adamantane residues and CD-L, referred to as Au-LbL/CD-L. Finally, a versatile surface coating with fibrinolytic activity (lysis of nascent clots), vascular cell selectivity and antibacterial properties was developed. Copyright © 2018 Elsevier B.V. All rights reserved.

Surface protection coating material for controlling the decay of major construction stone

NASA Astrophysics Data System (ADS)

Arun, T.; Ray, D. K.; Gupta, V. P.; Panda, S. S.; Sahoo, P. K.; Ghosh, Jaydip; Sengupta, Pranesh; Satyam, P. V.

2017-05-01

Degradation of the building stones are creating instability in the old building and monuments which is to be protected. To investigate the characteristics of such a stones used for the construction in eastern India, we have collected the khondalite stones. The microstructural and elemental composition analysis of the khondalite stones are analyzed by using SEM, EDX and PIXE trace elemental analysis. We have prepared surface protection coating material with graphene oxide and cobalt ferrite as a base material along with other residuals. The prepared coating materials is coated on the galvanized iron substrate for further characterization. The surface morphology characteristics of the coating material is analyzed by SEM and AFM. The corrosion resistance characteristics of the prepared coating material is studied by the electrochemical impedance spectroscopy. The results suggests that the prepared coating material can be used as a surface protection materials to control the self-destruction of khondalite stones.

Some aspects of applying nanostructured materials in air filtration, water filtration and electrical engineering

NASA Astrophysics Data System (ADS)

Kimmer, Dusan; Vincent, Ivo; Lovecka, Lenka; Kazda, Tomas; Giurg, Adam; Skorvan, Ondrej

2017-05-01

Nanostructures prepared from nanofibres and nanostructured composites prepared from nanofibres and fillers are gradually becoming increasingly demanded materials for applications in various industrial branches connected with catalysis, environment protection (air filtration, waste water treatment, sound absorption), in biological engineering, electronics (battery separators, electrode materials), etc. Selected applications of these materials prepared in the company SPUR a.s. are summed up in the following presentation.

[Development of the certified reference material of mercury in lyophilized human urine].

PubMed

Zhao, Wei; Zhang, Fu-gang; DU, Hui-fang; Pan, Ya-juan; Yan, Hui-fang

2011-02-01

To develop the certified reference material of mercury in lyophilized human urine. Human urine samples from normal level mercury districts were filtered, homogenized, dispensed, lyophilized and radio-sterilized. Homogeneity test, stability inspection and certification were conducted using a atom fluorescence spectrophotometric method. The physical and chemical stability of the certified reference material were assessed for 18 months. The certified values are based on analysis made by three independent laboratories. The certified values are as follows: low level was (35.6 ± 2.1) µg/L, high level was (50.5 ± 3.0) µg/L. The certified reference material of mercury in lyophilized human urine in this research reached the national certified reference material requirements and could be used for the quality control.

Devices for the Production of Reference Gas Mixtures.

PubMed

Fijało, Cyprian; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

2016-09-02

For many years there has been growing demand for gaseous reference materials, which is connected with development in many fields of science and technology. As a result, new methodological and instrumental solutions appear that can be used for this purpose. Appropriate quality assurance/quality control (QA/QC) must be used to make sure that measurement data are a reliable source of information. Reference materials are a significant element of such systems. In the case of gas samples, such materials are generally called reference gas mixtures. This article presents the application and classification of reference gas mixtures, which are a specific type of reference materials, and the methods for obtaining them are described. Construction solutions of devices for the production of reference gas mixtures are detailed, and a description of a prototype device for dynamic production of reference gas mixtures containing aroma compounds is presented.

Development of Certified Reference Materials for Diarrhetic Shellfish Poisoning Toxins, Part 1: Calibration Solutions.

PubMed

Beach, Daniel G; Crain, Sheila; Lewis, Nancy; LeBlanc, Patricia; Hardstaff, William R; Perez, Ruth A; Giddings, Sabrina D; Martinez-Farina, Camilo F; Stefanova, Roumiana; Burton, Ian W; Kilcoyne, Jane; Melanson, Jeremy E; Quilliam, Michael A; McCarron, Pearse

2016-09-01

Okadaic acid (OA) and its analogs dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic polyethers produced by marine dinoflagellates. These toxins accumulate in shellfish and cause diarrhetic shellfish poisoning (DSP) in humans. Regulatory testing of shellfish is essential to safeguard public health and for international trade. Certified reference materials (CRMs) play a key role in analytical monitoring programs. This paper presents an overview of the interdisciplinary work that went into the planning, production, and certification of calibration-solution CRMs for OA, DTX1, and DTX2. OA and DTX1 were isolated from large-scale algal cultures and DTX2 from naturally contaminated mussels. Toxins were isolated by a combination of extraction and chromatographic steps with processes adapted to suit the source and concentration of each toxin. New 19-epi-DSP toxin analogs were identified as minor impurities. Once OA, DTX1, and DTX2 were established to be of suitable purity, solutions were prepared and dispensed into flame-sealed glass ampoules. Certification measurements were carried out using quantitative NMR spectroscopy and LC-tandem MS. Traceability of measurements was established through certified external standards of established purity. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization, with components from the measurement, stability, and homogeneity studies being propagated into final combined uncertainties.

A manual for a laboratory information management system (LIMS) for light stable isotopes

USGS Publications Warehouse

Coplen, Tyler B.

1997-01-01

The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program is presented herein. Major benefits of this system include (i) an increase in laboratory efficiency, (ii) reduction in the use of paper, (iii) reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) decreased errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for stable isotope laboratories. Since the original publication of the manual for LIMS for Light Stable Isotopes, the isotopes 3 H, 3 He, and 14 C, and the chlorofluorocarbons (CFCs), CFC-11, CFC-12, and CFC-113, have been added to this program.

A manual for a Laboratory Information Management System (LIMS) for light stable isotopes

USGS Publications Warehouse

Coplen, Tyler B.

1998-01-01

The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program is presented herein. Major benefits of this system include (i) an increase in laboratory efficiency, (ii) reduction in the use of paper, (iii) reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) decreased errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for stable isotope laboratories. Since the original publication of the manual for LIMS for Light Stable Isotopes, the isotopes 3 H, 3 He, and 14 C, and the chlorofluorocarbons (CFCs), CFC-11, CFC-12, and CFC-113, have been added to this program.

Detection of nanomaterials in food and consumer products: bridging the gap from legislation to enforcement.

PubMed

Stamm, H; Gibson, N; Anklam, E

2012-08-01

This paper describes the requirements and resulting challenges for the implementation of current and upcoming European Union legislation referring to the use of nanomaterials in food, cosmetics and other consumer products. The European Commission has recently adopted a recommendation for the definition of nanomaterials. There is now an urgent need for appropriate and fit-for-purpose analytical methods in order to identify nanomaterials properly according to this definition and to assess whether or not a product contains nanomaterials. Considering the lack of such methods to date, this paper elaborates on the challenges of the legislative framework and the type of methods needed, not only to facilitate implementation of labelling requirements, but also to ensure the safety of products coming to the market. Considering the many challenges in the analytical process itself, such as interaction of nanoparticles with matrix constituents, potential agglomeration and aggregation due to matrix environment, broad variety of matrices, etc., there is a need for integrated analytical approaches, not only for sample preparation (e.g. separation from matrix), but also for the actual characterisation. Furthermore, there is an urgent need for quality assurance tools such as validated methods and (certified) reference materials, including materials containing nanoparticles in a realistic matrix (food products, cosmetics, etc.).

The bactericidal activity of glutaraldehyde-impregnated polyurethane.

PubMed

Sehmi, Sandeep K; Allan, Elaine; MacRobert, Alexander J; Parkin, Ivan

2016-10-01

Although glutaraldehyde is known to be bactericidal in solution, its potential use to create novel antibacterial polymers suitable for use in healthcare environments has not been evaluated. Here, novel materials were prepared in which glutaraldehyde was either incorporated into polyurethane using a simple "swell-encapsulation-shrink" method (hereafter referred to as "glutaraldehyde-impregnated polyurethane"), or simply applied to the polymer surface (hereafter referred to as "glutaraldehyde-coated polyurethane"). The antibacterial activity of glutaraldehyde-impregnated and glutaraldehyde-coated polyurethane samples was tested against Escherichia coli and Staphylococcus aureus. Glutaraldehyde-impregnated polyurethane resulted in a 99.9% reduction in the numbers of E. coli within 2 h and a similar reduction of S. aureus within 1 h, whereas only a minimal reduction in bacterial numbers was observed when the biocide was bound to the polymer surface. After 15 days, however, the bactericidal activity of the impregnated material was substantially reduced presumably due to polymerization of glutaraldehyde. Thus, although glutaraldehyde retains antibacterial activity when impregnated into polyurethane, activity is not maintained for extended periods of time. Future work should examine the potential of chemical modification of glutaraldehyde and/or polyurethane to improve the useful lifespan of this novel antibacterial polymer. © 2016 The Authors. MicrobiologyOpen published by John Wiley & Sons Ltd.

Nanocrystalline ceramic materials

DOEpatents

Siegel, Richard W.; Nieman, G. William; Weertman, Julia R.

1994-01-01

A method for preparing a treated nanocrystalline metallic material. The method of preparation includes providing a starting nanocrystalline metallic material with a grain size less than about 35 nm, compacting the starting nanocrystalline metallic material in an inert atmosphere and annealing the compacted metallic material at a temperature less than about one-half the melting point of the metallic material.

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

PubMed

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

2014-04-01

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

Quantification of methionine and selenomethionine in biological samples using multiple reaction monitoring high performance liquid chromatography tandem mass spectrometry (MRM-HPLC-MS/MS).

PubMed

Vu, Dai Long; Ranglová, Karolína; Hájek, Jan; Hrouzek, Pavel

2018-05-01

Quantification of selenated amino-acids currently relies on methods employing inductively coupled plasma mass spectrometry (ICP-MS). Although very accurate, these methods do not allow the simultaneous determination of standard amino-acids, hampering the comparison of the content of selenated versus non-selenated species such as methionine (Met) and selenomethionine (SeMet). This paper reports two approaches for the simultaneous quantification of Met and SeMet. In the first approach, standard enzymatic hydrolysis employing Protease XIV was applied for the preparation of samples. The second approach utilized methanesulfonic acid (MA) for the hydrolysis of samples, either in a reflux system or in a microwave oven, followed by derivatization with diethyl ethoxymethylenemalonate. The prepared samples were then analyzed by multiple reaction monitoring high performance liquid chromatography tandem mass spectrometry (MRM-HPLC-MS/MS). Both approaches provided platforms for the accurate determination of selenium/sulfur substitution rate in Met. Moreover the second approach also provided accurate simultaneous quantification of Met and SeMet with a low limit of detection, low limit of quantification and wide linearity range, comparable to the commonly used gas chromatography mass spectrometry (GC-MS) method or ICP-MS. The novel method was validated using certified reference material in conjunction with the GC-MS reference method. Copyright © 2018. Published by Elsevier B.V.

Oxygen electrodes for rechargeable alkaline fuel cells

NASA Technical Reports Server (NTRS)

Swette, Larry; Giner, Jose

1987-01-01

Electrocatalysts and supports for the positive electrode of moderate temperature single unit rechargeable alkaline fuel cells were investigated and developed. The electrocatalysts are defined as the material with a higher activity for the oxygen electrode reaction than the support. Advanced development will require that the materials be prepared in high surface area forms, and may also entail integration of various candidate materials. Eight candidate support materials and seven electrocatalysts were investigated. Of the 8 support, 3 materials meet the preliminary requirements in terms of electrical conductivity and stability. Emphasis is now on preparing in high surface area form and testing under more severe corrosion stress conditions. Of the 7 electrocatalysts prepared and evaluated, at least 5 materials remain as potential candidates. The major emphasis remains on preparation, physical characterization and electrochemical performance testing.

Some possible reference materials for fire toxicity tests

NASA Technical Reports Server (NTRS)

Hilado, C. J.; Solis, A. N.

1977-01-01

Suitable reference materials need to be selected in order to standardize any test method. The evaluation of cotton, polyethylene, polyether sulfone, polycarbonate, polystyrene, and polyurethane flexible and rigid foams as possible reference materials for the University of San Francisco/NASA toxicity screening test method is discussed.

Quaternary Geologic Map of the Lake Nipigon 4 Degrees x 6 Degrees Quadrangle, United States and Canada

USGS Publications Warehouse

Sado, Edward V.; Fullerton, David S.; Farrand, William R.; Edited and Integrated by Fullerton, David S.

1994-01-01

The Quaternary Geologic Map of the Lake Nipigon 4 degree x 6 degree Quadrangle was mapped as part of the Quaternary Geologic Atlas of the United States. The atlas was begun as an effort to depict the areal distribution of surficial geologic deposits and other materials that accumulated or formed during the past 2+ million years, the period that includes all activities of the human species. These materials are at the surface of the earth. They make up the 'ground' on which we walk, the 'dirt' in which we dig foundations, and the 'soil' in which we grow crops. Most of our human activity is related in one way or another to these surface materials that are referred to collectively by many geologists as regolith, the mantle of fragmental and generally unconsolidated material that overlies the bedrock foundation of the continent. The maps were compiled at 1:1,000,000 scale. This map is a product of collaboration of the Ontario Geological Survey, the University of Michigan, and the U.S. Geological Survey, and is designed for both scientific and practical purposes. It was prepared in two stages. First, separate maps and map explanations were prepared by the compilers. Second, the maps were combined, integrated, and supplemented by the editor. Map unit symbols were revised to a uniform system of classification and the map unit descriptions were prepared by the editor from information received from the compilers and from additional sources listed under Sources of Information. Diagrams accompanying the map were prepared by the editor. For scientific purposes, the map differentiates Quaternary surficial deposits on the basis of lithology or composition, texture or particle size, structure, genesis, stratigraphic relationships, engineering geologic properties, and relative age, as shown on the correlation diagram and indicated in the map unit descriptions. Deposits of some constructional landforms, such as kame moraine deposits, are distinguished as map units. Deposits of erosional landforms, such as outwash terraces, are not distinguished, although glaciofluvial, ice-contact, and lacustrine deposits that are mapped may be terraced. As a Quaternary geologic map it serves as a base from which a variety of maps relating Quaternary geologic history can be derived. For practical purposes, the map is a surficial materials map. Materials are distinguished on the basis of lithology or composition, texture or particle size, and other physical, chemical, and engineering characteristics. It is not a map of soils that are recognized and classified in pedology or agronomy. Rather, it is a generalized map of soils as recognized in engineering geology, or of substrata or parent materials in which pedologic or agronomic soils are formed. As a materials map it serves as a base from which a variety of maps for use in planning engineering, land use, or land management projects can be derived.

40 CFR Table 3 to Subpart Uuuu of... - Initial Compliance With Emission Limits and Work Practice Standards

Code of Federal Regulations, 2012 CFR

2012-07-01

...) you prepare a material balance that includes the pertinent data used to determine the percent... uncontrolled total sulfide emissions were reduced by at least 75%; (3) you prepare a material balance that... uncontrolled total sulfide emissions were reduced by at least 35%; (3) you prepare a material balance that...

40 CFR Table 3 to Subpart Uuuu of... - Initial Compliance With Emission Limits and Work Practice Standards

Code of Federal Regulations, 2013 CFR

2013-07-01

...) you prepare a material balance that includes the pertinent data used to determine the percent... uncontrolled total sulfide emissions were reduced by at least 75%; (3) you prepare a material balance that... uncontrolled total sulfide emissions were reduced by at least 35%; (3) you prepare a material balance that...

40 CFR Table 3 to Subpart Uuuu of... - Initial Compliance With Emission Limits and Work Practice Standards

Code of Federal Regulations, 2014 CFR

2014-07-01

...) you prepare a material balance that includes the pertinent data used to determine the percent... uncontrolled total sulfide emissions were reduced by at least 75%; (3) you prepare a material balance that... uncontrolled total sulfide emissions were reduced by at least 35%; (3) you prepare a material balance that...

Trace elements in a commercial freeze-dried human urine reference material.

PubMed

Veillon, C; Patterson, K Y

1996-07-01

A large batch of freeze-dried human urine reference material, Seronorm Trace Elements Urine, Lot 101021, was prepared commercially (Nycomed Pharma AS, Oslo, Norway) for quality control purposes in trace element analysis. Analytes are being determined by a voluntary, international co-operative effort so that the material will be available to the scientific community at modest cost. The material is in stoppered glass vials and is to be reconstituted with 5.00 ml of water prior to use. We have evaluated the trace element content for several elements, including chromium and zinc, elements for which we have two independent methods available for the determinations, namely isotope dilution mass spectrometry (IDMS) and atomic absorption spectrometry (AAS). We also report on other trace elements measured by IDMS alone, such as Se, for which we have enriched stable isotopes available. Results for chromium indicate a mean +/- standard deviation (n = 10) of 1.2 +/- 0.3 (by IDMS) and 1.4 +/- 0.3 (by AAS) ng Cr per ml of reconstituted urine, indicating possible inhomogeneity and/or contamination (21-25% relative standard deviation, RSD). Approximately half of the observed chromium originates from the sample container. The values observed for zinc were 590 +/- 90 ng ml-1 (15% RSD) for freshly reconstituted material, 760 +/- 60 ng ml-1 (8% RSD) for material reconstituted 4 d earlier, and 940 +/- 60 ng ml-1 (6% RSD) 2 months after reconstitution. Selenium values by IDMS were very reproducible, with a mean concentration of 16 +/- 0.15 ng g-1 (0.9% RSD), suggesting little or no contamination and a high degree of sample homogeneity for this element. The source of potential contaminants has been evaluated by multielement determinations of leachates of the vials and stoppers. Elements noted in significant amounts include B, Ba, Sr, Mo, Cu and Zn, with most of the zinc coming from the rubber stopper.

Evaluation of purity with its uncertainty value in high purity lead stick by conventional and electro-gravimetric methods

PubMed Central

2013-01-01

Background A conventional gravimetry and electro-gravimetry study has been carried out for the precise and accurate purity determination of lead (Pb) in high purity lead stick and for preparation of reference standard. Reference materials are standards containing a known amount of an analyte and provide a reference value to determine unknown concentrations or to calibrate analytical instruments. A stock solution of approximate 2 kg has been prepared after dissolving approximate 2 g of Pb stick in 5% ultra pure nitric acid. From the stock solution five replicates of approximate 50 g have been taken for determination of purity by each method. The Pb has been determined as PbSO4 by conventional gravimetry, as PbO2 by electro gravimetry. The percentage purity of the metallic Pb was calculated accordingly from PbSO4 and PbO2. Results On the basis of experimental observations it has been concluded that by conventional gravimetry and electro-gravimetry the purity of Pb was found to be 99.98 ± 0.24 and 99.97 ± 0.27 g/100 g and on the basis of Pb purity the concentration of reference standard solutions were found to be 1000.88 ± 2.44 and 1000.81 ± 2.68 mg kg-1 respectively with 95% confidence level (k = 2). The uncertainty evaluation has also been carried out in Pb determination following EURACHEM/GUM guidelines. The final analytical results quantifying uncertainty fulfills this requirement and gives a measure of the confidence level of the concerned laboratory. Conclusions Gravimetry is the most reliable technique in comparison to titremetry and instrumental method and the results of gravimetry are directly traceable to SI unit. Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In classical gravimetry the major uncertainties are due to repeatability but in electro-gravimetry several other factors also affect the final results. PMID:23800080

Evaluation of purity with its uncertainty value in high purity lead stick by conventional and electro-gravimetric methods.

PubMed

Singh, Nahar; Singh, Niranjan; Tripathy, S Swarupa; Soni, Daya; Singh, Khem; Gupta, Prabhat K

2013-06-26

A conventional gravimetry and electro-gravimetry study has been carried out for the precise and accurate purity determination of lead (Pb) in high purity lead stick and for preparation of reference standard. Reference materials are standards containing a known amount of an analyte and provide a reference value to determine unknown concentrations or to calibrate analytical instruments. A stock solution of approximate 2 kg has been prepared after dissolving approximate 2 g of Pb stick in 5% ultra pure nitric acid. From the stock solution five replicates of approximate 50 g have been taken for determination of purity by each method. The Pb has been determined as PbSO4 by conventional gravimetry, as PbO2 by electro gravimetry. The percentage purity of the metallic Pb was calculated accordingly from PbSO4 and PbO2. On the basis of experimental observations it has been concluded that by conventional gravimetry and electro-gravimetry the purity of Pb was found to be 99.98 ± 0.24 and 99.97 ± 0.27 g/100 g and on the basis of Pb purity the concentration of reference standard solutions were found to be 1000.88 ± 2.44 and 1000.81 ± 2.68 mg kg-1 respectively with 95% confidence level (k = 2). The uncertainty evaluation has also been carried out in Pb determination following EURACHEM/GUM guidelines. The final analytical results quantifying uncertainty fulfills this requirement and gives a measure of the confidence level of the concerned laboratory. Gravimetry is the most reliable technique in comparison to titremetry and instrumental method and the results of gravimetry are directly traceable to SI unit. Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In classical gravimetry the major uncertainties are due to repeatability but in electro-gravimetry several other factors also affect the final results.

A Paradigm for EST Materials Preparation.

ERIC Educational Resources Information Center

Carreon, Edwina S.; Balarbar, Corazon V.

In many countries, suitable English for special purposes (ESP) textbooks and materials are difficult to find. ESP teachers and program coordinators often must develop their own materials, but preparing such materials requires training. One model that has served as a guide to numerous ESP materials projects is the Hutchinson and Waters' model. This…

SPME-GC-pyrolysis-AFS determination of methylmercury in marine fish products by alkaline sample preparation and aqueous phase phenylation derivatization.

PubMed

Jókai, Zsuzsa; Abrankó, László; Fodor, Péter

2005-07-13

Characterization of a cost-efficient analytical method based on alkaline sample digestion with KOH and NaOH, followed by aqueous phase phenylation derivatization with NaBPh4 and solid phase microextraction (SPME) for the determination of methylmercury in typical fish-containing food samples commercially available in Hungary, is reported. The sample preparation procedure along with the applied SPME-GC-pyrolysis-AFS system was validated by measuring certified reference materials (CRM) BCR-464, TORT-2, and a candidate CRM BCR 710. To carry out an estimation of average Hungarian methylmercury exposures via marine fish and/or fish-containing food consumption, 16 commercially available products and 3 pooled representative seafood samples of-according to a previous European survey--the three most consumed fish species in Hungary, herring, sardines, and hake, were analyzed. Methylmercury concentrations of the analyzed samples were in the range 0.016-0.137 microg of MeHg g(-1) dry weight as Hg.

Evaluation of inorganic elements in cat's claw teas using ICP OES and GF AAS.

PubMed

Pereira, João B; Dantas, Kelly G F

2016-04-01

The determination of Ba, Ca, Cu, Fe, Mg, Mn, P, Pb, and Zn by inductively coupled plasma optical emission spectrometry (ICP OES), and Se by graphite furnace atomic absorption spectrometry (GF AAS), has been carried out in dry matter and teas from 11 samples of the cat's claw plant. The accuracy and precision values were verified against GBW 07604 (Poplar leaves) certified reference material and by the recovery test. Results showed a high content of Ca in the medicinal plant studied, followed by Mg and P. The values obtained showed that the elements studied have different concentrations depending on the method of tea preparation. The highest levels were observed in Ca and Mg, and the lowest for Se and Pb, by both infusion and decoction. Teas prepared from this plant were found to be at safe levels for human consumption, and may be suitable as sources of these elements in the human diet. Copyright © 2015 Elsevier Ltd. All rights reserved.

The XRD Study of the Effect of Slight Change in Structure on the Superconductivity of Y-Ba-Cu-O System Material

NASA Astrophysics Data System (ADS)

Huaqin, Wang; Shiyuan, Zhang; Tongzheng, Jin; Shiying, Han; Dirong, Qiu; Hao, Wang; Ningsheng, Zhou

In this paper the differences in diffraction intensities from some crystal planes in the X-ray diffraction patterns of high Tc Y-Ba-Cu-O system superconductors prepared by different processing conditions and the difference among various structure cells in references are interpreted using computer fitting. The results suggest that there exists two structure cells in the single phase YBa2Cu3O7-x samples. Both structure cells have the same crystal symmetry and almost the same lattice parameters, a=3.821Å, b=3.892Å and c=11.676Å, but the different distortion degree of Cu2-O plane. According to EPR spectra measured on the same samples, it is considered that the improvement of superconductivity for the samples prepared by two-step annealing in flowing oxygen may be related to concentration of the structure cell with more serious distortion on the Cu2-O plane.

Room-temperature processed tin oxide thin film as effective hole blocking layer for planar perovskite solar cells

NASA Astrophysics Data System (ADS)

Tao, Hong; Ma, Zhibin; Yang, Guang; Wang, Haoning; Long, Hao; Zhao, Hongyang; Qin, Pingli; Fang, Guojia

2018-03-01

Tin oxide (SnO2) film with high mobility and good transmittance has been reported as a promising semiconductor material for high performance perovskite solar cells (PSCs). In this study, ultrathin SnO2 film synthesized by radio frequency magnetron sputtering (RFMS) method at room temperature was employed as hole blocking layer for planar PSCs. The room-temperature sputtered SnO2 film not only shows favourable energy band structure but also improves the surface topography of fluorine doped SnO2 (FTO) substrate and perovskite (CH3NH3PbI3) layer. Thus, this SnO2 hole blocking layer can efficiently promote electron transport and suppress carrier recombination. Furthermore, the best efficiency of 13.68% was obtained for planar PSC with SnO2 hole blocking layer prepared at room temperature. This research highlights the room-temperature preparation process of hole blocking layer in PSC and has a certain reference significance for the usage of flexible and low-cost substrates.

Controlled release of therapeutics using interpenetrating polymeric networks.

PubMed

Aminabhavi, Tejraj M; Nadagouda, Mallikarjuna N; More, Uttam A; Joshi, Shrinivas D; Kulkarni, Venkatrao H; Noolvi, Malleshappa N; Kulkarni, Padmakar V

2015-04-01

The ever-increasing developments in pharmaceutical formulations have led to the widespread use of biodegradable polymers in various forms and configurations. In particular, interpenetrating network (IPN) and semi-IPN polymer structures that are capable of releasing drugs in a controlled manner have gained much wider importance in recent years. Recently, IPNs and semi-IPNs have emerged as innovative materials of choice in controlled release (CR) of drugs as the release from these systems depends on pH of the media and temperature in addition to the nature of the system. These networks can be prepared as smart hydrogels following chemical or physical crosslinking methods to show remarkable drug release patterns compared to single polymer systems. A large number of IPNs and semi-IPNs have been reported in the literature. The present review is focused on the preparation methods and their CR properties with reference to anticancer, anti-asthmatic, antibiotic, anti-inflammatory, anti-tuberculosis and antihypertensive drugs, as majority of these drugs have been reported to be the ideal choices for using IPNs and semi-IPNs.

A spray technique for preparing uniform large-area PIXE calibration standards from aqueous solutions

NASA Astrophysics Data System (ADS)

Menzel, N.; Hietel, B.; Leirer, M.; Szymczak, W.; Wittmaack, K.

1999-04-01

We describe a procedure for preparing reference standards that can be used to calibrate PIXE spectra of aerosol deposits collected on suitable backing films made, for example, of synthesised polymers (polypropylene, polycarbonate etc.) or chemically modified biopolymers (e.g., cellulose actetate). Aqueous solutions of well defined concentration were prepared from metal salts. The solutions were spray-deposited on cellulose acetate backings using a nebuliser. Lateral uniformity of the deposited layer over areas ranging from several mm to several cm was accomplished by raster scanning the table on which the backing was mounted. By optimising the experimental parameters, deposition could be accomplished without any detectable wetting of delicate substrates like paper. The areal density of the deposited material was calculated from the concentration of the solute, the volume of the consumed solution and the raster scanned area. The reference standards were analysed by PIXE using an external beam chamber backfilled with helium. The Si(Li) based detection system contained a thin funny filter so that X-ray spectra could be measured down to 1 keV. The proton energy on impact was 1.1 MeV. This relatively low probe energy has the advantage of producing favourable elemental X-ray peak heights relative to the bremsstrahlung-background, notably at energies between 2 and 7 keV. Under the same conditions sufficiently high X-ray yields were achieved for heavy elements like Zn and Pb. Using large area beams, bombardment-induced stress in the backing films could be kept at a low level so that very reproducible background spectra were obtained. Hence a straightforward background subtraction routine could be employed. Sensitivities were determined for 23 elements ranging from Na to Pb. Advantages and problems associated with the different metal salts are discussed briefly.

Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS).

PubMed

Torres, D P; Martins-Teixeira, M B; Silva, E F; Queiroz, H M

2012-01-01

A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 µg kg(-1). This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.

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

NASA Astrophysics Data System (ADS)

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

2017-02-01

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

10 CFR 431.105 - Materials incorporated by reference.

Code of Federal Regulations, 2012 CFR

2012-01-01

... Storage Tanks Test Procedures § 431.105 Materials incorporated by reference. (a) The Department... Water Supply Boilers, and Unfired Hot Water Storage Tanks,” Docket No. EE-RM/TP-99-480, Forrestal... 10 Energy 3 2012-01-01 2012-01-01 false Materials incorporated by reference. 431.105 Section 431...

Nicotine, acetanilide and urea multi-level 2H-, 13C- and 15N-abundance reference materials for continuous-flow isotope ratio mass spectrometry.

PubMed

Schimmelmann, Arndt; Albertino, Andrea; Sauer, Peter E; Qi, Haiping; Molinie, Roland; Mesnard, François

2009-11-01

Accurate determinations of stable isotope ratios require a calibration using at least two reference materials with different isotopic compositions to anchor the isotopic scale and compensate for differences in machine slope. Ideally, the delta values of these reference materials should bracket the isotopic range of samples with unknown delta values. While the practice of analyzing two isotopically distinct reference materials is common for water (VSMOW-SLAP) and carbonates (NBS 19 and L-SVEC), the lack of widely available organic reference materials with distinct isotopic composition has hindered the practice when analyzing organic materials by elemental analysis/isotope ratio mass spectrometry (EA-IRMS). At present only L-glutamic acids USGS40 and USGS41 satisfy these requirements for delta13C and delta15N, with the limitation that L-glutamic acid is not suitable for analysis by gas chromatography (GC). We describe the development and quality testing of (i) four nicotine laboratory reference materials for on-line (i.e. continuous flow) hydrogen reductive gas chromatography-isotope ratio mass-spectrometry (GC-IRMS), (ii) five nicotines for oxidative C, N gas chromatography-combustion-isotope ratio mass-spectrometry (GC-C-IRMS, or GC-IRMS), and (iii) also three acetanilide and three urea reference materials for on-line oxidative EA-IRMS for C and N. Isotopic off-line calibration against international stable isotope measurement standards at Indiana University adhered to the 'principle of identical treatment'. The new reference materials cover the following isotopic ranges: delta2H(nicotine) -162 to -45 per thousand, delta13C(nicotine) -30.05 to +7.72 per thousand, delta15N(nicotine) -6.03 to +33.62 per thousand; delta15N(acetanilide) +1.18 to +40.57 per thousand; delta13C(urea) -34.13 to +11.71 per thousand, delta15N(urea) +0.26 to +40.61 per thousand (recommended delta values refer to calibration with NBS 19, L-SVEC, IAEA-N-1, and IAEA-N-2). Nicotines fill a gap as the first organic nitrogen stable isotope reference materials for GC-IRMS that are available with different delta15N values. Comparative delta13C and delta15N on-line EA-IRMS data from 14 volunteering laboratories document the usefulness and reliability of acetanilides and ureas as EA-IRMS reference materials. Copyright 2009 John Wiley & Sons, Ltd.

Nanocrystalline ceramic materials

DOEpatents

Siegel, R.W.; Nieman, G.W.; Weertman, J.R.

1994-06-14

A method is disclosed for preparing a treated nanocrystalline metallic material. The method of preparation includes providing a starting nanocrystalline metallic material with a grain size less than about 35 nm, compacting the starting nanocrystalline metallic material in an inert atmosphere and annealing the compacted metallic material at a temperature less than about one-half the melting point of the metallic material. 19 figs.

Baseline Assessment of 25-Hydroxyvitamin D Reference Material and Proficiency Testing/External Quality Assurance Material Commutability: A Vitamin D Standardization Program Study.

PubMed

Phinney, Karen W; Sempos, Christopher T; Tai, Susan S-C; Camara, Johanna E; Wise, Stephen A; Eckfeldt, John H; Hoofnagle, Andrew N; Carter, Graham D; Jones, Julia; Myers, Gary L; Durazo-Arvizu, Ramon; Miller, W Greg; Bachmann, Lorin M; Young, Ian S; Pettit, Juanita; Caldwell, Grahame; Liu, Andrew; Brooks, Stephen P J; Sarafin, Kurtis; Thamm, Michael; Mensink, Gert B M; Busch, Markus; Rabenberg, Martina; Cashman, Kevin D; Kiely, Mairead; Galvin, Karen; Zhang, Joy Y; Kinsella, Michael; Oh, Kyungwon; Lee, Sun-Wha; Jung, Chae L; Cox, Lorna; Goldberg, Gail; Guberg, Kate; Meadows, Sarah; Prentice, Ann; Tian, Lu; Brannon, Patsy M; Lucas, Robyn M; Crump, Peter M; Cavalier, Etienne; Merkel, Joyce; Betz, Joseph M

2017-09-01

The Vitamin D Standardization Program (VDSP) coordinated a study in 2012 to assess the commutability of reference materials and proficiency testing/external quality assurance materials for total 25-hydroxyvitamin D [25(OH)D] in human serum, the primary indicator of vitamin D status. A set of 50 single-donor serum samples as well as 17 reference and proficiency testing/external quality assessment materials were analyzed by participating laboratories that used either immunoassay or LC-MS methods for total 25(OH)D. The commutability test materials included National Institute of Standards and Technology Standard Reference Material 972a Vitamin D Metabolites in Human Serum as well as materials from the College of American Pathologists and the Vitamin D External Quality Assessment Scheme. Study protocols and data analysis procedures were in accordance with Clinical and Laboratory Standards Institute guidelines. The majority of the test materials were found to be commutable with the methods used in this commutability study. These results provide guidance for laboratories needing to choose appropriate reference materials and select proficiency or external quality assessment programs and will serve as a foundation for additional VDSP studies.

A guide for the laboratory information management system (LIMS) for light stable isotopes--Versions 7 and 8

USGS Publications Warehouse

Coplen, Tyler B.

2000-01-01

The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program, the Laboratory Information Management System (LIMS) for Light Stable Isotopes, is presented herein. Major benefits of this system include (i) a dramatic improvement in quality assurance, (ii) an increase in laboratory efficiency, (iii) a reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) a decrease in errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for laboratories. LIMS for Light Stable Isotopes is available for both Microsoft Office 97 Professional and Microsoft Office 2000 Professional as versions 7 and 8, respectively. Both source code (mdb file) and precompiled executable files (mde) are available. Numerous improvements have been made for continuous flow isotopic analysis in this version (specifically 7.13 for Microsoft Access 97 and 8.13 for Microsoft Access 2000). It is much easier to import isotopic results from Finnigan ISODAT worksheets, even worksheets on which corrections for amount of sample (linearity corrections) have been added. The capability to determine blank corrections using isotope mass balance from analyses of elemental analyzer samples has been added. It is now possible to calculate and apply drift corrections to isotopic data based on the time of day of analysis. Whereas Finnigan ISODAT software is confined to using only a single peak for calculating delta values, LIMS now enables one to use the mean of two or more reference injections during a continuous flow analysis to calculate delta values. This is useful with Finnigan?s GasBench II online sample preparation system. Concentrations of carbon, nitrogen, and sulfur can be calculated based one or more isotopic reference materials analyzed with a group of samples. Both sample data and isotopic analysis data can now be exported to Excel files. A calculator for determining the amount of sample needed for isotopic analysis based on a previous amount of sample and continuous flow area is now an integral part of LIMS for Light Stable Isotopes. LIMS for Light Stable Isotopes can now assign an error code to Finnigan elemental analyzer analyses in which one of the electrometers has saturated due to analysis of too much sample material, giving rise to incorrect isotopic abundances. Information on downloading this report and downloading code and databases is provided at the Internet addresses: http://water.usgs.gov/software/geochemical.html or http://www.geogr.uni-jena.de/software/geochemical.html in the Eastern Hemisphere.

A nationwide multicentre study in Turkey for establishing reference intervals of haematological parameters with novel use of a panel of whole blood

PubMed Central

Ozarda, Yesim; Ichihara, Kiyoshi; Bakan, Ebubekir; Polat, Harun; Ozturk, Nurinnisa; Baygutalp, Nurcan K.; Taneli, Fatma; Guvenc, Yesim; Ormen, Murat; Erbayraktar, Zubeyde; Aksoy, Nurten; Sezen, Hatice; Demir, Meltem; Eskandari, Gulcin; Polat, Gurbuz; Mete, Nuriye; Yuksel, Hatice; Vatansev, Husamettin; Gun, Fatma; Akin, Okhan; Ceylan, Ozlem; Noyan, Tevfik; Gozlukaya, Ozgul; Aliyazicioglu, Yuksel; Kahraman, Sevim; Dirican, Melahat; Tuncer, Gul Ozlem; Kimura, Shogo; Eker, Pinar

2017-01-01

Introduction A nationwide multicentre study was conducted to establish well-defined reference intervals (RIs) of haematological parameters for the Turkish population in consideration of sources of variation in reference values (RVs). Materials and methods K2-EDTA whole blood samples (total of 3363) were collected from 12 laboratories. Sera were also collected for measurements of iron, UIBC, TIBC, and ferritin for use in the latent abnormal values exclusion (LAVE) method. The blood samples were analysed within 2 hours in each laboratory using Cell Dyn and Ruby (Abbott), LH780 (Beckman Coulter), or XT-2000i (Sysmex). A panel of freshly prepared blood from 40 healthy volunteers was measured in common to assess any analyser-dependent bias in the measurements. The SD ratio (SDR) based on ANOVA was used to judge the need for partitioning RVs. RIs were computed by the parametric method with/without applying the LAVE method. Results Analyser-dependent bias was found for basophils (Bas), MCHC, RDW and MPV from the panel test results and thus those RIs were derived for each manufacturer. RIs were determined from all volunteers’ results for WBC, neutrophils, lymphocytes, monocytes, eosinophils, MCV, MCH and platelets. Gender-specific RIs were required for RBC, haemoglobin, haematocrit, iron, UIBC and ferritin. Region-specific RIs were required for RBC, haemoglobin, haematocrit, UIBC, and TIBC. Conclusions With the novel use of a freshly prepared blood panel, manufacturer-specific RIs’ were derived for Bas, Bas%, MCHC, RDW and MPV. Regional differences in RIs were observed among the 7 regions of Turkey, which may be attributed to nutritional or environmental factors, including altitude. PMID:28694726

Round robin test on quantification of amyloid-β 1-42 in cerebrospinal fluid by mass spectrometry.

PubMed

Pannee, Josef; Gobom, Johan; Shaw, Leslie M; Korecka, Magdalena; Chambers, Erin E; Lame, Mary; Jenkins, Rand; Mylott, William; Carrillo, Maria C; Zegers, Ingrid; Zetterberg, Henrik; Blennow, Kaj; Portelius, Erik

2016-01-01

Cerebrospinal fluid (CSF) amyloid-β 1-42 (Aβ42) is an important biomarker for Alzheimer's disease, both in diagnostics and to monitor disease-modifying therapies. However, there is a great need for standardization of methods used for quantification. To overcome problems associated with immunoassays, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has emerged as a critical orthogonal alternative. We compared results for CSF Aβ42 quantification in a round robin study performed in four laboratories using similar sample preparation methods and LC-MS instrumentation. The LC-MS results showed excellent correlation between laboratories (r(2) >0.98), high analytical precision, and good correlation with enzyme-linked immunosorbent assay (r(2) >0.85). The use of a common reference sample further decreased interlaboratory variation. Our results indicate that LC-MS is suitable for absolute quantification of Aβ42 in CSF and highlight the importance of developing a certified reference material. Copyright © 2016 The Alzheimer's Association. Published by Elsevier Inc. All rights reserved.

Validation of powder X-ray diffraction following EN ISO/IEC 17025.

PubMed

Eckardt, Regina; Krupicka, Erik; Hofmeister, Wolfgang

2012-05-01

Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase identification. In case of the detection limit, a statistical evaluation of the signal-to-noise ratio showed that a peak criterion of three sigma is inadequate and recommendations for a more realistic peak criterion are given. Finally, the results of an international proficiency test showed the secure performance of PXRD. © 2012 American Academy of Forensic Sciences.

Comparison of two confocal micro-XRF spectrometers with different design aspects

PubMed Central

Smolek, S; Nakazawa, T; Tabe, A; Nakano, K; Tsuji, K; Streli, C; Wobrauschek, P

2014-01-01

Two different confocal micro X-ray fluorescence spectrometers have been developed and installed at Osaka City University and the Vienna University of Technology Atominstitut. The Osaka City University system is a high resolution spectrometer operating in air. The Vienna University of Technology Atominstitut spectrometer has a lower spatial resolution but is optimized for light element detection and operates under vacuum condition. The performance of both spectrometers was compared. In order to characterize the spatial resolution, a set of nine specially prepared single element thin film reference samples (500 nm in thickness, Al, Ti, Cr, Fe Ni, Cu, Zr, Mo, and Au) was used. Lower limits of detection were determined using the National Institute of Standards and Technology standard reference material glass standard 1412. A paint layer sample (cultural heritage application) and paint on automotive steel samples were analyzed with both instruments. The depth profile information was acquired by scanning the sample perpendicular to the surface. © 2013 The Authors. X-Ray Spectrometry published by John Wiley & Sons, Ltd. PMID:26430286

Comparison of two confocal micro-XRF spectrometers with different design aspects.

PubMed

Smolek, S; Nakazawa, T; Tabe, A; Nakano, K; Tsuji, K; Streli, C; Wobrauschek, P

2014-03-01

Two different confocal micro X-ray fluorescence spectrometers have been developed and installed at Osaka City University and the Vienna University of Technology Atominstitut. The Osaka City University system is a high resolution spectrometer operating in air. The Vienna University of Technology Atominstitut spectrometer has a lower spatial resolution but is optimized for light element detection and operates under vacuum condition. The performance of both spectrometers was compared. In order to characterize the spatial resolution, a set of nine specially prepared single element thin film reference samples (500 nm in thickness, Al, Ti, Cr, Fe Ni, Cu, Zr, Mo, and Au) was used. Lower limits of detection were determined using the National Institute of Standards and Technology standard reference material glass standard 1412. A paint layer sample (cultural heritage application) and paint on automotive steel samples were analyzed with both instruments. The depth profile information was acquired by scanning the sample perpendicular to the surface. © 2013 The Authors. X-Ray Spectrometry published by John Wiley & Sons, Ltd.

Multidimensional Analysis of Curved Root Canal Preparation Using Continuous or Reciprocating Nickel-titanium Instruments

PubMed Central

Mamede-Neto, Iussif; Borges, Álvaro Henrique; Alencar, Ana Helena Gonçalves; Duarte, Marco Antonio Hungaro; Sousa Neto, Manoel Damião; Estrela, Carlos

2018-01-01

Objective: To evaluate transportation (T) and centering ability (CA) of root canal preparations using continuous or reciprocating nickel-titanium endodontic files. Materials and Methods: Ninety-six mesiobuccal root canals of mandibular first and second molars were randomly divided into 6 groups (n=16) according to the rotary file used: 1. ProTaper Next; 2. ProTaper Gold; 3. Mtwo; 4. BioRaCe; 5. WaveOne Gold; 6. Reciproc. Root canals were prepared according to manufacturer’s instructions. Cone beam computed tomography scans were obtained before and after root canal preparation. Measurements were made at six different reference points: 2, 3 and 4 mm from the apex and 2, 3 and 4 mm below furcation in different directions. Results: The greatest Mesiodistal (MD) Transportation (T) was found for Reciproc files (p<0.05), and the greatest buccolingual (BL) T, for Reciproc, ProTaper Gold and ProTaper Next files (p<0.05). The greatest Mesiodistal (MD) Centering Ability (CA) was found for BioRaCe files (p<0.05), and the greatest Buccolingual (BL) CA, for BioRaCe and Mtwo files (p<0.05). Conclusion: All systems produced root canal transportation. No file system achieved perfect CA of root preparation. Reciproc files had the greatest MD T and BL T. BioRaCe files had the greatest MD CA, whereas BL CA was similar for BioRaCe and Mtwo files. PMID:29456772

Evaluation of droplet digital PCR for characterizing plasmid reference material used for quantifying ammonia oxidizers and denitrifiers.

PubMed

Dong, Lianhua; Meng, Ying; Wang, Jing; Liu, Yingying

2014-02-01

DNA reference materials of certified value have a critical function in many analytical processes of DNA measurement. Quantification of amoA genes in ammonia oxidizing bacteria (AOB) and archaea (AOA), and of nirS and nosZ genes in the denitrifiers is very important for determining their distribution and abundance in the natural environment. A plasmid reference material containing nirS, nosZ, amoA-AOB, and amoA-AOA is developed to provide a DNA standard with copy number concentration for ensuring comparability and reliability of quantification of these genes. Droplet digital PCR (ddPCR) was evaluated for characterization of the plasmid reference material. The result revealed that restriction endonuclease digestion of plasmids can improve amplification efficiency and minimize the measurement bias of ddPCR. Compared with the conformation of the plasmid, the size of the DNA fragment containing the target sequence and the location of the restriction site relative to the target sequence are not significant factors affecting plasmid quantification by ddPCR. Liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) was used to provide independent data for quantifying the plasmid reference material. The copy number concentration of the digested plasmid determined by ddPCR agreed well with that determined by LC-IDMS, improving both the accuracy and reliability of the plasmid reference material. The reference value, with its expanded uncertainty (k = 2), of the plasmid reference material was determined to be (5.19 ± 0.41) × 10(9) copies μL(-1) by averaging the results of two independent measurements. Consideration of the factors revealed in this study can improve the reliability and accuracy of ddPCR; thus, this method has the potential to accurately quantify DNA reference materials.

49 CFR 572.30 - Incorporated materials.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 49 Transportation 7 2011-10-01 2011-10-01 false Incorporated materials. 572.30 Section 572.30....30 Incorporated materials. (a) The drawings and specifications referred to in this regulation that... Federal Register has approved the materials incorporated by reference. For materials subject to change...

49 CFR 572.30 - Incorporated materials.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 49 Transportation 7 2010-10-01 2010-10-01 false Incorporated materials. 572.30 Section 572.30....30 Incorporated materials. (a) The drawings and specifications referred to in this regulation that... Federal Register has approved the materials incorporated by reference. For materials subject to change...

49 CFR 572.30 - Incorporated materials.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 49 Transportation 7 2012-10-01 2012-10-01 false Incorporated materials. 572.30 Section 572.30....30 Incorporated materials. (a) The drawings and specifications referred to in this regulation that... Federal Register has approved the materials incorporated by reference. For materials subject to change...

49 CFR 572.30 - Incorporated materials.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 49 Transportation 7 2013-10-01 2013-10-01 false Incorporated materials. 572.30 Section 572.30....30 Incorporated materials. (a) The drawings and specifications referred to in this regulation that... Federal Register has approved the materials incorporated by reference. For materials subject to change...

Application of ionic liquid for extraction and separation of bioactive compounds from plants.

PubMed

Tang, Baokun; Bi, Wentao; Tian, Minglei; Row, Kyung Ho

2012-09-01

In recent years, ionic liquids (ILs), as green and designer solvents, have accelerated research in analytical chemistry. This review highlights some of the unique properties of ILs and provides an overview of the preparation and application of IL or IL-based materials to extract bioactive compounds in plants. IL or IL-based materials in conjunction with liquid-liquid extraction (LLE), ultrasonic-assisted extraction (UAE), microwave-assisted extraction (MAE), high performance liquid chromatography (HPLC) and solid-phase extraction (SPE) analytical technologies etc., have been applied successfully to the extraction or separation of bioactive compounds from plants. This paper reviews the available data and references to examine the advantages of IL and IL-based materials in these applications. In addition, the main target compounds reviewed in this paper are bioactive compounds with multiple therapeutic effects and pharmacological activities. Based on the importance of the targets, this paper reviews the applications of ILs, IL-based materials or co-working with analytical technologies. The exploitation of new applications of ILs on the extraction of bioactive compounds from plant samples is expected to increase. Copyright © 2012 Elsevier B.V. All rights reserved.

Changes in chroma of two indirect composite materials polymerized with different polymerization systems.

PubMed

Ayano, Michiya

2012-01-01

This study evaluated chroma change in two composite materials (Sinfony and Pearleste) polymerized with two different systems. Disk specimens were prepared using a metal halide unit (Hyper LII) and an exposure time of 60 to 180 s. The proprietary polymerization systems (Visio and Pearlcure systems) were used as the reference polymerization modes. After storage at 37°C for 24 h, CIE 1976 L*a*b* values were measured by using a dental chroma meter (ShadeEye NCC) with a gray background. The specimens were then immersed in water or tea. Color change from baseline to 4 weeks was evaluated by measuring ΔL*, Δa*, and Δb*, after which ΔE*(ab) values were calculated. The brightness of Sinfony specimens was reduced by tea immersion. The color of both materials shifted to yellow after tea immersion, although color change in Sinfony specimens was greater than that in Pearleste specimens. For both materials, color change was less after polymerization with the metal halide unit. In conclusion, Sinfony polymerized with the Hyper LII unit, and Pearleste polymerized with either system, were stable against discoloration due to tea immersion.

Calibrated sulfur isotope abundance ratios of three IAEA sulfur isotope reference materials and V-CDT with a reassessment of the atomic weight of sulfur

NASA Astrophysics Data System (ADS)

Ding, T.; Valkiers, S.; Kipphardt, H.; De Bièvre, P.; Taylor, P. D. P.; Gonfiantini, R.; Krouse, R.

2001-08-01

Calibrated values have been obtained for sulfur isotope abundance ratios of sulfur isotope reference materials distributed by the IAEA (Vienna). For the calibration of the measurements, a set of synthetic isotope mixtures were prepared gravimetrically from high purity Ag2S materials enriched in32S, 33S, and 34S. All materials were converted into SF6 gas and subsequently, their sulfur isotope ratios were measured on the SF5+ species using a special gas source mass spectrometer equipped with a molecular flow inlet system (IRMM's Avogadro II amount comparator). Values for the 32S/34S abundance ratios are 22.650 4(20), 22.142 4(20), and 23.393 3(17) for IAEA-S-1, IAEA-S-2, and IAEA-S-3, respectively. The calculated 32S/34S abundance ratio for V-CDT is 22.643 6(20), which is very close to the calibrated ratio obtained by Ding et al. (1999). In this way, the zero point of the VCDT scale is anchored firmly to the international system of units SI. The 32S/33S abundance ratios are 126.942(47), 125.473(55), 129.072(32), and 126.948(47) for IAEA-S-1, IAEA-S-2, IAEA-S-3, and V-CDT, respectively. In this way, the linearity of the V-CDT scale is improved over this range. The values of the sulfur molar mass for IAEA-S-1 and V-CDT were calculated to be 32.063 877(56) and 32.063 911(56), respectively, the values with the smallest combined uncertainty ever reported for the sulfur molar masses (atomic weights).

Development of Argon Isotope Reference Standards for the U.S. Geological Survey

PubMed Central

Miiller, Archie P.

2006-01-01

The comparison of physical ages of geological materials measured by laboratories engaged in geochronological studies has been limited by the accuracy of mineral standards or monitors for which reported ages have differed by as much as 2 %. In order to address this problem, the U.S. Geological Survey is planning to calibrate the conventional 40Ar/40K age of a new preparation of an international hornblende standard labeled MMhb-2. The 40K concentration in MMhb-2 has already been determined by the Analytical Chemistry Division at NIST with an uncertainty of 0.2 %. The 40Ar concentration will be measured by the USGS using the argon isotope reference standards that were recently developed by NIST and are described in this paper. The isotope standards were constructed in the form of pipette/reservoir systems and calibrated by gas expansion techniques to deliver small high-precision aliquots of high-purity argon. Two of the pipette systems will deliver aliquots of 38Ar having initial molar quantities of 1.567 × 10−10 moles and 2.313 × 10−10 moles with expanded (k = 2) uncertainties of 0.058 % and 0.054 %, respectively. Three other pipette systems will deliver aliquots (nominally 4 × 10−10 moles) of 40Ar:36Ar artificial mixtures with similar accuracy and with molar ratios of 0.9974 ± 0.06 %, 29.69 ± 0.06 %, and 285.7 ± 0.08 % (k = 2). These isotope reference standards will enable the USGS to measure the 40Ar concentration in MMhb-2 with an expanded uncertainty of ≈ 0.1 %. In the process of these measurements, the USGS will re-determine the isotopic composition of atmospheric Ar and calculate a new value for its atomic weight. Upon completion of the USGS calibrations, the MMhb-2 mineral standard will be certified by NIST for its K and Ar concentrations and distributed as a Standard Reference Material (SRM). The new SRM and the NIST-calibrated transportable pipette systems have the potential for dramatically improving the accuracy of interlaboratory calibrations and thereby the measured ages of geological materials, by as much as a factor of ten. PMID:27274937

Towards absolute quantification of allergenic proteins in food--lysozyme in wine as a model system for metrologically traceable mass spectrometric methods and certified reference materials.

PubMed

Cryar, Adam; Pritchard, Caroline; Burkitt, William; Walker, Michael; O'Connor, Gavin; Burns, Duncan Thorburn; Quaglia, Milena

2013-01-01

Current routine food allergen quantification methods, which are based on immunochemistry, offer high sensitivity but can suffer from issues of specificity and significant variability of results. MS approaches have been developed, but currently lack metrological traceability. A feasibility study on the application of metrologically traceable MS-based reference procedures was undertaken. A proof of concept involving proteolytic digestion and isotope dilution MS for quantification of protein allergens in a food matrix was undertaken using lysozyme in wine as a model system. A concentration of lysozyme in wine of 0.95 +/- 0.03 microg/g was calculated based on the concentrations of two peptides, confirming that this type of analysis is viable at allergenically meaningful concentrations. The challenges associated with this promising method were explored; these included peptide stability, chemical modification, enzymatic digestion, and sample cleanup. The method is suitable for the production of allergen in food certified reference materials, which together with the achieved understanding of the effects of sample preparation and of the matrix on the final results, will assist in addressing the bias of the techniques routinely used and improve measurement confidence. Confirmation of the feasibility of MS methods for absolute quantification of an allergenic protein in a food matrix with results traceable to the International System of Units is a step towards meaningful comparison of results for allergen proteins among laboratories. This approach will also underpin risk assessment and risk management of allergens in the food industry, and regulatory compliance of the use of thresholds or action levels when adopted.

40 CFR Table 3 to Subpart Uuuu of... - Initial Compliance With Emission Limits and Work Practice Standards

Code of Federal Regulations, 2010 CFR

2010-07-01

... uncontrolled total sulfide emissions were reduced by at least 25%; (3) you prepare a material balance that... reduced by at least 75%; (3) you prepare a material balance that includes the pertinent data used to... emissions were reduced by at least 35%; (3) you prepare a material balance that includes the pertinent data...

40 CFR Table 3 to Subpart Uuuu of... - Initial Compliance With Emission Limits and Work Practice Standards

Code of Federal Regulations, 2011 CFR

2011-07-01

... uncontrolled total sulfide emissions were reduced by at least 25%; (3) you prepare a material balance that... reduced by at least 75%; (3) you prepare a material balance that includes the pertinent data used to... emissions were reduced by at least 35%; (3) you prepare a material balance that includes the pertinent data...

NASA/USRA University advanced design program

NASA Technical Reports Server (NTRS)

Lembeck, Michael F.; Prussing, John

1989-01-01

The participation of the University of Illinois at Urbana-Champaign in the NASA/USRA University Advanced Design Program for the 1988 to 1989 academic year is reviewed. The University's design project was the Logistics Resupply and Emergency Crew Return System for Space Station Freedom. Sixty-one students divided into eight groups, participated in the spring 1989 semester. A presentation prepared by three students and a graduate teaching assistant for the program's summer conference summarized the project results. Teamed with the NASA Marshall Space Flight Center (MSFC), the University received support in the form of remote telecon lectures, reference material, and previously acquired applications software. In addition, a graduate teaching assistant was awarded a summer 1989 internship at MSFC.

Heat-assisted aqueous extraction of rice flour for arsenic speciation analysis.

PubMed

Narukawa, Tomohiro; Chiba, Koichi

2010-07-28

A versatile heat-assisted pretreatment aqueous extraction method for the analysis of arsenic species in rice was developed. Rice flour certified reference materials NIST SRM1568a and NMIJ CRM 7503-a and a flour made from polished rice were used as samples, and HPLC-ICP-MS was employed for the determination of arsenic species. Arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) were detected in NIST SRM, and As(III), As(V) and DMAA were found in NMIJ CRM and the prepared polished rice flour. The sums of the concentrations of all species in each rice flour sample were 97-102% of the total arsenic concentration in each sample.

Effect of Pt Nanoparticles on the Photocatalytic Activity of ZnO Nanofibers

NASA Astrophysics Data System (ADS)

Di Mauro, Alessandro; Zimbone, Massimo; Scuderi, Mario; Nicotra, Giuseppe; Fragalà, Maria Elena; Impellizzeri, Giuliana

2015-12-01

For this study, we originally realized ZnO nanofibers (˜50 nm in mean radius) mixed with Pt nanoparticles (˜30 nm in mean radius), prepared by pulsed laser ablation in liquid, and investigated their photocatalytic performance. The material was synthesized by the simple electrospinning method coupled with subsequent thermal treatments. Methylene blue was employed as a representative dye pollutant to evaluate the photocatalytic activity of the nanofibers. It was found that the Pt-ZnO fibers exhibit a photodegradation reaction rate that is ˜40 % higher than the one obtained for reference ZnO fibers. These encouraging results demonstrate that Pt-ZnO nanofibers can be fruitfully applied for environmental applications.

Improved infiltration series for studying stomatal opening as illustrated with coffee

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

Alvim, P.deT.; Havis, J.R.

1956-01-01

Very satisfactory results have been obtained in estimation of the degree of stomatal opening of several plant species by using infiltration series prepared with Nujol mineral oil diluted with xylol, kerosene, n-dodecane, n-tetradecane, or Bayol-D. All of these materials, except Nujol, infiltrate the leaves when the stomata are only slightly open. Nujol does not penetrate even wide open stomata, except for plants with particularly large stomata. The results with coffee plants show that leaves exposed to direct sunlight decreased their stomatal aperture during periods of strong illumination in the middle of the day (more than about 8000 fc). 9 references,more » 2 figures.« less

Skylab Saturn 1B flight manual

NASA Technical Reports Server (NTRS)

1972-01-01

A Saturn 1B Flight Manual provides launch vehicle systems descriptions and predicted performance data for the Skylab missions. Vehicle SL-2 (SA-206) is the baseline for this manual; but, as a result of the great similarity, the material is representative of SL-3 and SL-4 launch vehicles, also. The Flight Manual is not a control document but is intended primarily as an aid to astronauts who are training for Skylab missions. In order to provide a comprehensive reference for that purpose, the manual also contains descriptions of the ground support interfaces, prelaunch operations, and emergency procedures. Mission variables and constraints are summarized, and mission control monitoring and data flow during launch preparation and flight are discussed.

A new procedure to produce lignocellulosic anion exchangers from agricultural waste materials.

PubMed

Orlando, U S; Baes, A U; Nishijima, W; Okada, M

2002-07-01

Two lignocellulosic agricultural waste materials (LCM), sugarcane bagasse (BG) and rice hull (RH), were converted into weak-base anion exchanger and evaluated for their exchanger capacity for nitrate. Pure cellulose (PC) and pure alkaline lignin (PL) were also used as reference materials to elucidate possible reactivity in LCM. Epoxy and amino groups were introduced into BG, RH, PC and PL substrates after the reaction with epichlorohydrin and dimethylamine in the presence of pyridine and an organic solvent N,N-dimethylformamide (DMF). Amino group incorporation into cellulose decreased with the presence of water in the reaction mixture and increased with the reaction time and presence of a catalyst (pyridine). The highest maximum nitrate exchange capacity (Qmax) and yields of the prepared exchangers was obtained from PL (1.8 mmol g(-1) and 412.5%), followed by BG (1.41 mmol g(-1) and 300%), PC (1.34 mmol g(-1) and 166%) and RH (1.32 mmol g(-1) and 180%). The proposed synthetic procedure was effective in modifying PL, PC and LCM chemically resulting in a higher yield and nitrate removal capacity.

A Comparison of US and Japanese Dental Restorative Care Present on Service Members Recovered from the WWII Era.

PubMed

Shiroma, Calvin Y

2017-11-01

The documentation of dental materials used in the USA during the WWII era is readily available, while references for the Japanese are minimal. It was therefore important to build a photographic database of Japanese restorative care which could be utilized as a comparison tool for the deployed odontologist. The dental restorative care of approximately 400 US and 100 Japanese sets of remains was evaluated. Both countries share many similar restorative techniques to include collared crowns, full-coverage restorations, cantilever bridge/pontics to close spaces; restorative materials such as amalgam, gold, and zinc phosphate (temporary) restorations; and removable prostheses. The dental restorative materials most commonly used by US dentists include the amalgam and silicate cement, while the full-coverage crown was the type of restoration most frequently seen on the Japanese remains. Silicates, porcelain and replaceable crowns, and partial-coverage prepared crowns were not observed on the recovered Japanese remains. Published 2017. This article is a U.S. Government work and is in the public domain in the USA.

Environment and human friendly colored materials prepared using black and white components.

PubMed

Takeoka, Yukikazu

2018-05-10

Our lives in the present age are full of colorful items. However, when many coloring materials cannot be used due to environmental concerns, this colorful life that has been constructed will be diminished. Maintaining our rich lifestyle necessitates the development of technologies that can make safe and secure color materials from materials with less burden on people and the environment. Herein, the author reveals that structural colored materials with little angle dependence can be prepared using various materials with short-range order in the refractive index, which is comparable to the wavelength of visible light, and with the aid of a black substance. This approach enables the preparation of colorful materials from materials that have a low environmental burden and are non-toxic to living things; examples of such materials include silica, carbon black, and iron oxide. If we can achieve mechanical stabilization and hue stabilization of these coloring materials, we can develop new green pigments with low toxicity, good color development, and high durability. The use of conventional angular-dependent structural colored materials has been limited. However, structural colored materials with no angle dependence, such as those prepared by the author, can be used in fields where pigments have traditionally been used. For example, they could be used in coating materials for automobiles and buildings, and in pigments used by artists. Environmentally friendly green color materials are expected to promote sustainable development. In this review, I will describe how to prepare structural colored materials with less angle dependency using white and black substances previously reported by the author.

[Studies on the identification of psychotropic substances. VIII. Preparation and various analytical data of reference standard of some stimulants, amfepramone, cathinone, N-ethylamphetamine, fenethylline, fenproporex and mefenorex].

PubMed

Shimamine, M; Takahashi, K; Nakahara, Y

1992-01-01

The Reference Standards for amfepramone, cathinone, N-ethylamphetamine, fenethylline, fenproporex and mefenorex were prepared. Their purities determined by HPLC were more than 99.5%. For the identification and determination of these six drugs, their analytical data were measured and discussed by TLC, UV, IR, HPLC, GC/MS and NMR.

History of reference materials for food and nutrition metrology: As represented in the series of BERM Symposia

USDA-ARS?s Scientific Manuscript database

Establishment of a metrology-based measurement system requires the solid foundation of traceability of measurements to available, appropriate certified reference materials (CRM). In the early 1970s the first “biological” Reference Material (RM) of Bowens Kale, Orchard Leaves, and Bovine Liver from ...

40 CFR 89.6 - Reference materials.

Code of Federal Regulations, 2010 CFR

2010-07-01

... set forth the material that has been incorporated by reference in this part. (1) ASTM material. The... 19428-2959. Document number and name 40 CFR part 89 reference ASTM D86-97: “Standard Test Method for Distillation of Petroleum Products at Atmospheric Pressure” Appendix A to Subpart D. ASTM D93-97: “Standard...

National Nutrition Education Clearing House Reference List, Secondary Teaching Materials and Teacher References.

ERIC Educational Resources Information Center

National Nutrition Education Clearing House, Berkeley, CA.

A reference list of teaching materials and teacher guides in the field of nutrition is compiled in this pamphlet. Primary emphasis is on resources for secondary grades. The section on teaching materials includes books, pamphlets, leaflets, posters, charts, transparencies, ditto masters, kits, games, films, filmstrips, records, TV videotapes, and…