WorldWideScience

Sample records for atomic weight determinations

  1. The role of mass spectrometry in atomic weight determinations.

    Science.gov (United States)

    De Laeter, John R

    2009-01-01

    The 1914 Nobel Prize for Chemistry was awarded to Theodore Richards, whose work provided an insight into the history of the birth and evolution of matter as embedded in the atomic weights. However, the secret to unlocking the hieroglyphics contained in the atomic weights is revealed by a study of the relative abundances of the isotopes. A consistent set of internationally accepted atomic weights has been a goal of the scientific community for over a century. Atomic weights were originally determined by chemical stoichiometry--the so-called "Harvard Method," but this methodology has now been superseded by the "physical method," in which the isotopic composition and atomic masses of the isotopes comprising an element are used to calculate the atomic weight with far greater accuracy than before. The role of mass spectrometry in atomic weight determinations was initiated by the discovery of isotopes by Thomson, and established by the pioneering work of Aston, Dempster, and Nier using sophisticated mass spectrographs. The advent of the sector field mass spectrometer in 1947, revolutionized the application of mass spectrometry for both solids and gases to other fields of science including atomic weights. Subsequently, technological advances in mass spectrometry have enabled atomic masses to be determined with an accuracy better than one part in 10(7), whilst the absolute isotopic composition of many elements has been determined to produce accurate values of their atomic weights. Conversely, those same technological developments have revealed significant variations in the isotope abundances of many elements caused by a variety of physiochemical mechanisms in natural materials. Although these variations were initially seen as an impediment to the accuracy with which atomic weights could be determined, it was quickly realized that nature had provided a new tool to investigate physiochemical and biogeochemical mechanisms in nature, which could be exploited by precise and

  2. THE ATOMIC WEIGHTS COMMISSION AND ISOTOPIC ABUNDANCE RATIO DETERMINATIONS.

    Energy Technology Data Exchange (ETDEWEB)

    HOLDEN, N.E.

    2005-08-07

    Following Thomson's discovery of stable isotopes in non-radioactive chemical elements, the derivation of atomic weight values from mass spectrometric measurements of isotopic abundance ratios moved very slowly. Forty years later, only 3 1/2 % of the recommended values were based on mass spectrometric measurements and only 38% in the first half century. It might be noted that two chemical elements (tellurium and mercury) are still based on chemical measurements, where the atomic weight value calculated from the relative isotopic abundance measurement either agrees with the value from the chemical measurement or the atomic weight value calculated from the relative isotopic abundance measurement falls within the uncertainty of the chemical measurement of the atomic weight. Of the 19 chemical elements, whose atomic weight is based on non-corrected relative isotopic abundance measurements, five of these are two isotope systems (indium, iridium, lanthanum, lutetium and tantalum) and one is a three-isotope system (oxygen).

  3. Atomic Weights and Isotopic Compositions

    Science.gov (United States)

    SRD 144 Atomic Weights and Isotopic Compositions (Web, free access)   The atomic weights are available for elements 1 through 111, and isotopic compositions or abundances are given when appropriate.

  4. On the atomic masses (weights?) Of the elements

    OpenAIRE

    Kaptay G.

    2012-01-01

    Atomic masses (weights?) is an essential information for mining and metallurgy. The paper discusses four subjects around this problem. First, the classification of all the elements is suggested into 4 classes, based on their isotope features, determining the accuracy of their known atomic masses. As part of that, the class of elements is discussed with uncertain atomic weights in accordance with the 2009 IUPAC recommendations. A better (easier to use) format of atomic weights is present...

  5. Clarifying Atomic Weights: A 2016 Four-Figure Table of Standard and Conventional Atomic Weights

    Science.gov (United States)

    Coplen, Tyler B.; Meyers, Fabienne; Holden, Norman E.

    2017-01-01

    To indicate that atomic weights of many elements are not constants of nature, in 2009 and 2011 the Commission on Isotopic Abundances and Atomic Weights (CIAAW) of the International Union of Pure and Applied Chemistry (IUPAC) replaced single-value standard atomic weight values with atomic weight intervals for 12 elements (hydrogen, lithium, boron,…

  6. Clarifying atomic weights: A 2016 four-figure table of standard and conventional atomic weights

    Science.gov (United States)

    Coplen, Tyler B.; Meyers, Fabienne; Holden, Norman E.

    2017-01-01

    To indicate that atomic weights of many elements are not constants of nature, in 2009 and 2011 the Commission on Isotopic Abundances and Atomic Weights (CIAAW) of the International Union of Pure and Applied Chemistry (IUPAC) replaced single-value standard atomic weight values with atomic weight intervals for 12 elements (hydrogen, lithium, boron, carbon, nitrogen, oxygen, magnesium, silicon, sulfur, chlorine, bromine, and thallium); for example, the standard atomic weight of nitrogen became the interval [14.00643, 14.00728]. CIAAW recognized that some users of atomic weight data only need representative values for these 12 elements, such as for trade and commerce. For this purpose, CIAAW provided conventional atomic weight values, such as 14.007 for nitrogen, and these values can serve in education when a single representative value is needed, such as for molecular weight calculations. Because atomic weight values abridged to four figures are preferred by many educational users and are no longer provided by CIAAW as of 2015, we provide a table containing both standard atomic weight values and conventional atomic weight values abridged to four figures for the chemical elements. A retrospective review of changes in four-digit atomic weights since 1961 indicates that changes in these values are due to more accurate measurements over time or to the recognition of the impact of natural isotopic fractionation in normal terrestrial materials upon atomic weight values of many elements. Use of the unit “u” (unified atomic mass unit on the carbon mass scale) with atomic weight is incorrect because the quantity atomic weight is dimensionless, and the unit “amu” (atomic mass unit on the oxygen scale) is an obsolete term: Both should be avoided.

  7. Atomic weights of the elements 2011 (IUPAC Technical Report)

    Science.gov (United States)

    Wieser, Michael E.; Holden, Norman; Coplen, Tyler B.; Böhlke, John K.; Berglund, Michael; Brand, Willi A.; De Bièvre, Paul; Gröning, Manfred; Loss, Robert D.; Meija, Juris; Hirata, Takafumi; Prohaska, Thomas; Schoenberg, Ronny; O'Connor, Glenda; Walczyk, Thomas; Yoneda, Shige; Zhu, Xiang-Kun

    2013-01-01

    The biennial review of atomic-weight determinations and other cognate data has resulted in changes for the standard atomic weights of five elements. The atomic weight of bromine has changed from 79.904(1) to the interval [79.901, 79.907], germanium from 72.63(1) to 72.630(8), indium from 114.818(3) to 114.818(1), magnesium from 24.3050(6) to the interval [24.304, 24.307], and mercury from 200.59(2) to 200.592(3). For bromine and magnesium, assignment of intervals for the new standard atomic weights reflects the common occurrence of variations in the atomic weights of those elements in normal terrestrial materials.

  8. Atomic weights: no longer constants of nature

    Science.gov (United States)

    Coplen, Tyler B.; Holden, Norman E.

    2011-01-01

    Many of us were taught that the standard atomic weights we found in the back of our chemistry textbooks or on the Periodic Table of the Chemical Elements hanging on the wall of our chemistry classroom are constants of nature. This was common knowledge for more than a century and a half, but not anymore. The following text explains how advances in chemical instrumentation and isotopic analysis have changed the way we view atomic weights and why they are no longer constants of nature

  9. Atomic weights of the elements 2009 (IUPAC technical report)

    Science.gov (United States)

    Wieser, M.E.; Coplen, T.B.

    2011-01-01

    The biennial review of atomic-weight determinations and other cognate data has resulted in changes for the standard atomic weights of 11 elements. Many atomic weights are not constants of nature, but depend upon the physical, chemical, and nuclear history of the material. The standard atomic weights of 10 elements having two or more stable isotopes have been changed to reflect this variability of atomic-weight values in natural terrestrial materials. To emphasize the fact that these standard atomic weights are not constants of nature, each atomic-weight value is expressed as an interval. The interval is used together with the symbol [a; b] to denote the set of atomic-weight values, Ar(E), of element E in normal materials for which a ≤ Ar(E) ≤ b. The symbols a and b denote the bounds of the interval [a; b]. The revised atomic weight of hydrogen, Ar(H), is [1.007 84; 1.008 11] from 1.007 94(7); lithium, Ar(Li), is [6.938; 6.997] from 6.941(2); boron, Ar(B), is [10.806; 10.821] from 10.811(7); carbon, Ar(C), is [12.0096; 12.0116] from 12.0107(8); nitrogen, Ar(N), is [14.006 43; 14.007 28] from 14.0067(2); oxygen, Ar(O), is [15.999 03; 15.999 77] from 15.9994(3); silicon, Ar(Si), is [28.084; 28.086] from 28.0855(3); sulfur, Ar(S), is [32.059; 32.076] from 32.065(2); chlorine, Ar(Cl), is [35.446; 35.457] from 35.453(2); and thallium, Ar(Tl), is [204.382; 204.385] from 204.3833(2). This fundamental change in the presentation of the atomic weights represents an important advance in our knowledge of the natural world and underscores the significance and contributions of chemistry to the well-being of humankind in the International Year of Chemistry 2011. The standard atomic weight of germanium, Ar(Ge), was also changed to 72.63(1) from 72.64(1).

  10. Atomic weights of the elements 2013 (IUPAC Technical Report)

    Science.gov (United States)

    Meija, Juris; Coplen, Tyler B.; Berglund, Michael; Brand, Willi A.; De Bièvre, Paul; Gröning, Manfred; Holden, Norman E.; Irrgeher, Johanna; Loss, Robert D.; Walczyk, Thomas; Prohaska, Thomas

    2016-01-01

    The biennial review of atomic-weight determinations and other cognate data has resulted in changes for the standard atomic weights of 19 elements. The standard atomic weights of four elements have been revised based on recent determinations of isotopic abundances in natural terrestrial materials:cadmium to 112.414(4) from 112.411(8),molybdenum to 95.95(1) from 95.96(2),selenium to 78.971(8) from 78.96(3), andthorium to 232.0377(4) from 232.038 06(2). The Commission on Isotopic Abundances and Atomic Weights (ciaaw.org) also revised the standard atomic weights of fifteen elements based on the 2012 Atomic Mass Evaluation:aluminium (aluminum) to 26.981 5385(7) from 26.981 5386(8),arsenic to 74.921 595(6) from 74.921 60(2),beryllium to 9.012 1831(5) from 9.012 182(3),caesium (cesium) to 132.905 451 96(6) from 132.905 4519(2),cobalt to 58.933 194(4) from 58.933 195(5),fluorine to 18.998 403 163(6) from 18.998 4032(5),gold to 196.966 569(5) from 196.966 569(4),holmium to 164.930 33(2) from 164.930 32(2),manganese to 54.938 044(3) from 54.938 045(5),niobium to 92.906 37(2) from 92.906 38(2),phosphorus to 30.973 761 998(5) from 30.973 762(2),praseodymium to 140.907 66(2) from 140.907 65(2),scandium to 44.955 908(5) from 44.955 912(6),thulium to 168.934 22(2) from 168.934 21(2), andyttrium to 88.905 84(2) from 88.905 85(2). The Commission also recommends the standard value for the natural terrestrial uranium isotope ratio, N(238U)/N(235U)=137.8(1).

  11. What determines hatchling weight: breeder age or incubated egg weight?

    Directory of Open Access Journals (Sweden)

    AB Traldi

    2011-12-01

    Full Text Available Two experiments were carried out to determine which factor influences weight at hatch of broiler chicks: breeder age or incubated egg weight. In Experiment 1, 2340 eggs produced by 29- and 55-week-old Ross® broiler breeders were incubated. The eggs selected for incubation weighed one standard deviation below and above average egg weight. In Experiment 2, 2160 eggs weighing 62 g produced by breeders of both ages were incubated. In both experiments, 50 additional eggs within the weight interval determined for each breeder age were weighed, broken, and their components were separated and weighed. At hatch, hatchlings were sexed and weighed, determining the average initial weight of the progeny of each breeder age. Data were analyzed using the Analyst program of SAS® software package. In Experiment 1, the weight difference between eggs produced by young and mature breeders was 10.92 g, and the component that mostly influenced this difference was the yolk (7.51 g heavier in mature breeders, compared with 4.23 g difference in albumen and 0.8 g in eggshell weights. Hatchling weight difference was 9.4 g higher in eggs from mature breeders. In Experiment 2, egg weight difference was only 0.74 g, but yolk weight was 4.59 g higher in the eggs of mature breeders. The results obtained in the present study indicate that hatchling weight is influenced by egg weight, and not by breeder age.

  12. RADIOACTIVE ELEMENTS IN THE STANDARD ATOMIC WEIGHTS TABLE

    Energy Technology Data Exchange (ETDEWEB)

    Holden, N.E.; Holden, N.; Holden,N.E.

    2011-07-27

    In the 1949 Report of the Atomic Weights Commission, a series of new elements were added to the Atomic Weights Table. Since these elements had been produced in the laboratory and were not discovered in nature, the atomic weight value of these artificial products would depend upon the production method. Since atomic weight is a property of an element as it occurs in nature, it would be incorrect to assign an atomic weight value to that element. As a result of that discussion, the Commission decided to provide only the mass number of the most stable (or longest-lived) known isotope as the number to be associated with these entries in the Atomic Weights Table. As a function of time, the mass number associated with various elements has changed as longer-lived isotopes of a particular element has been found in nature, or as improved half-life values of an element's isotopes might cause a shift in the longest-lived isotope from one mass to another. In the 1957 Report of the Atomic Weights Commission, it was decided to discontinue the listing of the mass number in the Atomic Weights Table on the grounds that the kind of information supplied by the mass number is inconsistent with the primary purpose of the Table, i.e., to provide accurate values of 'these constants' for use in various chemical calculations. In addition to the Table of Atomic Weights, the Commission included an auxiliary Table of Radioactive Elements for the first time, where the entry would be the isotope of that element which was the most stable, i.e., the one with the longest known half-life. In their 1973 Report, the Commission noted that the users of the main Table of Atomic Weights were dissatisfied with the omission of values for some elements in that Table and it was decided to reintroduce the mass number for the radioactive elements into the main Table. In their 1983 Report, the Commission decided that radioactive elements were considered to lack a characteristic terrestrial

  13. Determinants of weighted path matrices

    CERN Document Server

    Talaska, Kelli

    2012-01-01

    We find rational expressions for all minors of the weighted path matrix of a directed graph, generalizing the classical Lindstrom/Gessel-Viennot result for acyclic directed graphs. The formulas are given in terms of certain flows in the graph.

  14. Weight Maintenance: Determinants of Success

    Science.gov (United States)

    2005-12-15

    submitted in partial fulfillment of the requirements for the degree of MASTER OF DIETETIC ADMINISTRATION In Nutrition and Food Sciences Approved: Tamara...Determinants Of Success by Cynthia Mitchell, Master of Dietetic Administration Utah State University, 2005 Major Professor: Tamara Vitale Department...a concern. Current data suggest that these foods are often higher in energy, fat and sodium, but deficient in fiber , vitamins A and C and folate

  15. Determinants of weight regain after bariatric surgery.

    Science.gov (United States)

    Bastos, Emanuelle Cristina Lins; Barbosa, Emília Maria Wanderley Gusmão; Soriano, Graziele Moreira Silva; dos Santos, Ewerton Amorim; Vasconcelos, Sandra Mary Lima

    2013-01-01

    Bariatric surgery leads to an average loss of 60-75% of excess body weight with maximum weight loss in the period between 18 and 24 months postoperatively. However, several studies show that weight is regained from two years of operation. To identify the determinants of weight regain in post-bariatric surgery users. Prospective cross-sectional study with 64 patients who underwent bariatric surgery with postoperative time > 2 years valued at significant weight regain. The variables analyzed were age, sex, education, socioeconomic status, work activity related to food, time after surgery, BMI, percentage of excess weight loss, weight gain, attendance monitoring nutrition, lifestyle, eating habits, self-perception of appetite, daily use of nutritional supplements and quality of life. There were 57 (89%) women and 7 (11%) men, aged 41.76 ± 7.93 years and mean postoperative period of 53.4 ± 18.4 months. The average weight and BMI were respectively 127.48 ± 24.2 kg and 49.56 ± 6.7 kg/m2 at surgery. The minimum weight and BMI were achieved 73.0 ± 18.6 kg and 28.3 ± 5.5 kg/m2, reached in 23.7 ± 12 months postoperatively. Regained significant weight occurred in 18 (28.1%) cases. The mean postoperative period of 66 ± 8.3 months and work activities related to food showed statistical significance (p=000 and p=0.003) for the regained weight. Bariatric surgery promotes adequate reduction of excess body weight, with significant weight regain observed after five years; post-operative time and work activity related to eating out as determining factors for the occurrence of weight regain.

  16. Determinants of inadequate weight gain in pregnancy.

    Science.gov (United States)

    Popa, Alina Delia; Niţă, Otilia; Popescu, Raluca Maria; Gherasim, Andreea; Arhire, Lidia luliana; Mihalache, Laura; Graur, Mariana

    2014-01-01

    The aim of the study was to explore the anthropometric maternal characteristics and prenatal care as determinants of pregnancy weight gain. We conducted a cross-sectional study on a total of 400 pregnant women admitted to Cuza-Vodă Obstetrics and Gynecology Clinical Hospital, Iaşi. Information on demographic characteristics, number of prenatal visits, and education on nutrition and food changes occurring during pregnancy were recorded in a structured questionnaire. Anthropometric parameters analyzed were pregestational BMI (body mass index) and weight gain during pregnancy. Weight gain was associated with pregestational BMI category. An increase in weight more than recommended occured more frequently in overweight (53.1%) and obese women (66.7%) (p < 0.001). Weight gain during pregnancy was related to area of residence, age, APCU (adequate prenatal care utilization) index. The multivariate analysis identified the following variables as significant determinants of pregnancy weight gain: inadequate prenatal care, BMI and changes in diet. Pregestational BMI and changes in diet during pregnancy identified as determinants of weight gain suggests that overweight and underweight women must carefully be counseled regarding recommendations for weight gain in pregnancy. Tracking diet changes is important to ensure that a weight gain lies within the guidelines recommendations.

  17. An objective approach to determining criteria weights

    Directory of Open Access Journals (Sweden)

    Milić R. Milićević

    2012-01-01

    Full Text Available This paper presents an objective approach to determining criteria weights that can be successfully used in multiple criteria models. The methods of entropy, CRITIC and FANMA are presented in this paper as well as a possible combination of the methods of objective and subjective approaches. Although based on different theoretical settings, and therefore with different algorithms of realization, all methods have a decision matrix as a starting point. An objective approach to determining the weight of criteria eliminates the negative impacts of a decision maker on criteria weights as well as on the final solution of multicriteria problems. The main aim of this paper is to systematize description procedures as a kind of help when encountering a problem of determining the criteria weights for solving multicriteria tasks. A possibility of the method application is shown in a numerical example.

  18. Weight Stigma Reduction and Genetic Determinism.

    Science.gov (United States)

    Hilbert, Anja

    2016-01-01

    One major approach to weight stigma reduction consists of decreasing beliefs about the personal controllability of-and responsibility for-obesity by educating about its biogenetic causes. Evidence on the efficacy of this approach is mixed, and it remains unclear whether this would create a deterministic view, potentially leading to detrimental side-effects. Two independent studies from Germany using randomized designs with delayed-intervention control groups served to (1) develop and pilot a brief, interactive stigma reduction intervention to educate N = 128 university students on gene × environment interactions in the etiology of obesity; and to (2) evaluate this intervention in the general population (N = 128) and determine mechanisms of change. The results showed (1) decreased weight stigma and controllability beliefs two weeks post-intervention in a student sample; and (2) decreased internal attributions and increased genetic attributions, knowledge, and deterministic beliefs four weeks post-intervention in a population sample. Lower weight stigma was longitudinally predicted by a decrease in controllability beliefs and an increase in the belief in genetic determinism, especially in women. The results underline the usefulness of a brief, interactive intervention promoting an interactionist view of obesity to reduce weight stigma, at least in the short term, lending support to the mechanisms of change derived from attribution theory. The increase in genetic determinism that occurred despite the intervention's gene × environment focus had no detrimental side-effect on weight stigma, but instead contributed to its reduction. Further research is warranted on the effects of how biogenetic causal information influences weight management behavior of individuals with obesity.

  19. Weight Stigma Reduction and Genetic Determinism

    Science.gov (United States)

    Hilbert, Anja

    2016-01-01

    One major approach to weight stigma reduction consists of decreasing beliefs about the personal controllability of—and responsibility for—obesity by educating about its biogenetic causes. Evidence on the efficacy of this approach is mixed, and it remains unclear whether this would create a deterministic view, potentially leading to detrimental side-effects. Two independent studies from Germany using randomized designs with delayed-intervention control groups served to (1) develop and pilot a brief, interactive stigma reduction intervention to educate N = 128 university students on gene × environment interactions in the etiology of obesity; and to (2) evaluate this intervention in the general population (N = 128) and determine mechanisms of change. The results showed (1) decreased weight stigma and controllability beliefs two weeks post-intervention in a student sample; and (2) decreased internal attributions and increased genetic attributions, knowledge, and deterministic beliefs four weeks post-intervention in a population sample. Lower weight stigma was longitudinally predicted by a decrease in controllability beliefs and an increase in the belief in genetic determinism, especially in women. The results underline the usefulness of a brief, interactive intervention promoting an interactionist view of obesity to reduce weight stigma, at least in the short term, lending support to the mechanisms of change derived from attribution theory. The increase in genetic determinism that occurred despite the intervention’s gene × environment focus had no detrimental side-effect on weight stigma, but instead contributed to its reduction. Further research is warranted on the effects of how biogenetic causal information influences weight management behavior of individuals with obesity. PMID:27631384

  20. ISO/GUM UNCERTAINTIES AND CIAAW (UNCERTAINTY TREATMENT FOR RECOMMENDED ATOMIC WEIGHTS AND ISOTOPIC ABUNDANCES)

    Energy Technology Data Exchange (ETDEWEB)

    HOLDEN,N.E.

    2007-07-23

    The International Organization for Standardization (ISO) has published a Guide to the expression of Uncertainty in Measurement (GUM). The IUPAC Commission on Isotopic Abundance and Atomic Weight (CIAAW) began attaching uncertainty limits to their recommended values about forty years ago. CIAAW's method for determining and assigning uncertainties has evolved over time. We trace this evolution to their present method and their effort to incorporate the basic ISO/GUM procedures into evaluations of these uncertainties. We discuss some dilemma the CIAAW faces in their present method and whether it is consistent with the application of the ISO/GUM rules. We discuss the attempt to incorporate variations in measured isotope ratios, due to natural fractionation, into the ISO/GUM system. We make some observations about the inconsistent treatment in the incorporation of natural variations into recommended data and uncertainties. A recommendation for expressing atomic weight values using a tabulated range of values for various chemical elements is discussed.

  1. The atomic weight and isotopic composition of boron and their variation in nature

    Energy Technology Data Exchange (ETDEWEB)

    Holden, N.E.

    1993-08-01

    The boron isotopic composition and atomic weight value and their variation in nature are reviewed. Questions are raised about the previously recommended value and the uncertainty for the atomic weight. The problem of what constitutes an acceptable range for normal material and what should then be considered geologically exceptional is discussed. Recent measurements make some previous decisions in need of re-evaluation.

  2. Determination of Atomic Data Pertinent to the Fusion Energy Program

    Energy Technology Data Exchange (ETDEWEB)

    Reader, J.

    2013-06-11

    We summarize progress that has been made on the determination of atomic data pertinent to the fusion energy program. Work is reported on the identification of spectral lines of impurity ions, spectroscopic data assessment and compilations, expansion and upgrade of the NIST atomic databases, collision and spectroscopy experiments with highly charged ions on EBIT, and atomic structure calculations and modeling of plasma spectra.

  3. Data reduction framework for standard atomic weights and isotopic compositions of the elements

    Science.gov (United States)

    Meija, Juris; Possolo, Antonio

    2017-04-01

    We outline a general framework to compute consensus reference values of standard atomic weights, isotope ratios, and isotopic abundances, and to evaluate associated uncertainties using modern statistical methods for consensus building that can handle mutually inconsistent measurement results. The multivariate meta-regression approach presented here is directly relevant to the work of the IUPAC Commission on Isotopic Abundances and atomic weights (CIAAW), and we illustrate the proposed method in meta-analyses of the isotopic abundances and atomic weights of zinc, platinum, antimony, and iridium.

  4. William Barlow and the Determination of Atomic Arrangement in Crystals.

    Science.gov (United States)

    Mauskopf, Seymour H

    2015-04-01

    William Barlow (1845-1934) was an important if unconventional scientist, known for having developed the 'closest-packing' atomic models of crystal structure. He resumed an early nineteenth-century tradition of utilizing crystallographical and chemical data to determine atomic arrangements in crystals. This essay recounts Barlow's career and scientific activity in three parts: (a) His place in the tradition of determining atomic arrangement in context of this earlier tradition and of contemporaneous developments of crystallography and chemistry, (b) his unconventional career, and (c) the 'success' of his program to determine atomic arrangements in crystals and its influence on the work of William Lawrence Bragg.

  5. Determination of absolute configuration using heavy atom based co-crystallization method: Halogen atom effects

    Science.gov (United States)

    Wang, Jian-Rong; Fan, Xiaowu; Ding, Qiaoce; Mei, Xuefeng

    2016-09-01

    Heavy atom (chloride, bromide, and iodide) based co-crystals for determination of absolute configuration (AC) for chiral molecules were synthesized and evaluated. Co-crystals of cholestanol and L-ascorbic acid were analysed and the effects and potential benefits of varying the heavy atom are discussed. Changing the halogen atoms (chloride, bromide, or iodide) affects the co-crystal formation, X-ray absorption, and anomalous dispersion, and hence the ability to determine AC.

  6. Determination of atomic cluster structure with cluster fusion algorithm

    DEFF Research Database (Denmark)

    Obolensky, Oleg I.; Solov'yov, Ilia; Solov'yov, Andrey V.

    2005-01-01

    We report an efficient scheme of global optimization, called cluster fusion algorithm, which has proved its reliability and high efficiency in determination of the structure of various atomic clusters.......We report an efficient scheme of global optimization, called cluster fusion algorithm, which has proved its reliability and high efficiency in determination of the structure of various atomic clusters....

  7. Method of trivalent chromium concentration determination by atomic spectrometry

    Science.gov (United States)

    Reheulishvili, Aleksandre N [Tbilisi, 0183, GE; Tsibakhashvili, Neli Ya [Tbilisi, 0101, GE

    2006-12-12

    A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

  8. Atomic-absorption determination of copper and zinc in ferroboron

    Energy Technology Data Exchange (ETDEWEB)

    Malinina, R.D.; Toropova, L.S.

    1986-03-01

    This paper reports on the development of an atomic-absorption method for determining copper and zinc impurities in ferroboron, used for alloying steels and special alloys. The work was done on a Model 503 Perkin-Elmer atomic absorption spectrophotometer. Effects of perchloric acid and alloy macrocomponents on zinc and copper atomization were studied. Results by atomic absorption spectrometry were compared with those found by polarography, using a PPT-6016 ac polarograph. Compared with the GOST 14021.7-78 method for determining copper, the proposed procedure is more rapid and decreases the detection limit from 1 X 10/sup -2/ to 5 X 10/sup -3/ wt. %.

  9. 7 CFR 981.60 - Determination of kernel weight.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 8 2010-01-01 2010-01-01 false Determination of kernel weight. 981.60 Section 981.60... Regulating Handling Volume Regulation § 981.60 Determination of kernel weight. (a) Almonds for which settlement is made on kernel weight. All lots of almonds, whether shelled or unshelled, for which...

  10. ADME evaluation in drug discovery. 2. Prediction of partition coefficient by atom-additive approach based on atom-weighted solvent accessible surface areas.

    Science.gov (United States)

    Hou, T J; Xu, X J

    2003-01-01

    A novel method for the calculations of 1-octanol/water partition coefficient (log P) of organic molecules has been presented here. The method, SLOGP v1.0, estimates the log P values by summing the contribution of atom-weighted solvent accessible surface areas (SASA) and correction factors. Altogether 100 atom/group types were used to classify atoms with different chemical environments, and two correlation factors were used to consider the intermolecular hydrophobic interactions and intramolecular hydrogen bonds. Coefficient values for 100 atom/group and two correction factors have been derived from a training set of 1850 compounds. The parametrization procedure for different kinds of atoms was performed as follows: first, the atoms in a molecule were defined to different atom/group types based on SMARTS language, and the correction factors were determined by substructure searching; then, SASA for each atom/group type was calculated and added; finally, multivariate linear regression analysis was applied to optimize the hydrophobic parameters for different atom/group types and correction factors in order to reproduce the experimental log P. The correlation based on the training set gives a model with the correlation coefficient (r) of 0.988, the standard deviation (SD) of 0.368 log units, and the absolute unsigned mean error of 0.261. Comparison of various procedures of log P calculations for the external test set of 138 organic compounds demonstrates that our method bears very good accuracy and is comparable or even better than the fragment-based approaches. Moreover, the atom-additive approach based on SASA was compared with the simple atom-additive approach based on the number of atoms. The calculated results show that the atom-additive approach based on SASA gives better predictions than the simple atom-additive one. Due to the connection between the molecular conformation and the molecular surface areas, the atom-additive model based on SASA may be a more

  11. Direct atomic structure determination by the inspection of structural phase.

    Science.gov (United States)

    Nakashima, Philip N H; Moodie, Alexander F; Etheridge, Joanne

    2013-08-27

    A century has passed since Bragg solved the first atomic structure using diffraction. As with this first structure, all atomic structures to date have been deduced from the measurement of many diffracted intensities using iterative and statistical methods. We show that centrosymmetric atomic structures can be determined without the need to measure or even record a diffracted intensity. Instead, atomic structures can be determined directly and quickly from the observation of crystallographic phases in electron diffraction patterns. Furthermore, only a few phases are required to achieve high resolution. This represents a paradigm shift in structure determination methods, which we demonstrate with the moderately complex α-Al2O3. We show that the observation of just nine phases enables the location of all atoms with a resolution of better than 0.1 Å. This level of certainty previously required the measurement of thousands of diffracted intensities.

  12. Determination of platinum, palladium, and lead in biological samples by atomic absorption spectrophotometry.

    Science.gov (United States)

    Tillery, J B; Johnson, D E

    1975-01-01

    A flameless atomic absorption method for the coextraction of platinum and palladium from biological and environmental samples by high molecular weight amine (HMWA) is given. Also, methods for lead determination in biological samples by use of extraction flameless analysis and direct aspiration-flame analysis are reported. A study of lead contamination of Vacutainer tubes is given. PMID:1227857

  13. Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Průša, Libor [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Hlavova 8, Prague 2, CZ 128 43 Czech Republic (Czech Republic); Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-12-04

    Graphical abstract: -- Highlights: •In-atomizer trapping HG-AAS was optimized for Sn. •A compact quartz trap-and-atomizer device was employed. •Generation, preconcentration and atomization steps were investigated in detail. •Hundred percent preconcentration efficiency for tin was reached. •Routine analytical method was developed for Sn determination (LOD of 0.03 ng mL{sup −1} Sn). -- Abstract: A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL{sup −1} Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.

  14. Hall Determination of Atomic Radii of Alkali Metals

    Science.gov (United States)

    Houari, Ahmed

    2008-01-01

    I will propose here an alternative method for determining atomic radii of alkali metals based on the Hall measurements of their free electron densities and the knowledge of their crystal structure. (Contains 2 figures.)

  15. Motivation, self-determination, and long-term weight control

    Directory of Open Access Journals (Sweden)

    Teixeira Pedro J

    2012-03-01

    Full Text Available Abstract This article explores the topics of motivation and self-regulation in the context of weight management and related behaviors. We focus on the role of a qualitative approach to address motivation - not only considering the level but also type of motivation - in weight control and related behaviors. We critically discuss the operationalization of motivation in current weight control programs, present a complementary approach to understanding motivation based on self-determination theory, and review empirical findings from weight control studies that have used self-determination theory measures and assessed their association with weight outcomes. Weight loss studies which used Motivational Interviewing (MI are also reviewed, considering MI's focus on enhancing internal motivation. We hypothesize that current weight control interventions may have been less successful with weight maintenance in part due to their relative disregard of qualitative dimensions of motivation, such as level of perceived autonomy, often resulting in a motivational disconnect between weight loss and weight-related behaviors. We suggest that if individuals fully endorse weight loss-related behavioral goals and feel not just competent but also autonomous about reaching them, as suggested by self-determination theory, their efforts are more likely to result in long-lasting behavior change.

  16. Motivation, self-determination, and long-term weight control

    Science.gov (United States)

    2012-01-01

    This article explores the topics of motivation and self-regulation in the context of weight management and related behaviors. We focus on the role of a qualitative approach to address motivation - not only considering the level but also type of motivation - in weight control and related behaviors. We critically discuss the operationalization of motivation in current weight control programs, present a complementary approach to understanding motivation based on self-determination theory, and review empirical findings from weight control studies that have used self-determination theory measures and assessed their association with weight outcomes. Weight loss studies which used Motivational Interviewing (MI) are also reviewed, considering MI's focus on enhancing internal motivation. We hypothesize that current weight control interventions may have been less successful with weight maintenance in part due to their relative disregard of qualitative dimensions of motivation, such as level of perceived autonomy, often resulting in a motivational disconnect between weight loss and weight-related behaviors. We suggest that if individuals fully endorse weight loss-related behavioral goals and feel not just competent but also autonomous about reaching them, as suggested by self-determination theory, their efforts are more likely to result in long-lasting behavior change. PMID:22385818

  17. A Robust Weighted Combination Forecasting Method Based on Forecast Model Filtering and Adaptive Variable Weight Determination

    Directory of Open Access Journals (Sweden)

    Lianhui Li

    2015-12-01

    Full Text Available Medium-and-long-term load forecasting plays an important role in energy policy implementation and electric department investment decision. Aiming to improve the robustness and accuracy of annual electric load forecasting, a robust weighted combination load forecasting method based on forecast model filtering and adaptive variable weight determination is proposed. Similar years of selection is carried out based on the similarity between the history year and the forecast year. The forecast models are filtered to select the better ones according to their comprehensive validity degrees. To determine the adaptive variable weight of the selected forecast models, the disturbance variable is introduced into Immune Algorithm-Particle Swarm Optimization (IA-PSO and the adaptive adjustable strategy of particle search speed is established. Based on the forecast model weight determined by improved IA-PSO, the weighted combination forecast of annual electric load is obtained. The given case study illustrates the correctness and feasibility of the proposed method.

  18. Absolute isotopic composition and atomic weight of neodymium using thermal ionization mass spectrometry.

    Science.gov (United States)

    Zhao, Motian; Zhou, Tao; Wang, Jun; Lu, Hai; Fang, Xiang; Guo, Chunhua; Li, Qiuli; Li, Chaofeng

    2005-01-01

    Synthetic mixtures prepared gravimetrically from highly enriched isotopes of neodymium in the form of oxides of well-defined purity were used to calibrate a thermal ionization mass spectrometer. A new error analysis was applied to calculate the final uncertainty of the atomic weight value. Measurements on natural neodymium samples yielded an absolute isotopic composition of 27.153(19) atomic percent (at.%) 142Nd, 12.173(18) at.% 143Nd, 23.798(12) at.% 144Nd, 8.293(7) at.% 145Nd, 17.189(17) at.% 146Nd, 5.756(8) at.% 148Nd, and 5.638(9) at.% 150Nd, and the atomic weight of neodymium as 144.2415(13), with uncertainties given on the basis of 95% confidence limits. No isotopic fractionation was found in terrestrial neodymium materials.

  19. Using atom mapping rules for an improved detection of relevant routes in weighted metabolic networks.

    Science.gov (United States)

    Blum, Torsten; Kohlbacher, Oliver

    2008-01-01

    Computational analysis of pathways in metabolic networks has numerous applications in systems biology. While graph theory-based approaches have been presented that find biotransformation routes from one metabolite to another in these networks, most of these approaches suffer from finding too many routes, most of which are biologically infeasible or meaningless. We present a novel approach for finding relevant routes based on atom mapping rules (describing which educt atoms are mapped onto which product atoms in a chemical reaction). This leads to a reformulation of the problem as a lightest path search in a degree-weighted metabolic network. The key component of the approach is a new method of computing optimal atom mapping rules.

  20. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  1. Variation in the terrestrial isotopic composition and atomic weight of argon

    Science.gov (United States)

    Böhlke, John Karl

    2014-01-01

    The isotopic composition and atomic weight of argon (Ar) are variable in terrestrial materials. Those variations are a source of uncertainty in the assignment of standard properties for Ar, but they provide useful information in many areas of science. Variations in the stable isotopic composition and atomic weight of Ar are caused by several different processes, including (1) isotope production from other elements by radioactive decay (radiogenic isotopes) or other nuclear transformations (e.g., nucleogenic isotopes), and (2) isotopic fractionation by physical-chemical processes such as diffusion or phase equilibria. Physical-chemical processes cause correlated mass-dependent variations in the Ar isotope-amount ratios (40Ar/36Ar, 38Ar/36Ar), whereas nuclear transformation processes cause non-mass-dependent variations. While atmospheric Ar can serve as an abundant and homogeneous isotopic reference, deviations from the atmospheric isotopic ratios in other Ar occurrences limit the precision with which a standard atomic weight can be given for Ar. Published data indicate variation of Ar atomic weights in normal terrestrial materials between about 39.7931 and 39.9624. The upper bound of this interval is given by the atomic mass of 40Ar, as some samples contain almost pure radiogenic 40Ar. The lower bound is derived from analyses of pitchblende (uranium mineral) containing large amounts of nucleogenic 36Ar and 38Ar. Within this interval, measurements of different isotope ratios (40Ar/36Ar or 38Ar/36Ar) at various levels of precision are widely used for studies in geochronology, water–rock interaction, atmospheric evolution, and other fields.

  2. Determination of Surface Exciton Energies by Velocity Resolved Atomic Desorption

    Energy Technology Data Exchange (ETDEWEB)

    Hess, Wayne P.; Joly, Alan G.; Beck, Kenneth M.; Sushko, Petr V.; Shluger, Alexander L.

    2004-08-20

    We have developed a new method for determining surface exciton band energies in alkali halides based on velocity-resolved atomic desorption (VRAD). Using this new method, we predict the surface exciton energies for K1, KBr, KC1, and NaC1 within +0.15 eV. Our data, combined with the available EELS data for alkali fluorides, demonstrate a universal linear correlation with the inverse inter-atomic distance in these materials. The results suggest that surface excitons exist in all alkali halides and their excitation energies can be predicted from the known bulk exciton energies and the obtained correlation plot.

  3. Bio- Social Determinants Of Birth Weight In Rural Urban Nagpur

    Directory of Open Access Journals (Sweden)

    Gawande U.H

    1994-01-01

    Full Text Available Research Questions: What are the bio â€" social determinants of birth weight of babies born in an urban- rural area? Objectives: 1. To study the biosocial determinants of birth weight 2. To determine which of the these affects birth weight. Design : Cross- sectional study. Setting : General hospital in Nagpur Participants: Mothers and their babies who were delivered in hospital. Study Variables : Mother’s age, parity, inter- pregnancy interval, socio-economic status, literacy status, antenatal care. Outcome Variable: Birth weight of the Infant. Statistical Analysis: Chi square test. Results: The proportion of low birth weight babies was high in teenage mothers(41.9% and those over the age of 30 years. Primi and grand multiparity were associated with higher prevalence of low birth weight babies (43.2% & 43.9% respectively. Interpregnancy interval of less than one and a half years had a high prevalence of LBW babies (44.7% but an interval of 5 years was also a risk as there were other associated risk factors like secondary sterility, tuberculosis etc. Low socio-economic status and low literacy levels were associated with significant proportion of LBW babies. Those mothers who had received adequate antenatal care gave birth to a significantly lower proportion of LBW babies than those who has not received antenatal care. Conclusion: Birthweight is determined by biosocial factors which are recognisable and some of which can be controlled.

  4. A simplified electrophoretic system for determining molecular weights of proteins.

    Science.gov (United States)

    Manwell, C

    1977-09-01

    Electrophoresis of 31 different proteins in commercially prepared polyacrylamide gradient gels, Gradipore, yields a linear relationship between a hypothetical limiting pore size (the reciprocal of a limiting gel concentration, GL) and the cube root of the mol.wt., over the range 13 500-9000 000. A regression analysis of these data reveals that 98.6% of all variability in 1/GL is explained by the molecular weight, and this degree of accuracy compares favourably with existing methods for the determination of molecular weight by retardation of mobility in polyacrylamide. This new procedure has the additional advantages that molecular-weight standards can be obtained from readily available body fluids or tissue extracts by localizing enzymes and other proteins by standard histochemical methods, and that the same electrophoretic system can be used in determining molecular weights as is used in routine surveys of populations for individual and species variation in protein heterogeneity.

  5. Orbiter spacecraft weight and center of gravity determination

    Science.gov (United States)

    Fraley, J. G.

    1983-01-01

    This paper describes the procedure for determination of the weight and the location of the center of gravity (c.g.) of a Space Shuttle Orbiter Spacecraft, at the Kennedy Space Center, Florida. This task is performed at the completion of the horizontal processing of each Orbiter in conjunction with jack down and preparation for vertical mating to the Shuttle launch vehicle. The operation is performed in the Orbiter Processing Facility. The paper contains a brief description of the general characteristics and physical dimensions of the Orbiter spacecraft, the program requirements and test procedure for weight and c.g. determination, data evaluation and a summary.

  6. A novel weight determination method for time series data aggregation

    Science.gov (United States)

    Xu, Paiheng; Zhang, Rong; Deng, Yong

    2017-09-01

    Aggregation in time series is of great importance in time series smoothing, predicting and other time series analysis process, which makes it crucial to address the weights in times series correctly and reasonably. In this paper, a novel method to obtain the weights in time series is proposed, in which we adopt induced ordered weighted aggregation (IOWA) operator and visibility graph averaging (VGA) operator and linearly combine the weights separately generated by the two operator. The IOWA operator is introduced to the weight determination of time series, through which the time decay factor is taken into consideration. The VGA operator is able to generate weights with respect to the degree distribution in the visibility graph constructed from the corresponding time series, which reflects the relative importance of vertices in time series. The proposed method is applied to two practical datasets to illustrate its merits. The aggregation of Construction Cost Index (CCI) demonstrates the ability of proposed method to smooth time series, while the aggregation of The Taiwan Stock Exchange Capitalization Weighted Stock Index (TAIEX) illustrate how proposed method maintain the variation tendency of original data.

  7. Determination of criteria weights in solving multi-criteria problems

    Science.gov (United States)

    Kasim, Maznah Mat

    2014-12-01

    A multi-criteria (MC) problem comprises of units to be analyzed under a set of evaluation criteria. Solving a MC problem is basically the process of finding the overall performance or overall quality of the units of analysis by using certain aggregation method. Based on these overall measures of each unit, a decision can be made whether to sort them, to select the best or to group them according to certain ranges. Prior to solving the MC problems, the weights of the related criteria have to be determined with the assumption that the weights represent the degree of importance or the degree of contribution towards the overall performance of the units. This paper presents two main approaches which are called as subjective and objective approaches, where the first one involves evaluator(s) while the latter approach depends on the intrinsic information contained in each criterion. The subjective and objective weights are defined if the criteria are assumed to be independent with each other, but if they are dependent, there is another type of weight, which is called as monotone measure weight or compound weights which represent degree of interaction among the criteria. The measure of individual weights or compound weights must be addressed in solving multi-criteria problems so that the solutions are more reliable since in the real world, evaluation criteria always come with different degree of importance or are dependent with each other. As the real MC problems have their own uniqueness, it is up to the decision maker(s) to decide which type of weights and which method are the most applicable ones for the problem under study.

  8. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Directory of Open Access Journals (Sweden)

    Hesham Salem

    2005-01-01

    Full Text Available Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate. The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed native fluorescence at 450 nm when excitation was at 290 nm. The calibration graph was rectilinear from 0.3-1.4 μg mL-1 (method I. Cobalt sulphate was used for precipitation of the ion associates formed from the reaction with the cited drugs. The formation and solubility of the solid complexes at the optimum conditions of pH and ionic strength values have been studied. The method depends on direct determination of the ions in the precipitate or indirect determination of the ions in the filtrate by atomic absorption spectroscopy. The optimum conditions for precipitation were carefully studied. Rectilinear calibration graphs were obtained in the range of 3-30 μg mL-1 for each of the investigated drugs. The molar ratios of the formed chelats were determined by Job's method and their association constants were also calculated (method II. Ammonium vanadate was used for the spectrophotometric determination of the selected fluoroquinolones by oxidation in sulphuric acid medium resulting in the development of a greenish blue colour measured at 766 nm which was attributed to the vanadium (IV produced by reduction of vanadium (V by the selected drugs. The optimum conditions for heating time, reagent concentration and sulphuric acid concentration were carefully studied. The accuracy and precision of the proposed method was confirmed by estimating five or six replicates within Beer's law limits were obtained in the range 10-40 μg mL-1 for each of the investigated drugs

  9. Determinants of birth weight in Portugal: 1988 to 2011.

    Science.gov (United States)

    Fuster, Vicente; Santos, Carlota

    2016-01-01

    The objective of this paper is to analyse temporal birth weight variation, its relationship to the frequency of premature births in Portugal, and the influence of native and immigrant mothers' characteristics as well as to determine the possible existence of a pattern of temporal change in birth weight in the Iberian Peninsula as a whole. Individual mother-child data from the Portuguese National Institute of Statistics regarding live births (N = 2,661,542) permitted an analysis, for the first time, of weight at birth in Portugal from a bio-demographic perspective. The results obtained show that from 1988 to 2011 there was a gradual decline in the average weight at birth in Portugal that may be related to shifts in the duration of gestation. An initial rapid decline in the relative frequency of post-term births took place, followed by small variations from 1995 on. Logistic regressions indicated a pattern unaffected by maternal origin or the sex of the newborn. With regard to weeks of gestation, the odds values obtained were < 1 when the reference category was < 28 weeks. For this factor, no significant differences were found in relation to the mother's origin. Portuguese mothers over 35 years were associated with a higher incidence of low birth weight. Regardless of maternal origin, being a newborn of parity 1, and with the mother not in a couple, resulted in unfavourable outcomes with regard to low birth weight. On the other hand, long gestation periods and having secondary or university education constituted a protective factor.

  10. Determinants of low birth weight in rural Bangladesh

    Directory of Open Access Journals (Sweden)

    Manzur Kader

    2013-04-01

    Full Text Available Introduction: Low birth weight (LBW is an important risk factor for childhood morbidity and mortality. Thus, it is an important public health concern. The study was aimed to identify the important socioeconomic, anthropometric and nutritional determinants associated with LBW. Factors included maternal household wealth status, age, literacy, nutritional status, parity, stature, gestational age and chewing betel nut or tobacco. Methods: The study included data of 4436 enrolled pregnant women in the Maternal and Infant Nutrition Intervention Matlab (MINIMat trial from November 2001 to October 2003. A random subset of (n= 3267 single live birth infants born between May 2002 and June 2004 with complete information on birth weight was analyzed. Pearson’s chi square test and logistic regression analysis were done to assess the association between the factors and LBW. Results: Almost one third of the infants were born with LBW and mean birth weight was 2693 g. Maternal poor wealth status, BMI less than 18.5, short stature (height < 152 cm and preterm (<37 weeks birth were found to be strong predictors of LBW. Women’s age, hemoglobin status and chewing tobacco or betel nut were not found to be associated with LBW. Conclusion: Women’s wealth status, literacy, maternal nutrition and prevention of preterm birth are the key factors that need to be considered to improve birth weight of infants. [Int J Reprod Contracept Obstet Gynecol 2013; 2(2.000: 130-134

  11. Quick-Determination of the Average Atomic Number Z by X-Ray Scattering

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar

    1972-01-01

    X-ray scattering ratio measurements are proposed for a quick determination of the average atomic number of rock powders.......X-ray scattering ratio measurements are proposed for a quick determination of the average atomic number of rock powders....

  12. Semantic Referencing - Determining Context Weights for Similarity Measurement

    Science.gov (United States)

    Janowicz, Krzysztof; Adams, Benjamin; Raubal, Martin

    Semantic similarity measurement is a key methodology in various domains ranging from cognitive science to geographic information retrieval on the Web. Meaningful notions of similarity, however, cannot be determined without taking additional contextual information into account. One way to make similarity measures context-aware is by introducing weights for specific characteristics. Existing approaches to automatically determine such weights are rather limited or require application specific adjustments. In the past, the possibility to tweak similarity theories until they fit a specific use case has been one of the major criticisms for their evaluation. In this work, we propose a novel approach to semi-automatically adapt similarity theories to the user's needs and hence make them context-aware. Our methodology is inspired by the process of georeferencing images in which known control points between the image and geographic space are used to compute a suitable transformation. We propose to semi-automatically calibrate weights to compute inter-instance and inter-concept similarities by allowing the user to adjust pre-computed similarity rankings. These known control similarities are then used to reference other similarity values.

  13. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.

  14. Determination of antimony by using tungsten trap atomic absorption spectrometry

    Science.gov (United States)

    Titretir, Serap; Kendüzler, Erdal; Arslan, Yasin; Kula, İbrahim; Bakırdere, Sezgin; Ataman, O. Yavuz.

    2008-08-01

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH 3 is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 °C. Following the preconcentration step, the trap is heated to 895 °C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH 4 solutions, H 2 and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l - 1 using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17.

  15. Determination of antimony by using tungsten trap atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Titretir, Serap [Department of Chemistry, Inoenue University, 44065 Malatya (Turkey); Kenduezler, Erdal [Department of Primary Education, Faculty of Education, Ahi Evran University, 40100 Kirsehir (Turkey); Arslan, Yasin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Atatuerk University, 25240 Erzurum (Turkey); Kula, Ibrahim [Department of Chemistry, Mugla University, 48000 Mugla (Turkey); Bakirdere, Sezgin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Zonguldak Karaelmas University, 67100 Zonguldak (Turkey); Ataman, O. Yavuz. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH{sub 3} is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH{sub 4} solutions, H{sub 2} and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l{sup -1} using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17.

  16. Method for the determination of cobalt from biological products with graphite furnace atomic absorption spectrometer

    Science.gov (United States)

    Zamfir, Oana-Liliana; Ionicǎ, Mihai; Caragea, Genica; Radu, Simona; Vlǎdescu, Marian

    2016-12-01

    Cobalt is a chemical element with symbol Co and atomic number 27 and atomic weight 58.93. 59 Co is the only stable cobalt isotope and the only isotope to exist naturally on Earth. Cobalt is the active center of coenzymes called cobalamin or cyanocobalamin the most common example of which is vitamin B12. Vitamin B12 deficiency can potentially cause severe and irreversible damage, especially to the brain and nervous system in the form of fatigue, depression and poor memory or even mania and psychosis. In order to study the degree of deficiency of the population with Co or the correctness of treatment with vitamin B12, a modern optoelectronic method for the determination of metals and metalloids from biological samples has been developed, Graphite Furnace - Atomic Absorption Spectrometer (GF- AAS) method is recommended. The technique is based on the fact that free atoms will absorb light at wavelengths characteristic of the element of interest. Free atoms of the chemical element can be produced from samples by the application of high temperatures. The system GF-AAS Varian used as biological samples, blood or urine that followed the digest of the organic matrix. For the investigations was used a high - performance GF-AAS with D2 - background correction system and a transversely heated graphite atomizer. As result of the use of the method are presented the concentration of Co in the blood or urine of a group of patient in Bucharest. The method is sensitive, reproducible relatively easy to apply, with a moderately costs.

  17. Modernization of Enoxaparin Molecular Weight Determination Using Homogeneous Standards

    Directory of Open Access Journals (Sweden)

    Katelyn M. Arnold

    2017-07-01

    Full Text Available Enoxaparin is a low-molecular weight heparin used to treat thrombotic disorders. Following the fatal contamination of the heparin supply chain in 2007–2008, the U.S. Pharmacopeia (USP and U.S. Food and Drug Administration (FDA have worked extensively to modernize the unfractionated heparin and enoxaparin monographs. As a result, the determination of molecular weight (MW has been added to the monograph as a measure to strengthen the quality testing and to increase the protection of the global supply of this life-saving drug. The current USP calibrant materials used for enoxaparin MW determination are composed of a mixture of oligosaccharides; however, they are difficult to reproduce as the calibrants have ill-defined structures due to the heterogeneity of the heparin parent material. To address this issue, we describe a promising approach consisting of a predictive computational model built from a library of chemoenzymatically synthesized heparin oligosaccharides for enoxaparin MW determination. Here, we demonstrate that this test can be performed with greater efficiency by coupling synthetic oligosaccharides with the power of computational modeling. Our approach is expected to improve the MW measurement for enoxaparin.

  18. Investigation of fetal weight determination in X-ray pelvimetry

    Energy Technology Data Exchange (ETDEWEB)

    Chung, M. D.; Tae, S.; Lee, H. K.; Kwon, K. H.; Chung, W. K.; Kim, K. J. [Soon Chung Hyang College Hospital, Chunan (Korea, Republic of)

    1981-06-15

    The X-ray pelvimetry is widely used for investigation of fetal weight determination by measuring the size of the fetal head. The report concerns 173 cases with Colcher-Sussman method from January 1'77 to December 31'80 at Soon Chun Hyang college hospital. We measured fetal head diameter in both A-P and lateral projections. The brief results are as follows: 1)Among the total 173 cases, vaginal delivery is 88 cases and Cesarean section is 85 cases. 2) The rate of Cesarean section is increased over 35 years of age and 4,000 gm of birth weight. 3) The rate of Cesarean section is increased in abnormal presentation. 4) The relationship between the fetal head diameter and the fetal weight is more significant in A-P plus lateral projection than A-P only. 5) The average size of the fetal head is 0.8cm larger in Cesarean section than in vaginal delivery.

  19. Determination of Lead in Blood by Atomic Absorption Spectrophotometry1

    Science.gov (United States)

    Selander, Stig; Cramér, Kim

    1968-01-01

    Lead in blood was determined by atomic absorption spectrophotometry, using a wet ashing procedure and a procedure in which the proteins were precipitated with trichloroacetic acid. In both methods the lead was extracted into isobutylmethylketone before measurement, using ammonium pyrrolidine dithiocarbamate as chelator. The simpler precipitation procedure was shown to give results identical with those obtained with the ashing technique. In addition, blood specimens were examined by the precipitation method and by spectral analysis, which method includes wet ashing of the samples, with good agreement. All analyses were done on blood samples from `normal' persons or from lead-exposed workers, and no additions of inorganic lead were made. The relatively simple protein precipitation technique gave accurate results and is suitable for the large-scale control of lead-exposed workers. PMID:5663425

  20. The determination of vanadium in brines by atomic absorption spectroscopy

    Science.gov (United States)

    Crump-Wiesner, Hans J.; Feltz, H.R.; Purdy, W.C.

    1971-01-01

    A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 ??g l-1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 ??g ml-1, respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels. ?? 1971.

  1. Weight Determining of Factors Influencing Grain Output Based on Entropy Weight Method

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    This article selects 8 main factors(the number of rural employees,total power of agricultural machinery,effective irrigation area of crops,growing area of grain crops,fertilizer consumption,electricity consumption in rural areas,area affected and area covered) as the factors influencing grain output,and offers the method of determining weight of factors influencing grain output using entropy weight method.According to the relevant data in the period 1985-2005,we analyze the weight of factors influencing grain output in China by example.The results show that the electricity consumption in rural areas has the greatest impact on grain output,followed by total power of agricultural machinery,fertilizer consumption and area covered.To increase grain output,we must enhance the degree of mechanization,free people from the former process of direct cultivation,strengthen water conservancy construction,and do a good job in disaster prevention and mitigation.

  2. Determination of Lead in Urine by Atomic Absorption Spectrophotometry1

    Science.gov (United States)

    Selander, Stig; Cramé, Kim

    1968-01-01

    A method for the determination of lead in urine by means of atomic absorption spectrophotometry (AAS) is described. A combination of wet ashing and extraction with ammonium pyrrolidine dithiocarbamate into isobutylmethylketone was used. The sensitivity was about 0·02 μg./ml. for 1% absorption, and the detection limit was about 0·02 μg./ml. with an instrumental setting convenient for routine analyses of urines. Using the scale expansion technique, the detection limit was below 0·01 μg./ml., but it was found easier to determine urinary lead concentrations below 0·05 μg./ml. by concentrating the lead in the organic solvent by increasing the volume of urine or decreasing that of the solvent. The method was applied to fresh urines, stored urines, and to urines, obtained during treatment with chelating agents, of patients with lead poisoning. Urines with added inorganic lead were not used. The results agreed well with those obtained with a colorimetric dithizone extraction method (r = 0·989). The AAS method is somewhat more simple and allows the determination of smaller lead concentrations. PMID:5647975

  3. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    Science.gov (United States)

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1).

  4. The atomic weight and isotopic composition of nitrogen and their variation in nature

    Energy Technology Data Exchange (ETDEWEB)

    Holden, N.E.

    1987-01-01

    Two stable isotopes of nitrogen exist in nature, /sup 14/N and /sup 15/N. The less abundant isotope, /sup 15/N, was discovered in 1929 by Naude, who studied the band spectra of nitric oxide, NO. However, the main source of a standard for this element is the air in the atmosphere, which is made up of approximately 78% N/sub 2/. Reviewed in this paper is the measurements of the isotopic composition in air and its variation around the world. Also investigated is the variation of the isotopic composition in the various compounds or sources of nitrogen compared to the value in air. Data on the atomic weight and non-terrestrial data for nitrogen is also reviewed.

  5. Atomic absorption method for the determination of lead in air

    Energy Technology Data Exchange (ETDEWEB)

    Szivos, K.; Polos, L.; Feher, I.; Pungor, E.

    1974-01-01

    An atomic absorption method for the determination of lead in air was used to analyze air quality at a busy area of Budapest. The air was sampled by a personal sampler carried by persons on street duty at one of the busiest spots in Budapest. The air sample was pumped through a membrane filter type Synpor-3. The filter was destroyed in th 3:2 mixture of strong nitric acid/hydrogen peroxide, the acid was distilled, and the residue was then dried and filled to 2 ml with an 0.5% tartaric acid solution. The results were evaluated by means of calibration curves. The method gave a standard deviation of 3 to 5% in 1 to 3 micrograms/ml concentration. In 0.5% tartaric acid solution, the sensitivity was 0.65 micrograms lead/ml 1% absorption. The presence of tartarate increased the sensitivity of the determination by 10 to 13%. A historgram was constructed of the lead contamination in air at one of the busiest spots of Budapest in 1971. The lead content of air was lower in the summer, probably due to the more intense air currents. The samples contained 0.6 to 13 micrograms of lead, depending on the amount and on the pollution of the air driven through the sampler.

  6. Determination of hydration film thickness using atomic force microscopy

    Institute of Scientific and Technical Information of China (English)

    PENG Changsheng; SONG Shaoxian; GU Qingbao

    2005-01-01

    Dispersion of a solid particle in water may lead to the formation of hydration film on the particle surface, which can strongly increase the repulsive force between the particles and thus strongly affect the stability of dispersions. The hydration film thickness, which varies with the variation of property of suspension particles, is one of the most important parameters of hydration film, and is also one of the most difficult parameters that can be measured accurately. In this paper, a method, based on force-distance curve of atomic force microscopy, for determining the hydration film thickness of particles is developed. The method utilizes the difference of cantilever deflection before, between and after penetrating the hydration films between tip and sample, which reflect the difference of slope on the force-distance curve. 3 samples, mica, glass and stainless steel, were used for hydration thickness determination, and the results show that the hydration film thickness between silicon tip and mica, glass and stainless steel are 30.0(2.0, 29.0(1.0 and 32.5(2.5 nm, respectively.

  7. Redshift determination through weighted phase correlation: a linearithmic implementation

    Science.gov (United States)

    Delchambre, L.

    2016-08-01

    We present a new algorithm having a time complexity of O(N log N) and designed to retrieve the phase at which an input signal and a set of not necessarily orthogonal templates match best in a weighted chi-squared sense. The proposed implementation is based on an orthogonalization algorithm and thus also benefits from high numerical stability. We apply this method successfully to the redshift determination of quasars from the twelfth Sloan Digital Sky Survey (SDSS) quasar catalogue and derive the proper spectral reduction and redshift selection methods. Derivations of the redshift uncertainty and the associated confidence are also provided. The results of this application are comparable to the performance of the SDSS pipeline, while not having a quadratic time dependence.

  8. MAGIA - using atom interferometry to determine the Newtonian gravitational constant

    Energy Technology Data Exchange (ETDEWEB)

    Stuhler, J; Fattori, M; Petelski, T; Tino, G M [Dipartimento di Fisica and LENS, Universita di Firenze, INFN - Sezione di Firenze, Via Sansone 1, I-50019 Sesto Fiorentino (Finland), Italy

    2003-04-01

    We describe our experiment MAGIA (misura accurata di G mediante interferometria atomica), in which we will use atom interferometry to perform a high precision measurement of the Newtonian gravitational constant G. Free-falling laser-cooled atoms in a vertical atomic fountain will be accelerated due to the gravitational potential of nearby source masses (SMs). Detecting this acceleration with techniques of Raman atom interferometry will enable us to assign a value to G. To suppress systematic effects we will implement a double-differential measurement. This includes launching two atom clouds in a gradiometer configuration and moving the SMs to different vertical positions. We briefly summarize the general idea of the MAGIA experiment and put it in the context of other high precision G-measurements. We present the current status of the experiment and report on analyses of the expected measurement accuracy.

  9. Atoms

    Institute of Scientific and Technical Information of China (English)

    刘洪毓

    2007-01-01

    Atoms(原子)are all around us.They are something like the bricks (砖块)of which everything is made. The size of an atom is very,very small.In just one grain of salt are held millions of atoms. Atoms are very important.The way one object acts depends on what

  10. Atomic Absorption Spectrophotometric Determination of Lead in White Rice

    Directory of Open Access Journals (Sweden)

    Sherryl M. Montalbo

    2015-11-01

    Full Text Available Recent studies on the heavy metal content of rice from various parts of the world have alarmed rice-eating nations, including the Philippines. In 2013, Philippine Rice Research Institute (PhilRice reported that rice in the Philippines needs to be evaluated to determine whether these contain heavy metals such as lead. This research aimed to assess the presence of lead in the three highest selling rice varieties harvested in Oriental Mindoro and sold in Batangas City public markets. It was done to asses if the lead concentration in the raw and cooked rice samples conform to the maximum acceptable level in food established by Joint FAO/WHO Expert Committee on Food Additives (JECFA Program Codex Alimentarius Commission. Survey analysis showed that the three highest selling rice varieties during the period when this study was conducted were Sinandomeng, Dinorado and C-4 Dinorado respectively. Lead analysis of rice samples was carried out using Flame Atomic Absorption Spectroscopy. The lead content in both the raw and cooked rice samples were not detected, meaning that the lead concentration were either not present or may be present but is less than the detection limit of the instrument used. The lead concentration in the rice samples from Oriental Mindoro conformed to the standards for food safety for lead content in rice, which is 0.2 mg/kg or 0.2 ppm, set by the Codex Alimentarius Commission.

  11. Uranium isotopes quantitatively determined by modified method of atomic absorption spectrophotometry

    Science.gov (United States)

    Lee, G. H.

    1967-01-01

    Hollow-cathode discharge tubes determine the quantities of uranium isotopes in a sample by using atomic absorption spectrophotometry. Dissociation of the uranium atoms allows a large number of ground state atoms to be produced, absorbing the incident radiation that is different for the two major isotopes.

  12. Molecule-specific determination of atomic polarizabilities with the polarizable atomic multipole model.

    Science.gov (United States)

    Woo Kim, Hyun; Rhee, Young Min

    2012-07-30

    Recently, many polarizable force fields have been devised to describe induction effects between molecules. In popular polarizable models based on induced dipole moments, atomic polarizabilities are the essential parameters and should be derived carefully. Here, we present a parameterization scheme for atomic polarizabilities using a minimization target function containing both molecular and atomic information. The main idea is to adopt reference data only from quantum chemical calculations, to perform atomic polarizability parameterizations even when relevant experimental data are scarce as in the case of electronically excited molecules. Specifically, our scheme assigns the atomic polarizabilities of any given molecule in such a way that its molecular polarizability tensor is well reproduced. We show that our scheme successfully works for various molecules in mimicking dipole responses not only in ground states but also in valence excited states. The electrostatic potential around a molecule with an externally perturbing nearby charge also exhibits a near-quantitative agreement with the reference data from quantum chemical calculations. The limitation of the model with isotropic atoms is also discussed to examine the scope of its applicability.

  13. Determination of riverbank erosion probability using Locally Weighted Logistic Regression

    Science.gov (United States)

    Ioannidou, Elena; Flori, Aikaterini; Varouchakis, Emmanouil A.; Giannakis, Georgios; Vozinaki, Anthi Eirini K.; Karatzas, George P.; Nikolaidis, Nikolaos

    2015-04-01

    Riverbank erosion is a natural geomorphologic process that affects the fluvial environment. The most important issue concerning riverbank erosion is the identification of the vulnerable locations. An alternative to the usual hydrodynamic models to predict vulnerable locations is to quantify the probability of erosion occurrence. This can be achieved by identifying the underlying relations between riverbank erosion and the geomorphological or hydrological variables that prevent or stimulate erosion. Thus, riverbank erosion can be determined by a regression model using independent variables that are considered to affect the erosion process. The impact of such variables may vary spatially, therefore, a non-stationary regression model is preferred instead of a stationary equivalent. Locally Weighted Regression (LWR) is proposed as a suitable choice. This method can be extended to predict the binary presence or absence of erosion based on a series of independent local variables by using the logistic regression model. It is referred to as Locally Weighted Logistic Regression (LWLR). Logistic regression is a type of regression analysis used for predicting the outcome of a categorical dependent variable (e.g. binary response) based on one or more predictor variables. The method can be combined with LWR to assign weights to local independent variables of the dependent one. LWR allows model parameters to vary over space in order to reflect spatial heterogeneity. The probabilities of the possible outcomes are modelled as a function of the independent variables using a logistic function. Logistic regression measures the relationship between a categorical dependent variable and, usually, one or several continuous independent variables by converting the dependent variable to probability scores. Then, a logistic regression is formed, which predicts success or failure of a given binary variable (e.g. erosion presence or absence) for any value of the independent variables. The

  14. A new formula for the statistical weight for a sequence of Rydberg levels in an atom or ion

    Science.gov (United States)

    Eriksson, M.; Lennerstad, H.

    2017-07-01

    We present a new formula for the total statistical weight of all Rydberg levels Gion (nl, nh ) for which the principal quantum number n is between higher, nh , and a lower, nl , limits. This formula can be used for all atoms in the periodic table and for all corresponding ions.

  15. [Determination of inorganic elements in different parts of Sonchus oleraceus L by flame atomic absorption spectrometry].

    Science.gov (United States)

    Wang, Nai-Xing; Cui, Xue-Gui; Du, Ai-Qin; Mao, Hong-Zhi

    2007-06-01

    Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (microg x g(-1)) for the 13 kinds of metal elements is as follows: leaf (77 213.72) > flower (47 927.15) > stem(42 280.99) > root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.

  16. Determination of deposited flux and energy of sputtered tungsten atoms on every stages of transport in HiPIMS discharge

    Science.gov (United States)

    Desecures, M.; de Poucques, L.; Bougdira, J.

    2017-02-01

    A time-resolved tunable diode-laser (DL) induced fluorescence (TR-TDLIF) technique has been used to identify different populations of atoms (on different stages of transport) to determine their corresponding deposited energy and flux. The temporal dimension permits the splitting of the processes of sputtering during the discharge and particles transport in the post-discharge where atoms and flux velocity distribution functions (AVDF, FVDF) of each population were measured varying the discharge parameters (power, voltage, pressure, and distance from target). Tungsten (W) was chosen, being an interesting case in terms of sputtered atom transport, considering its weight which implies weak changes of directivity or energy transfer after collisions with the buffer gas. The high temporal and spectral resolutions of TR-TDLIF are the keys for the distinction of the atoms populations and the stage corresponding to the transition from the ballistic to diffusive regime of transport was observed for the first time and named quasi-diffusive regime. Thus, the ability to dissociate populations of atoms and to determine their deposited flux and energy may be of great interest to adjust film properties as desired for applications.

  17. Determination of molecular, atomic, electronic cross-sections and effective atomic number of some boron compounds and TSW

    Energy Technology Data Exchange (ETDEWEB)

    Icelli, Orhan [Department of physics Education, Faculty of Education Erzincan University, 24030 Erzincan (Turkey)], E-mail: orhanicelli@gmail.com; Erzeneoglu, Salih [Department of physics, Faculty of Sciences, Atatuerk University, Erzurum (Turkey); Boncukcuoglu, Recep [Department of Environmental Engineering, Faculty of Engineering, Atatuerk University, Erzurum (Turkey)

    2008-07-15

    The transmission of gamma-rays of some boron compounds (H{sub 3}BO{sub 3}, Na{sub 2}B{sub 4}O{sub 7}) and the trommel sieve waste (TSW) have been measured by using an extremely narrow-collimated-beam transmission method in the energy range 15.74-40.93 keV. Molecular, atomic and electronic cross-sections and effective atomic numbers have been determinated on the basis of mixture rule and compared with the results obtained from theory.

  18. Determination of the effective atomic number of thick samples of unknown composition using scattering studies

    Science.gov (United States)

    Sankarshan, B. M.; Athrey, C. D.; Umesh, T. K.

    2017-06-01

    The effective atomic number ( Z_eff is a quantity which gives the fraction of the total number of electrons in a composite material participating in the photon-atom interaction. The effective atomic number has been determined for the materials of known composition by using different methods. However, no method has been reported so far to determine Z_eff for thick samples of unknown composition. In view of this, we have evolved a simple method to determine the effective atomic number, which uses the scattering intensity ratios measured at two scattering angles, in which a sample of known Z_eff or Z is taken as a reference sample. The values of Z_eff obtained by this method agree with those obtained from the Auto-Zeff software within the stated errors. This method could be helpful in determining the effective atomic number of samples of unknown composition.

  19. Determination of finite-difference weights using scaled binomial windows

    KAUST Repository

    Chu, Chunlei

    2012-05-01

    The finite-difference method evaluates a derivative through a weighted summation of function values from neighboring grid nodes. Conventional finite-difference weights can be calculated either from Taylor series expansions or by Lagrange interpolation polynomials. The finite-difference method can be interpreted as a truncated convolutional counterpart of the pseudospectral method in the space domain. For this reason, we also can derive finite-difference operators by truncating the convolution series of the pseudospectral method. Various truncation windows can be employed for this purpose and they result in finite-difference operators with different dispersion properties. We found that there exists two families of scaled binomial windows that can be used to derive conventional finite-difference operators analytically. With a minor change, these scaled binomial windows can also be used to derive optimized finite-difference operators with enhanced dispersion properties. © 2012 Society of Exploration Geophysicists.

  20. Determination of gold in geologic materials by solvent extraction and atomic-absorption spectrometry

    Science.gov (United States)

    Huffman, Claude; Mensik, J.D.; Riley, L.B.

    1967-01-01

    The two methods presented for the determination of traces of gold in geologic materials are the cyanide atomic-absorption method and the fire-assay atomic-absorption method. In the cyanide method gold is leached with a sodium-cyanide solution. The monovalent gold is then oxidized to the trivalent state and concentrated by extracting into methyl isobutyl ketone prior to estimation by atomic absorption. In the fire-assay atomic-absorption method, the gold-silver bead obtained from fire assay is dissolved in nitric and hydrochloric acids. Gold is then concentrated by extracting into methyl isobutyl ketone prior to determination by atomic absorption. By either method concentrations as low as 50 parts per billion of gold can be determined in a 15-gram sample.

  1. Ab initio determination of kinetics for atomic layer deposition modeling

    Science.gov (United States)

    Remmers, Elizabeth M.

    A first principles model is developed to describe the kinetics of atomic layer deposition (ALD) systems. This model requires no fitting parameters, as it is based on the reaction pathways, structures, and energetics obtained from quantum-chemical studies. Using transition state theory and partition functions from statistical mechanics, equilibrium constants and reaction rates can be calculated. Several tools were created in Python to aid in the calculation of these quantities, and this procedure was applied to two systems- zinc oxide deposition from diethyl zinc (DEZ) and water, and alumina deposition from trimethyl aluminum (TMA) and water. A Gauss-Jordan factorization is used to decompose the system dynamics, and the resulting systems of equations are solved numerically to obtain the temporal concentration profiles of these two deposition systems.

  2. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  3. Determination of three-dimensional atomic positions from tomographic reconstruction using ensemble empirical mode decomposition

    Science.gov (United States)

    Li, Po-Nan; Wu, Zong-Han; Hsiao, Chien-Nan; Lee, Ting-Kuo; Chen, Chien-Chun

    2016-08-01

    Tomographic reconstruction from a tilt series of electron micrographs has raised great interest in materials, chemical, and condensed matters science because of its capability of revealing 3D local atomic structures within nanomaterials. Previous breakthroughs have demonstrated that the positions of individual atoms can not only be visualized but also determined by combining a scanning transmission electron microscope with a high-angle annular dark-field detector, equally sloped tomography, and the filtering/denoising method. However, the filtering/denoising approach—whether imposed on 2D projections or 3D reconstruction—raises concerns regarding the robustness of image processing, the accuracy of atomic positions, and the artificial atoms introduced during filtering. In this article, we report a general method that overcomes these limitations. By removing unphysical oscillations in 2D projections through ensemble empirical mode decomposition and applying a standard Wiener filter to the 3D reconstruction, we are able to determine atomic structures with higher accuracy.

  4. Electrothermal atomization atomic absorption spectrometry for the determination of lead in urine: results of an interlaboratory study

    Science.gov (United States)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

    Results of an interlaboratory study are reported for the determination of lead in urine. Two levels of a lyophilized material containing biologically-bound lead were prepared using pooled urine obtained from lead-poisoned children undergoing the CaNa 2EDTA mobilization test. The materials were circulated to a group of reference laboratories that participate in the `New York State Proficiency Testing Program for Blood Lead'. Results of the initial round-robin gave all-method consensus target values of 145±22 μg/l (S.D.) for lot 17 and 449±43 μg/l (S.D.) for lot 20. The interlaboratory exercise was repeated some 5 years later and consensus target values were re-calculated using the grand mean (excluding outliers) of results reported by laboratories using electrothermal atomization atomic absorption spectrometry (ETAAS). The re-calculated target values were 139±10 μg/l (S.D.) and 433±12 μg/l (S.D.). The urine reference materials were also analyzed for lead by several laboratories using other instrumental techniques including isotope dilution (ID), inductively coupled plasma (ICP) mass spectrometry (MS), flame atomic absorption with extraction, ICP-atomic emission spectrometry, ID-gas chromatography MS and flow injection-hydride generation AAS, thus providing a rich source of analytical data with which to characterize them. The materials were also used in a long-term validation study of an ETAAS method developed originally for blood lead determinations that has since been used unmodified for the determination of lead in urine also. Recently, urine lead method performance has been tracked in a proficiency testing program specifically for this analysis. In addition, a number of commercial control materials have been analyzed and evaluated.

  5. Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Various experimental conditions were described for the vanadium determination by graphite furnace atomic ab-sorption spectroscopy (GFAAS). The experiments showed that when atomization took place under the conditions where thecombination of a pyrolytic coating graphite tube and fast raising temperature were used and the temperature was stable, thesignal peak shapes could be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curve method.

  6. The Cucker-Smale Equation: Singular Communication Weight, Measure-Valued Solutions and Weak-Atomic Uniqueness

    Science.gov (United States)

    Mucha, Piotr B.; Peszek, Jan

    2017-08-01

    The Cucker-Smale flocking model belongs to a wide class of kinetic models that describe a collective motion of interacting particles that exhibit some specific tendency, e.g. to aggregate, flock or disperse. This paper examines the kinetic Cucker-Smale equation with a singular communication weight. Given a compactly supported measure as an initial datum we construct a global in time weak measure-valued solution in the space {C_{weak}(0,∞;M)} . The solution is defined as a mean-field limit of the empirical distributions of particles, the dynamics of which is governed by the Cucker-Smale particle system. The studied communication weight is {ψ(s)=|s|^{-α}} with {α \\in (0, 1/2)} . This range of singularity admits the sticking of characteristics/trajectories. The second result concerns the weak-atomic uniqueness property stating that a weak solution initiated by a finite sum of atoms, i.e. Dirac deltas in the form {m_i δ_{x_i} ⊗ δ_{v_i}} , preserves its atomic structure. Hence these coincide with unique solutions to the system of ODEs associated with the Cucker-Smale particle system.

  7. Selenosugar determination in porcine liver using multidimensional HPLC with atomic and molecular mass spectrometry.

    Science.gov (United States)

    Lu, Ying; Pergantis, Spiros A

    2009-01-01

    A methodology based on liquid chromatography coupled online with atomic and molecular mass spectrometry was developed for identifying trace amounts of the selenosugar methyl 2-acetamido-2-deoxy-1-seleno-β-D-galactopyranoside (SeGalNAc) in porcine liver, obtained from an animal that had not received selenium supplementation. Sample preparation was especially critical for the identification of SeGalNAc by molecular mass spectrometry. This involved liver extraction using a Tris buffer, followed by sequential centrifugations. The resulting cytosolic fraction was pre-concentrated and the low molecular weight selenium (LMWSe) fraction obtained from a size exclusion column was collected, concentrated, and subsequently analyzed using a tandem dual-column HPLC-ICP-MS system which consisted of strong cation exchange (SCX) and reversed phase (RP) columns coupled in tandem. Hepatocytosolic SeGalNAc was tentatively identified by retention time matching and spiking. Its identity was further confirmed by using the same type of chromatography on-line with atmospheric pressure chemical ionization tandem mass spectrometry operated in the selected reaction monitoring (SRM) mode. Four SRM transitions, characteristic of SeGalNAc, were monitored and their intensity ratios determined in order to confirm SeGalNAc identification. Instrument limits of detection for SeGalNAc by SCX-RP HPLC-ICP-MS and SCX-RP HPLC-APCI-MS/MS were 3.4 and 2.9 μg Se L(-1), respectively. Selenium mass balance analysis revealed that trace amounts of SeGalNAc, 2.16±0.94 μg Se kg(-1) liver (wet weight) were present in the liver cytosol, corresponding to 0.4% of the total Se content in the porcine liver.

  8. Methods for determining healthy body weight in end stage renal disease.

    Science.gov (United States)

    Harvey, Kathy Schiro

    2006-07-01

    Several formulas for calculating desirable body weight are used in chronic kidney failure patients. Ideal body weight (IBW) derived from Metropolitan Life Insurance tables has been available since the 1950s. The Hamwi formula was proposed in the 1960s as a simple tool for quickly estimating desirable body weight, especially in people with diabetes. Since the 1970s, National Health and Nutrition Evaluation Surveys I, II, and III have provided an in-depth evaluation of the average body weights of Americans. These standard body weights (SBW) are often interpreted to be normal and healthy weight goals. Body mass index (BMI) has also been studied for decades and is used internationally as the standard for determining healthy weight, especially in relationship to obesity. These 4 methods are discussed and compared along with a brief review of the history of using the adjusted body weight (ABW) formulas, followed by recommendations for clinical practice.

  9. Using Weighted Graphs for Computationally Efficient WLAN Location Determination

    DEFF Research Database (Denmark)

    Thomsen, Bent; Hansen, Rene

    2007-01-01

    Indoor location-based services hold promise for a multitude of valuable services, but require micro-detailed geo-referencing not achievable with "outdoor" technologies such as GPS and cellular networks. A widely used technique for accurate indoor positioning is location fingerprinting which makes...... burden for large buildings and is thus problematic for tracking users in real time on processor-constrained mobile devices. In this paper we present a technique for improving the computational efficiency of the fingerprinting technique such that location determination becomes tractable on a mobile device...

  10. Speciation of zinc in low molecular weight proteins of breast milk and infant formulas by size exclusion chromatography/flame atomic absorption spectroscopy.

    Science.gov (United States)

    Bermejo, P; Peña, E M; Fompedriña, D; Domínguez, R; Bermejo, A; Cocho, J A; Fernández, J R; Fraga, J M

    2001-01-01

    Size exclusion chromatography (SEC) and flame atomic absorption spectroscopy (FAAS) were used for the separation of metal-containing species in milk whey. After milk ultracentrifugation, the sample was injected into a TSK-Gel G2000 glass column and eluted with 0.2M NH4NO3-NH3, pH 6.7. Low molecular weight proteins were fractionated, and the fractions were characterized by molecular weight. Zinc distributions were obtained by FAAS using a high performance nebulizer. The method was very sensitive (limit of detection = 2.6 x 10(-3) microg/mL; limit of quantitation = 8.9 x 10(-3) microg/mL) and precise (RSDs < or =10%). This method was applied to the determination of Zn in binding compounds in breast milk whey and in commercial cow's milk-based formulas. Distribution patterns were different. The presence of Zn in most fractions in breast milk was most significant, whereas in infant formulas Zn was detected only in fractions of molecular weight <5 kDa and in the highest molecular weight peak.

  11. Determination of cadmium and lead in urine by derivative flame atomic absorption spectrometry using the atom trapping technique

    Science.gov (United States)

    Han-wen, Sun; De-qiang, Zhang; Li-li, Yang; Jian-min, Sun

    1997-06-01

    A method is described for the determinations of cadmium and lead in urine by derivative flame atomic absorption spectrometry with a modified water-cooled stainless steel atom trapping tube. The effects of the trap position, the flame conditions, the coolant flow rates, and the collection time were studied. With a 1 min collection time, the characteristic concentrations (derivative absorbance of 0.0044) for cadmium and lead were 0.028 and 1.4 μg L -1, the detection limits (3σ) were 0.02 and 0.27 μg L -1, respectively. The detection limits and sensitivities of the proposed method were 2 and 3 orders of magnitude higher for 1-3 min collection time than those of conventional flame atomic absorption spectrometry for cadmium and lead, respectively. Urine samples from a small population of normal individuals have been analyzed for cadmium and lead by the proposed method. Satisfactory recoveries of 91-110% and 91-106%, for Cd and Pb were obtained with these urine samples.

  12. Determination of Weight Suspension Rigidity in the Transport-Erector Aggregates

    Directory of Open Access Journals (Sweden)

    V. A. Zverev

    2016-01-01

    Full Text Available The aim is to determine weight suspension rigidity in aggregates designed to perform technological transport-erector operations at the miscellaneous launch complexes.We consider the weight suspension comprising the following distinctive structural components: the executive weight-lowering mechanism, polyspast mechanism, rope, traverse, and rods. A created structural dynamic model of suspension allowed us to define weight suspension rigidity. Within the framework of design analysis of a dynamic model we determined the rigidity of its structural units, i.e. traverse, rope, and polyspast.Known analytical relationships were used to calculate the rope rigidity. To determine rigidity of polyspast and traverse have been created special models based on the finite element method. For each model deformation in the specific points under the test load have been defined. Data obtained were used to determine trigidity of traverses and polyspast, and also rigidity of suspension in total. The rigidity models of polispast mechanism and traverse have been developed and calculated using the software complex "Zenit-95".As the research results, the paper presents a dynamic model of the weight suspension of the transport-erector aggregate, the finite element models of the polispast mechanism and traverse, an algorithm for determining the weight suspension rigidity and relevant analytical relationships.Independent calculation of weight suspension rigidity enables us to simplify further dynamic calculation of the aggregate-weight system because it allows attaining a simpler model of the aggregate-weight system that uses the weight suspension model as an element of equivalent rigidity. Despite this simplification the model allows us to determine correctly weight movement parameters and overloads in the aggregate-weight system in the process of technical operations.

  13. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Morzan, Ezequiel; Piano, Ornela; Stripeikis, Jorge; Tudino, Mabel, E-mail: tudino@qi.fcen.uba.ar

    2012-11-15

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 {mu}g mL{sup -1}, sensitivity: 0.306 ({mu}g mL{sup -1}){sup -1}, RSD% (n = 10, 1 {mu}g mL{sup -1}): 2.5, linear range: 0.01-4 {mu}g mL{sup -1} and sample throughput: 72 h{sup -1}. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided. - Highlights: Black-Right-Pointing-Pointer Quartz tubes as furnaces in TS-FFAAS. Black-Right-Pointing-Pointer Small tubes for controlling radial dispersion. Black-Right-Pointing-Pointer Improved figures of merit for gold determination. Black-Right-Pointing-Pointer Analysis of homeopathic medicines.

  14. A generic procedure for determining atomic LS spectral terms and their LS eigenfunctions

    Institute of Scientific and Technical Information of China (English)

    Xiong Zhuang; Bacalis N C

    2009-01-01

    This paper develops a Fortran code which is capable to construct the simplest LS eigcnfunctions for desired symmetry and determine all permitted atomic LS spectral terms under a given orbital occupancy by implementing and extending the Schaefer and Harris method. Examples (in some cases the most complete set to date) of multiple spectroscopic terms of LS coupling of atomic states for both non-equlvalent and equivalent electronic configurations arc given. It also corrects a few observed errors from the recent literature.

  15. Determination of $\\pi\\pi$ scattering lengths from measurement of $\\pi^+\\pi^-$ atom lifetime

    CERN Document Server

    Adeva, B; Benayoun, M; Benelli, A; Berka, Z; Brekhovskikh, V; Caragheorgheopol, G; Cechak, T; Chiba, M; Chliapnikov, P V; Ciocarlan, C; Constantinescu, S; Costantini, S; Curceanu, C; Doskarova, P; Dreossi, D; Drijard, D; Dudarev, A; Ferro-Luzzi, M; Fungueiriño Pazos, J L; Gallas Torreira, M; Gerndt, J; Gianotti, P; Goldin, D; Gomez, F; Gorin, A; Gorchakov, O; Guaraldo, C; Gugiu, M; Hansroul, M; Hons, Z; Hosek, R; Iliescu, M; Karpukhin, V; Kluson, J; Kobayashi, M; Kokkas, P; Komarov, V; Kruglov, V; Kruglova, L; Kulikov, A; Kuptsov, A; Kuroda, K I; Lamberto, A; Lanaro, A; Lapshin, V; Lednicky, R; Leruste, P; Levi Sandri, P; Lopez Aguera, A; Lucherini, V; Maki, T; Manuilov, I; Marin, J; Narjoux, J L; Nemenov, L; Nikitin, M; Nunez Pardo, T; Okada, K; Olchevskii, V; Pazos, A; Pentia, M; Penzo, A; Perreau, J M; Plo, M; Ponta, T; Rappazzo, G F; Riazantsev, A; Rodriguez, J M; Rodriguez Fernandez, A; Romero Vidal, A; Ronjin, V.M.; Rykalin, V; Saborido, J; Santamarina, C; Schacher, J; Schuetz, C; Sidorov, A; Smolik, J; Takeutchi, F; Tarasov, A; Tauscher, L; Tobar, M J; Trojek, T; Trusov, S; Utkin, V; Vazquez Doce, O; Vlachos, S; Voskresenskaya, O; Vrba, T; Willmott, C; Yazkov, V; Yoshimura, Y; Zhabitsky, M; Zrelov, P

    2011-01-01

    The DIRAC experiment at CERN has achieved a sizeable production of $\\pi^+\\pi^-$ atoms and has significantly improved the precision on its lifetime determination. From a sample of 21227 atomic pairs, a 4% measurement of the S-wave $\\pi\\pi$ scattering length difference $|a_0-a_2| = (.0.2533^{+0.0080}_{-0.0078}|_\\mathrm{stat}.{}^{+0.0078}_{-0.0073}|_\\mathrm{syst})M_{\\pi^+}^{-1}$ has been attained, providing an important test of Chiral Perturbation Theory.

  16. Some problems connected with boron determination by atomic absorption spectroscopy and the sensitivity improvement

    Directory of Open Access Journals (Sweden)

    JELENA J. SAVOVIC

    2001-08-01

    Full Text Available Two atomizers were compared: an N2O–C2H2 flame and a stabilized U-shaped DC arc with aerosol supply. Both the high plasma temperature and the reducing atmosphere obtained by acetylene addition to the argon stream substantially increase the sensitivity of boron determination by atomic absorption spectroscopy (AAS when the arc atomizer is used. The results were compared with those for silicon as a control element. The experimental characteristic concentrations for both elements were compared with the computed values. The experimentally obtained characteristic concentration for boron when using the arc atomizer was in better agreement with the calculated value. It was estimated that the influence of stable monoxide formation on the sensitivity for both elements was about the same, but reduction of analyte and formation of non-volatile carbide particles was more important for boron, which is the main reason for the low sensitivity of boron determination using a flame atomizer. The use of an arc atomizer suppresses this interference and significantly improves the sensitivity of the determination.

  17. Determination of the Relative Atomic Masses of Metals by Liberation of Molecular Hydrogen

    Science.gov (United States)

    Waghorne, W. Earle; Rous, Andrew J.

    2009-01-01

    Students determine the relative atomic masses of calcium, magnesium, and aluminum by reaction with hydrochloric acid and measurement of the volume of hydrogen gas liberated. The experiment demonstrates stoichiometry and illustrates clearly that mass of the reagent is not the determinant of the amounts in chemical reactions. The experiment is…

  18. Determination of the Relative Atomic Masses of Metals by Liberation of Molecular Hydrogen

    Science.gov (United States)

    Waghorne, W. Earle; Rous, Andrew J.

    2009-01-01

    Students determine the relative atomic masses of calcium, magnesium, and aluminum by reaction with hydrochloric acid and measurement of the volume of hydrogen gas liberated. The experiment demonstrates stoichiometry and illustrates clearly that mass of the reagent is not the determinant of the amounts in chemical reactions. The experiment is…

  19. History of the recommended atomic-weight values from 1882 to 1997: A comparision of differences from current values to the estimated uncertainties of earlier values.

    Science.gov (United States)

    Coplen, T.B.; Peiser, H.S.

    1998-01-01

    International commissions and national committees for atomic weights (mean relative atomic masses) have recommended regularly updated, best values for these atomic weights as applicable to terrestrial sources of the chemical elements. Presented here is a historically complete listing starting with the values in F. W. Clarke's 1882 recalculation, followed by the recommended values in the annual reports of the American Chemical Society's Atomic Weights Commission. From 1903, an International Commission published such reports and its values (scaled to an atomic weight of 16 for oxygen) are here used in preference to those of national committees of Britain, Germany, Spain, Switzerland, and the U.S.A. We have, however, made scaling adjustments from Ar(16O) to Ar(12C) where not negligible. From 1920, this International Commission constituted itself under the International Union of Pure and Applied Chemistry (IUPAC). Since then, IUPAC has published reports (mostly biennially) listing the recommended atomic weights, which are reproduced here. Since 1979, these values have been called the "standard atomic weights" and, since 1969, all values have been published, with their estimated uncertainties. Few of the earlier values were published with uncertainties. Nevertheless, we assessed such uncertainties on the basis of our understanding of the likely contemporary judgement of the values' reliability. While neglecting remaining uncertainties of 1997 values, we derive "differences" and a retrospective index of reliability of atomic-weight values in relation to assessments of uncertainties at the time of their publication. A striking improvement in reliability appears to have been achieved since the commissions have imposed upon themselves the rule of recording estimated uncertainties from all recognized sources of error.

  20. Direct determination of arsenic in petroleum derivatives by graphite furnace atomic absorption spectrometry: A comparison between filter and platform atomizers

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene; Rampazzo, Roger T.; Dessuy, Morgana B. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Silva, Marcia M. da [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Katskov, Dmitri A. [Tshwane University of Technology (TUT), Faculty of Science, Chemistry Department, Pretoria 0001 (South Africa)

    2011-05-15

    In the present work a direct method for the determination of arsenic in petroleum derivatives has been developed, comparing the performance of a commercial transversely heated platform atomizer (THPA) with that of a transversely heated filter atomizer (THFA). The THFA results in a reduction of background absorption and an improved sensitivity as has been reported earlier for this atomizer. The mixture of 0.1% (m/v) Pd + 0.03% (m/v) Mg + 0.05% (v/v) Triton X-100 was used as the chemical modifier for both atomizers. The samples (naphtha, gasoline and petroleum condensate) were stabilized in the form of a three-component solution (detergentless microemulsion) with the sample, propan-1-ol and 0.1% (v/v) HNO{sub 3} in a ratio of 3.0:6.4:0.6. The characteristic mass of 13 pg found in the THFA was about a factor of two better than that of 28 pg obtained with the THPA; however, the limits of detection (LOD) and quantification (LOQ) were essentially the same for both atomizers (1.9 and 6.2 {mu}g L{sup -1}, respectively, for THPA, and 1.8 and 5.9 {mu}g L{sup -1}, respectively, for THFA) due to the increased noise observed with the THFA. A possible explanation for that is a partial blockage of the radiation from the hollow cathode lamp by the narrow inner diameter of this tube and the associated loss of radiation energy. Due to the lack of an appropriate certified reference material, recovery tests were carried out with inorganic and organic arsenic standards and the results were between 89% and 111%. The only advantage of the THFA found in this work was a reduction of the total analysis time by about 20% due to the 'hot injection' that could be realized with this furnace. The arsenic concentrations varied from < LOQ to 43.3 {mu}g L{sup -1} in the samples analyzed in this work.

  1. A proposed method for determination of weighted despreading sequences for a DS/CDMA system

    OpenAIRE

    Jabrane, Younes; Iqdour, Radouane; Ait Es Said, Brahim; Naja, Najib

    2007-01-01

    The steeping chip weighting waveforms are used in multiple access interference cancellation by emphasizing the received spreading signal, therefore, that allows to solve the problem of orthogonality for the chip waveforms. Our paper presents a useful method based on fuzzy systems to determine the despreading sequences weighted by the steeping chip weighting waveforms for Direct Sequence Code Division Multiple Access DS/CDMA. The validity of our proposed method has been tested by numerical exa...

  2. Determining Component Weights in a Communications Assessment Using Judgmental Policy Capturing.

    Science.gov (United States)

    Harvill, Leo M; Lang, F Forrest; McCord, Ronald S

    2004-12-01

    Tools are needed for determining appropriate weights for complex performance assessment components in medical education. The feasibility of using judgmental policy capturing (JPC), a procedure to statistically describe the information processing strategies of experts, for this purpose was investigated. Iterative JPC was used to determine appropriate weighting for the six core communication skill scores from a communications objective structured clinical examination (OSCE) for medical students using a panel of four communication skill experts. The mean regression weights from the panel indicated they placed less importance on information management (8.5%), moderate and nearly equal importance on rapport building (15.8%), agenda setting (15.4%), and addressing feelings (14.1%), and greater importance on active listening (20.1%) and reaching common ground with the patient (25.5%). JPC is an effective procedure for determining appropriate weights for complex clinical assessment components. The derived weights may be very different for those assessment components.

  3. Determinants of Weight Loss prior to Diagnosis in Inflammatory Bowel Disease: A Retrospective Observational Study

    Directory of Open Access Journals (Sweden)

    Yasser Elsherif

    2014-01-01

    Full Text Available Aims. To identify prevalence, severity, and environmental determinants of weight loss in inflammatory bowel disease (IBD patients just prior to time of formal diagnosis. Methodology. IBD patients attending outpatient clinic were questioned about weight loss prior to diagnosis and other environmental and demographic variables. The percentage BMI loss was calculated for each subject and factors associated with weight loss were determined. Results. Four hundred and ninety-four subjects were recruited (237 cases of Crohn’s disease (CD and 257 cases of ulcerative colitis (UC. Overall, 57% of subjects with CD and 51% of subjects with UC experienced significant weight loss prior to diagnosis (>5% BMI loss. Younger age at diagnosis and history of previous IBD surgery were significantly associated with both lower BMI at diagnosis and increased weight loss prior to diagnosis. In CD patients, increasing age at diagnosis was inversely associated with weight loss prior to diagnosis. Ileal disease was a risk factor of weight loss, whereas prior appendectomy was associated with reduced risk of weight loss. Conclusions. Weight loss is a significant problem for many IBD patients at presentation, especially in younger age and CD with ileal involvement. Appendectomy is associated with diminished weight loss.

  4. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  5. Leisure-time activity is an important determinant of long-term weight maintenance after weight loss in the Sibutramine Trial on Obesity Reduction and Maintenance (STORM trial)

    DEFF Research Database (Denmark)

    van Baak, Marleen A; van Mil, Edgar; Astrup, Arne V

    2003-01-01

    The success rate of long-term maintenance of weight loss in obese patients is usually low. To improve the success rate, determinants of long-term weight maintenance must be identified.......The success rate of long-term maintenance of weight loss in obese patients is usually low. To improve the success rate, determinants of long-term weight maintenance must be identified....

  6. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...... were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well...

  7. Determination of total magnesium in biological samples using electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Hulanicki, Adam; Godlewska, Beata; Brzóska, Malgorzata

    1995-11-01

    Magnesium content is an important diagnostic parameter in medicine. It is recognized that its determination in one compartment is not sufficient for reliable information about the magnesium status in the body. In addition to the common procedures of magnesium determination in blood by flame atomic absorption spectrometry, the procedure of electrothermal atomization has also been developed and applied to the analysis of blood fractions, mononuclear cells and isolated nuclei of liver cells. Electrothermal atomization is preferred in cases where the sample size is limited and the magnesium content low. The total errors are in the order of 3-4%. Various techniques of sample pretreatment have been tested and direct dilution with 0.05 mol l -1 nitric acid was optimal when the samples were not mineralized. The calibration graph based on standards containing albumin was found to give the best results, as the form of magnesium in the samples may influence the ashing and atomization processes. Good agreement was obtained for determination of magnesium in standard serum. The results are compared with those obtained by the standard flame atomization technique.

  8. Two-step laser excited atomic fluorescence spectrometry determination of mercury

    Science.gov (United States)

    Resto, W.; Badini, R. G.; Smith, B. W.; Stevenson, C. L.; Winefordner, J. D.

    1993-04-01

    A novel method for the determination of mercury by laser excited atomic fluorescence with electrothermal atomization (LEAFS-ETA) has been developed. The experimental set-up consisted of a dual dye-laser system pumped with a XeCl excimer laser operated at 10 Hz, and an electrothermal atomizer with platform atomization. The atomization program allowed time for the injection of Pd (as a matrix modifier) and used a drying step at 110°C and an atomization step at 1200°C. The collection is made at 90° using a pierced mirror, an achromat lens and a long-pass filter. The monochromator is fitted with a 1P28 PMT. The signal is processed by using a boxcar and an analog to digital interface. The excitation scheme is a two-step process, with λ 1 = 253.7 nm and λ 2 = 435.8 nm. Direct fluorescence is observed at 546.1 nm. The limit of detection (LOD) obtained is 90 fg (9 pptr with 10 μ1 injection). The linear dynamic range (LDR) is five orders of magnitude and is limited by the non-linearity of the co-operative processes occurring at higher concentrations. In order to extend the LDR to higher amounts of mercury, indirect fluorescence is collected with the less sensitive line at 407.8 nm, allowing concentrations of 1 ppm and up to be measured, extending the LDR of the technique to at least seven orders of magnitude.

  9. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  10. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed...

  11. Chemical modifiers in electrothermal atomic absorption determination of Platinum and Palladium containing preparations in blood serum

    Directory of Open Access Journals (Sweden)

    Аntonina Alemasova

    2012-11-01

    Full Text Available The biological liquids matrixes influence on the characteristic masses and repeatability of Pt and Pd electrothermal atomic absorption spectroscopy (ETAAS determination was studied. The chemical modifiers dimethylglyoxime and ascorbic acid for matrix interferences elimination and ETAAS results repeatability improvement were proposed while bioliquids ETAAS analysis, and their action mechanism was discussed.

  12. Quantitative Determination of Arsenic in Bottled Drinking Water Using Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    Maria Guţu Claudia

    2013-10-01

    Full Text Available Background: Many studies have been performed in the past few years, to determine arsenic speciation in drinking water, food chain and environment, arsenic being a well-recognized carcinogenic and toxic agent mainly in its inorganic species. The instrumental techniques used for arsenic determination, such as hydride generation atomic absorption spectrometry (HGAAS, graphite furnace atomic absorption spectrometry (GFAAS and inductively coupled plasma mass spectrometry (ICP-MS, can provide a great sensitivity only on the total amount. Objective: The aim of this study was to develop a simple and rapid method and to analyze the concentration of total inorganic arsenic in bottled drinking water. Methods: Total arsenic was determined in samples from six different types of commercially available bottled drinking water using atomic absorption spectrometry with electrothermal or hydride generation vaporisation. All drinking water samples were acidified with 0.1M nitric acid to match the acidity of the standards. Results: The method was linear within the studied range (1-5 μg/L, R = 0.9943. The quantification limits for arsenic determination were 0.48 μg/L (HGAAS and 0.03 μg/L (GFAAS. The evaluated arsenic content in drinking water was within the accepted limits provided by law. Conclusions: A simple and sensitive method for the quantification of arsenic in drinking water using atomic absorbtion spectroscopy was described, which can be further used in toxicological studies. As an additional advantage, the system is very fast, efficient and environmental friendly

  13. Micro determination of plasma and erythrocyte copper by atomic absorption spectrophotometry

    Science.gov (United States)

    Blomfield, Jeanette; Macmahon, R. A.

    1969-01-01

    The free and total plasma copper and total erythrocyte copper levels have been determined by simple, yet sensitive and highly specific methods, using atomic absorption spectrophotometry. For total copper determination, the copper was split from its protein combination in plasma or red cells by the action of hydrochloric acid at room temperature. The liberated copper was chelated by ammonium pyrrolidine dithiocarbamate and extracted into n-butyl acetate by shaking and the organic extract was aspirated into the atomic absorption spectrophotometer flame. The entire procedure was carried out in polypropylene centrifuge tubes, capped during shaking. For the free plasma copper measurement the hydrochloric acid step was omitted. Removal of the plasma or erythrocyte proteins was found to be unnecessary, and, in addition, the presence of trichloracetic acid caused an appreciable lowering of absorption. Using a double-beam atomic absorption spectrophotometer and scale expansion × 10, micro methods have been derived for determining the total copper of plasma or erythrocytes with 0·1 ml of sample, and the free copper of plasma with 0·5 ml. The macro plasma copper method requires 2 ml of plasma and is suitable for use with single-beam atomic absorption spectrophotometers. With blood from 50 blood donors, normal ranges of plasma and erythrocyte copper have been determined. PMID:5776543

  14. DETERMINING BERYLLIUM IN DRINKING WATER BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY

    Science.gov (United States)

    A direct graphite furnace atomic absorption spectroscopy method for the analysis of beryllium in drinking water has been derived from a method for determining beryllium in urine. Ammonium phosphomolybdate and ascorbic acid were employed as matrix modifiers. The matrix modifiers s...

  15. DETERMINATION OF COPPER AND ZINC IN MINERAL WATERS BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

    Directory of Open Access Journals (Sweden)

    Tatiana Mitina

    2011-12-01

    Full Text Available The content of copper and zinc in mineral waters were determined by atomic spectroscopy with preliminary extraction of metals. Validation of the technique was carried out by the method of standard additions and proved the reliability of analytical data.

  16. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  17. Determination of a high spatial resolution geopotential model using atomic clock comparisons

    OpenAIRE

    Lion, Guillaume; Panet, Isabelle; Wolf, Peter; Guerlin, Christine; Bize, Sébastien; Delva, Pacôme

    2016-01-01

    Recent technological advances in optical atomic clocks are opening new perspectives for the direct determination of geopotential differences between any two points at a centimeter-level accuracy in geoid height. However, so far detailed quantitative estimates of the possible improvement in geoid determination when adding such clock measurements to existing data are lacking. We present a first step in that direction with the aim and hope of triggering further work and efforts in this emerging ...

  18. Site specific incorporation of heavy atom-containing unnatural amino acids into proteins for structure determination

    Science.gov (United States)

    Xie, Jianming; Wang, Lei; Wu, Ning; Schultz, Peter G.

    2008-07-15

    Translation systems and other compositions including orthogonal aminoacyl tRNA-synthetases that preferentially charge an orthogonal tRNA with an iodinated or brominated amino acid are provided. Nucleic acids encoding such synthetases are also described, as are methods and kits for producing proteins including heavy atom-containing amino acids, e.g., brominated or iodinated amino acids. Methods of determining the structure of a protein, e.g., a protein into which a heavy atom has been site-specifically incorporated through use of an orthogonal tRNA/aminoacyl tRNA-synthetase pair, are also described.

  19. A method for determining customer requirement weights based on TFMF and TLR

    Science.gov (United States)

    Ai, Qingsong; Shu, Ting; Liu, Quan; Zhou, Zude; Xiao, Zheng

    2013-11-01

    'Customer requirements' (CRs) management plays an important role in enterprise systems (ESs) by processing customer-focused information. Quality function deployment (QFD) is one of the main CRs analysis methods. Because CR weights are crucial for the input of QFD, we developed a method for determining CR weights based on trapezoidal fuzzy membership function (TFMF) and 2-tuple linguistic representation (TLR). To improve the accuracy of CR weights, we propose to apply TFMF to describe CR weights so that they can be appropriately represented. Because the fuzzy logic is not capable of aggregating information without loss, TLR model is adopted as well. We first describe the basic concepts of TFMF and TLR and then introduce an approach to compute CR weights. Finally, an example is provided to explain and verify the proposed method.

  20. Determination of the presence of hyaluronic acid in preparations containing amino acids: the molecular weight characterization.

    Science.gov (United States)

    Bellomaria, A; Nepravishta, R; Mazzanti, U; Marchetti, M; Piccioli, P; Paci, M

    2014-10-15

    Several pharmaceutical preparations contain hyaluronic acid in the presence of a large variety of low molecular weight charged molecules like amino acids. In these mixtures, it is particularly difficult to determine the concentration and the molecular weight of the hyaluronic acid fragments. In fact zwitterionic compounds in high concentration behave by masking the hyaluronic acid due to the electrostatic interactions between amino acids and hyaluronic acid. In such conditions the common colorimetric test of the hyaluronic acid determination appears ineffective and in the (1)H NMR spectra the peaks of the polymer disappear completely. By a simple separation procedure the presence of hyaluronic acid was revealed by the DMAB test and (1)H NMR while its average molecular weight in the final product was determined by DOSY NMR spectroscopy alone. The latter determination is very important due to the healthy effects of some sizes of this polymer's fragments.

  1. Estimating and verifying soil unit weight determined on the basis of SCPTu tests

    Directory of Open Access Journals (Sweden)

    Bagińska Irena

    2016-09-01

    Full Text Available The unit weight, as a basic physical feature of soil, is an elementary quantity, and knowledge of this parameter is necessary in each geotechnical and geo-engineering task. Estimation of this quantity can be made with both laboratory and field techniques. The paper comprises a multi-scale evaluation of unit weight of cohesive soil, based on several measurements made in nearby locations using the SCPTu static probe. The procedures used were based on the two classifications and two solutions from literature. The results were referenced to the actual values of unit weight determined with a direct procedure from undisturbed samples. The resulting solutions were the basis for proposing a new formula to determine the soil unit weight from SCPTu measurements, as well as comparative analysis using exemplary values taken from the national Polish standard.

  2. An accurate determination of the Avogadro constant by counting the atoms in a 28Si crystal

    CERN Document Server

    Andreas, B; Bartl, G; Becker, P; Bettin, H; Borys, M; Busch, I; Gray, M; Fuchs, P; Fujii, K; Fujimoto, H; Kessler, E; Krumrey, M; Kuetgens, U; Kuramoto, N; Mana, G; Manson, P; Massa, E; Mizushima, S; Nicolaus, A; Picard, A; Pramann, A; Rienitz, O; Schiel, D; Valkiers, S; Waseda, A

    2010-01-01

    The Avogadro constant links the atomic and the macroscopic properties of matter. Since the molar Planck constant is well known via the measurement of the Rydberg constant, it is also closely related to the Planck constant. In addition, its accurate determination is of paramount importance for a definition of the kilogram in terms of a fundamental constant. We describe a new approach for its determination by "counting" the atoms in 1 kg single-crystal spheres, which are highly enriched with the 28Si isotope. It enabled isotope dilution mass spectroscopy to determine the molar mass of the silicon crystal with unprecedented accuracy. The value obtained, 6.02214084(18) x 10^23 mol^-1, is the most accurate input datum for a new definition of the kilogram.

  3. [Determination of trace selenium in edible fungi with graphite furnace atomic absorption spectroscopy].

    Science.gov (United States)

    Tie, Mei; Zhang, Wei; Li, Jing; Jing, Kui; Zang, Shu-liang; Li, Hua-wei

    2006-01-01

    In the present article, samples were digested by a quartz high-pressure digestion pot, reducing the loss of selenium in digestion. The content of selenium in edible fungi was determined by using graphite furnace atomic absorption spectroscopy, and the results showed that when the content of selenium in edible fungi was determined by using 1% Ni(NO3)2 as a matrix modifier, ashing temperature of 500 degreed C, and atomization temperature of 2 500 degrees C, and rectifying background by deuterium light, the recovery was in the range of 92.1%-115.5%, the relative standard deviation of the method was 1.28%, and the limit of detection was 15.8 microg x L(-1). The method was suitable for the determination of trace selenium in edible fungi with the advantages of being simple, rapid, sensitive, stable and accurate etc., and the results were satisfactory.

  4. Sample tilt effects on atom column position determination in ABF–STEM imaging

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Dan, E-mail: D.Zhou@fkf.mpg.de [Max Planck Institute for Solid State Research, Stuttgart Center for Electron Microscopy, Heisenbergstrasse 1, 70569 Stuttgart (Germany); Müller-Caspary, Knut [Institut für Festkörperphysik, Universität Bremen, Otto-Hahn-Allee 1, D-28359 Bremen (Germany); Sigle, Wilfried [Max Planck Institute for Solid State Research, Stuttgart Center for Electron Microscopy, Heisenbergstrasse 1, 70569 Stuttgart (Germany); Krause, Florian F.; Rosenauer, Andreas [Institut für Festkörperphysik, Universität Bremen, Otto-Hahn-Allee 1, D-28359 Bremen (Germany); Aken, Peter A. van [Max Planck Institute for Solid State Research, Stuttgart Center for Electron Microscopy, Heisenbergstrasse 1, 70569 Stuttgart (Germany)

    2016-01-15

    The determination of atom positions from atomically resolved transmission electron micrographs is fundamental for the analysis of crystal defects and strain. In recent years annular bright-field (ABF) imaging has become a popular imaging technique owing to its ability to map both light and heavy elements. Contrast formation in ABF is partially governed by the phase of the electron wave, which renders the technique more sensitive to the tilt of the electron beam with respect to the crystal zone axis than high-angle annular dark-field imaging. Here we show this sensitivity experimentally and use image simulations to quantify this effect. This is essential for error estimation in future quantitative ABF studies. - Highlights: • Experimental observations of deviations of atom column position in ABF–STEM imaging. • Quantification of the deviations for different convergence semi-angles, collection semi-angles and tilt amounts for an aberration-free probe. • Suggestions on minimizing the errors in the atom column position determination by ABF imaging.

  5. Kinetic theory and atomic physics corrections for determination of ion velocities from charge-exchange spectroscopy

    Science.gov (United States)

    Muñoz Burgos, J. M.; Burrell, K. H.; Solomon, W. M.; Grierson, B. A.; Loch, S. D.; Ballance, C. P.; Chrystal, C.

    2013-09-01

    Charge-exchange spectroscopy is a powerful diagnostic tool for determining ion temperatures, densities and rotational velocities in tokamak plasmas. This technique depends on detailed understanding of the atomic physics processes that affect the measured apparent velocities with respect to the true ion rotational velocities. These atomic effects are mainly due to energy dependence of the charge-exchange cross-sections, and in the case of poloidal velocities, due to gyro-motion of the ion during the finite lifetime of the excited states. Accurate lifetimes are necessary for correct interpretation of measured poloidal velocities, specially for high density plasma regimes on machines such as ITER, where l-mixing effects must be taken into account. In this work, a full nl-resolved atomic collisional radiative model coupled with a full kinetic calculation that includes the effects of electric and magnetic fields on the ion gyro-motion is presented for the first time. The model directly calculates from atomic physics first principles the excited state lifetimes that are necessary to evaluate the gyro-orbit effects. It is shown that even for low density plasmas where l-mixing effects are unimportant and coronal conditions can be assumed, the nl-resolved model is necessary for an accurate description of the gyro-motion effects to determine poloidal velocities. This solution shows good agreement when compared to three QH-mode shots on DIII-D, which contain a wide range of toroidal velocities and high ion temperatures where greater atomic corrections are needed. The velocities obtained from the model are compared to experimental velocities determined from co- and counter-injection of neutral beams on DIII-D.

  6. The determination of aluminum, copper, iron, and lead in glycol formulations by atomic absorption spectroscopy

    Science.gov (United States)

    1977-01-01

    Initial screening tests and the results obtained in developing procedures to determine Al, Cu, Fe, and Pb in glycol formulations are described. Atomic absorption completion was selected for Cu, Fe and Pb, and after comparison with emission spectroscopy, was selected for Al also. Before completion, carbon, iron, and lead are extracted with diethyl dithio carbamate (DDC) into methyl isobutyl ketone (MIBK). Aluminum was also extracted into MIBK using 8-hydroxyquinoline as a chelating agent. As little as 0.02 mg/l carbon and 0.06 mg/l lead or iron may be determined in glycol formulations. As little as 0.3 mg/l aluminum may be determined.

  7. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  8. Mixing weight determination for retrieving optical properties of polluted dust with MODIS and AERONET data

    Science.gov (United States)

    Chang, Kuo-En; Hsiao, Ta-Chih; Hsu, N. Christina; Lin, Neng-Huei; Wang, Sheng-Hsiang; Liu, Gin-Rong; Liu, Chian-Yi; Lin, Tang-Huang

    2016-08-01

    In this study, an approach in determining effective mixing weight of soot aggregates from dust-soot aerosols is proposed to improve the accuracy of retrieving properties of polluted dusts by means of satellite remote sensing. Based on a pre-computed database containing several variables (such as wavelength, refractive index, soot mixing weight, surface reflectivity, observation geometries and aerosol optical depth (AOD)), the fan-shaped look-up tables can be drawn out accordingly for determining the mixing weights, AOD and single scattering albedo (SSA) of polluted dusts simultaneously with auxiliary regional dust properties and surface reflectivity. To validate the performance of the approach in this study, 6 cases study of polluted dusts (dust-soot aerosols) in Lower Egypt and Israel were examined with the ground-based measurements through AErosol RObotic NETwork (AERONET). The results show that the mean absolute differences could be reduced from 32.95% to 6.56% in AOD and from 2.67% to 0.83% in SSA retrievals for MODIS aerosol products when referenced to AERONET measurements, demonstrating the soundness of the proposed approach under different levels of dust loading, mixing weight and surface reflectivity. Furthermore, the developed algorithm is capable of providing the spatial distribution of the mixing weights and removing the requirement to assume that the dust plume properties are uniform. The case study further shows the spatially variant dust-soot mixing weight would improve the retrieval accuracy in AODmixture and SSAmixture about 10.0% and 1.4% respectively.

  9. Automatic weight determination in nonlinear model predictive control of wind turbines using swarm optimization technique

    Science.gov (United States)

    Tofighi, Elham; Mahdizadeh, Amin

    2016-09-01

    This paper addresses the problem of automatic tuning of weighting coefficients for the nonlinear model predictive control (NMPC) of wind turbines. The choice of weighting coefficients in NMPC is critical due to their explicit impact on efficiency of the wind turbine control. Classically, these weights are selected based on intuitive understanding of the system dynamics and control objectives. The empirical methods, however, may not yield optimal solutions especially when the number of parameters to be tuned and the nonlinearity of the system increase. In this paper, the problem of determining weighting coefficients for the cost function of the NMPC controller is formulated as a two-level optimization process in which the upper- level PSO-based optimization computes the weighting coefficients for the lower-level NMPC controller which generates control signals for the wind turbine. The proposed method is implemented to tune the weighting coefficients of a NMPC controller which drives the NREL 5-MW wind turbine. The results are compared with similar simulations for a manually tuned NMPC controller. Comparison verify the improved performance of the controller for weights computed with the PSO-based technique.

  10. Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

    Science.gov (United States)

    Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

    2006-04-11

    A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

  11. Determination of Trace Iron in High Purity Sodium Fluoride by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A method is described for the direct determination of iron in high purity sodium fluoride using graphite furnace atomic absorption spectrometry. Interferences caused by the matrix are investigated. It is shown that the ashing temperature can be increased to 1 400°C and matrix interferences eliminated, the sensi tivity of iron increased in 1.27 fold by the addition of nickel nitrate. The method is applied to the determina tion of iron in sodium fluoride and satisfactory results are obtained.

  12. Determination of diethyllead in the urine by flameless atomic absorption spectrometry.

    OpenAIRE

    Turlakiewicz, Z; Jakubowski, M.; Chmielnicka, J

    1985-01-01

    A method for the determination of diethyllead in urine by flameless atomic absorption spectrometry after chelation with glyoxal-bis (2-hydroxyanil) and extraction of the formed complex with methyl isobutyl ketone is described. The method is specific in relation to both triethyllead and inorganic lead. The limit of detection was 3.2 micrograms Pb/l and the relative standard deviation in the concentration range 20-100 micrograms Pb/l was 0.076.

  13. Determination of Uranium in Apatite Minerals by Solvent Extraction--Inductively Coupled Plasma Atomic Emission Spectrometry

    OpenAIRE

    1993-01-01

    [Abstract] Solvent, extraction-ICP atomic emission spectrometry was applied to the determination of uranium in apatite minerals. Apatite minerals were treated with nitric acid. After removing a small quantity of insoluble residue, uranium was extracted with 0.05 mol/dm^3 1-phonyl-3-mcthyl-4-trifluoroacetyl-5-pyrazolonc-diisobutyl kctone at pH 0.8. The uranium content in the apatite was found to be (20.3〜132.9)×10^%.

  14. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

  15. Slurry sampling techniques for the determination of lead in Bangladeshi fish samples by electrothermal atomic absorption spectrometry with a metal tube atomizer.

    Science.gov (United States)

    Rahman, Mohammad Arifur; Kaneco, Satoshi; Suzuki, Tohru; Katsumata, Hideyuki; Ohta, Kiyohisa

    2005-05-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry with a metal tube atomizer has been applied to the determination of lead in Bangladeshi fish samples. The slurry sampling conditions, such as slurry stabilizing agent, slurry concentration, pyrolysis temperature for the slurried fish samples, particle size and ultrasonic agitation time, were optimized for electrothermal atomic absorption spectrometry with the Mo tube atomizer. Thiourea was used as the chemical modifier for the interference of matrix elements. The detection limit was 53 fg (3S/N). The determined amount of lead in Bangladeshi fish samples was consistent with those measured in the dissolved acid-digested samples. The advantages of the proposed methods are easy calibration, simplicity, low cost and rapid analysis.

  16. Determining Component Weights in a Communications Assessment Using Judgmental Policy Capturing

    Directory of Open Access Journals (Sweden)

    Leo M. Harvill, PhD

    2004-01-01

    Full Text Available Abstract Objectives: Tools are needed for determining appropriate weights for complex performance assessment components in medical education. The feasibility of using judgmental policy capturing (JPC, a procedure to statistically describe the information processing strategies of experts, for this purpose was investigated. Methods: Iterative JPC was used to determine appropriate weighting for the six core communication skill scores from a communications objective structured clinical examination (OSCE for medical students using a panel of four communication skill experts. Results: The mean regression weights from the panel indicated they placed less importance on information management (8.5%, moderate and nearly equal importance on rapport building (15.8%, agenda setting (15.4%, and addressing feelings (14.1%, and greater importance on active listening (20.1% and reaching common ground with the patient (25.5%. Discussion: JPC is an effective procedure for determining appropriate weights for complex clinical assessment components. The derived weights may be very different for those assessment components

  17. A study of birth weight of full term neonates and its′ determinants

    Directory of Open Access Journals (Sweden)

    Yugantara R Kadam

    2014-01-01

    Full Text Available Background: Low birth weight (LBW is highly prevalent in India and has a multifactorial causation. There is a need to study and identify the modifiable and non-modifiable risk factors determining birth weight. This will help in planning ante natal care more effectively. Materials and Methods : Study-type-cross-sectional study-setting: Hospital based. Study-subject: Mothers and their new borns. Sample size: All the births taken place during the study period. Study period: July 2010-June 2011. Study tools : (0 i Questionnaire. (ii pediatric weighing machine. Inclusion criteria : m0 others attending ante natal care (ANC clinic from 1 st trimester with minimum three antenatal visits, non-anemic at the end of 2 nd trimester, had full-term and singleton delivery. Exclusion criteria : H/O pregnancy induced hypertension (PIH, diabetes mellieutus (DM, tuberculosis (TB, urinary tract infection (UTI, delivered preterm and tobacco chewers or mishri users. Statistical Analysis : Percentages, mean and SD of birth weight, χ2 test, ANOVA, Z-test, and Binary logistic. Results: By using birth weight as a continuous data it was observed that birth-weight was significantly associated with maternal age (F = 3.360, df = 2, P = 0.035, education (F = 4.401, df = 4, P = 0.002 and breakfast (z = 3.970, P = 0.00. Proportion of LBW was 42.4%. For analysis, groups of newborns on the basis of birth weight showed significant association between LBW and maternal education (χ2 = 12.734, df = 4, P = 0.013, breakfast (χ2 = 13.241, df = 1, P = 0.00 and evening snacks (χ2 = 4.275, df = 1, P = 0.013. According to the binary logistic regression, breakfast and education were significant and best predictors for birth weight. Conclusion: Education and breakfast are strong determinants of birth-weight. Less educated women need more intense health education.

  18. Superior grains determined by grain weight are not fully correlated with the lfowering order in rice

    Institute of Scientific and Technical Information of China (English)

    PENG Ting; ZHAO Quan-zhi; L Qiang; ZHAO Ya-fan; SUN Hong-zheng; HAN Ying-chun; DU Yan-xiu; ZHANG Jing; LI Jun-zhou; WANG Lin-lin

    2015-01-01

    Rice panicles are composed of many branches with two types of extreme grains, the superior and the inferior. Traditional y, it has been wel accepted that earlier lfowers result in superior grains and late lfowers generate inferior grains. However, these correlations have never been strictly examined in practice. In order to determine the accurate relationship between superior and inferior grains and the lfowering order, we localized al the seeds in a panicle in four distinct rice species and systematical y documented the rice lfowering order, lfower locations and the ifnal grain weight for their relationships. Our results demonstrated that the grain weight is more heavily determined by the position of the seeds than by the lfowering order. Despite earlier lfowering has a positive correlation with the grain weight in general, grains from lfowers blooming on the second day after anthesis general y gained the highest weight. This suggests earlier lfowers may not result in superior grains. Therefore, we concluded that superior and inferior grains, commonly determined by grain weight, are not ful y cor-related with the lfowering order in rice. Fol owing the order of the grain weight, the superior grains are general y localized at the middle parts of the primary branches, whereas inferior grains were mainly on the last two secondary branches of the lower half part of the panicle. In addition, the weight of inferior grains were affected by spikelet thinning and spraying with exogenous plant growth regulators, indicating that physiological incompetence might be the major reason for the occurrence of the inferior grains.

  19. Improved statistical determination of absolute neutrino masses via radiative emission of neutrino pairs from atoms

    Science.gov (United States)

    Zhang, Jue; Zhou, Shun

    2016-06-01

    The atomic transition from an excited state |e ⟩ to the ground state |g ⟩ by emitting a neutrino pair and a photon, i.e., |e ⟩→|g ⟩+|γ ⟩+|νi⟩+|ν¯j⟩ with i , j =1 , 2, 3, has been proposed by Yoshimura and his collaborators as an alternative way to determine the absolute scale m0 of neutrino masses. More recently, a statistical analysis of the fine structure of the photon spectrum from this atomic process has been performed [N. Song et al. Phys. Rev. D 93, 013020 (2016)] to quantitatively examine the experimental requirements for a realistic determination of absolute neutrino masses. In this paper, we show how to improve the statistical analysis and demonstrate that the previously required detection time can be reduced by one order of magnitude for the case of a 3 σ determination of m0˜0.01 eV with an accuracy better than 10%. Such an improvement is very encouraging for further investigations on measuring absolute neutrino masses through atomic processes.

  20. Determination of the neutral oxygen atom density in a plasma reactor loaded with metal samples

    Energy Technology Data Exchange (ETDEWEB)

    Mozetic, Miran; Cvelbar, Uros [Jozef Stefan Institute, Jamova cesta 39, 1000 Ljubljana (Slovenia)], E-mail: miran.mozetic@ijs.si

    2009-08-15

    The density of neutral oxygen atoms was determined during processing of metal samples in a plasma reactor. The reactor was a Pyrex tube with an inner diameter of 11 cm and a length of 30 cm. Plasma was created by an inductively coupled radiofrequency generator operating at a frequency of 27.12 MHz and output power up to 500 W. The O density was measured at the edge of the glass tube with a copper fiber optics catalytic probe. The O atom density in the empty tube depended on pressure and was between 4 and 7 x 10{sup 21} m{sup -3}. The maximum O density was at a pressure of about 150 Pa, while the dissociation fraction of O{sub 2} molecules was maximal at the lowest pressure and decreased with increasing pressure. At about 300 Pa it dropped below 10%. The measurements were repeated in the chamber loaded with different metallic samples. In these cases, the density of oxygen atoms was lower than that in the empty chamber. The results were explained by a drain of O atoms caused by heterogeneous recombination on the samples.

  1. WEIGHT LOSS DETERMINATION OF LAMB CARCASSES DURING THE PRECOOLING AND FREEZING PROCESS

    Directory of Open Access Journals (Sweden)

    İbrahim YILMAZ

    1995-01-01

    Full Text Available Total weight loss of Morkaraman breed lamb carcasses were determined during the precooling and also during the freezing process of the carcasses. Research was carried out in the cooling and freezing rooms of Turkish State Slaughter House (EBK of Erzurum. Determined results were compared with the literature values given by different researches. Some suggestions were made to optimize the precooling and frozen process. In each trial, 64 lambs were selected randomly from different herds had been come to slaughter. After slaughter and dressing carcasses were showered with cold water, and removing the kidney and peripheral fats, the carcasses were used in precooling and freezing experiments. Precooling, freezing and all the other treatments were done in the practical handling conditions of EBK, that is none of those conditions were rearranged or altered, and what had been happening in those conditions were aimed to be determined. Experiment was repeated 7 times, thus total of 448 whole carcasses were used in the entire research work. At the end of this study, the average precooling and freezing weight losses were 1.88% and 1.3% respectively and their sum was 3.18%. It was determined that duration of precooling and freezing, average carcass weight, relative humidity, air circulation and loading percentage of the rooms were very effective on the weight losses.

  2. Adhesives, fillers & potting compounds: Special report molecular weight determinations of dimethypolysiloxane polymers

    Energy Technology Data Exchange (ETDEWEB)

    Luthey, Z.A.

    1968-09-03

    Using a Mechrolab Vapor Phase Osmometer and a Hallikainen Automatic Membrane Osmometer the number-average molecular weight of two samples of dimethylpolysiloxane - 2300 and 8000 cstk - as well as samples made by mixing the two previously mentioned materials were determined.

  3. ABOUT THE CALCULATED METHOD OF DETERMINING THE COORDINATES OF THE CENTER OF WEIGHT OF TYPICAL VEHICLES

    Directory of Open Access Journals (Sweden)

    D. Leontiev

    2015-12-01

    Full Text Available Based on the analysis of experimental data there was provided a method for determining loading on the rear wheels when the front wheels are raised. By comparing the results of calculations and experiments, it was revealed that the calculation error does not exceed 5 %. A smaller error for the actual weighted vehicles.

  4. ABOUT THE CALCULATED METHOD OF DETERMINING THE COORDINATES OF THE CENTER OF WEIGHT OF TYPICAL VEHICLES

    OpenAIRE

    D. Leontiev

    2015-01-01

    Based on the analysis of experimental data there was provided a method for determining loading on the rear wheels when the front wheels are raised. By comparing the results of calculations and experiments, it was revealed that the calculation error does not exceed 5 %. A smaller error for the actual weighted vehicles.

  5. Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

    Science.gov (United States)

    Chao, T.T.; Fishman, M. J.; Ball, J.W.

    1969-01-01

    A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

  6. Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

    Maifanite is a nature medicinal stone used in many fields for long time. The research on it showed that there are many trace elements in maifanite. In this paper, 36 trace elements in maifanite were determined by outer cover electrode atomic emission spectrometry, and the determination conditions were studied systematically. The results show that the concentrafions of elements, which are beneficial to human health, are higher, and the elements harmful to people health such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy were also discussed.

  7. Determining the Criteria and Their Weights for Medical Schools' Ranking: A National Consensus.

    Science.gov (United States)

    Mojtahedzadeh, Rita; Mohammadi, Aeen; Kohan, Noushin; Gharib, Mitra; Zolfaghari, Mitra

    2016-06-01

    Delphi as a consensus development technique enables anonymous, systematic refinement of expert opinion with the aim of arriving at a combined or consensual position. In this study, we determined the criteria and their weights for Iranian Medical Schools' ranking through a Delphi process. An expert committee devised 13 proposed criteria with 32 indicators with their weights, which were arranged hierarchically in the form of a tree diagram. We used the Delphi technique to reach a consensus on these criteria and weights among the deans of 38 public Iranian medical schools. For this purpose, we devised and sent a questionnaire to schools and asked them to suggest or correct the criteria and their weights. We repeated this process in two rounds till all the schools reached an acceptable consensus on them. All schools reached a consensus on the set of 13 criteria and 30 indicators and their weights in three main contexts of education, research and facilities, and equipment which were used for Medical Schools' ranking. Using Delphi technique for devising the criteria and their weights in evaluation processes such as ranking makes their results more acceptable among universities.

  8. [Determinants of weight and linear growth deficits in children under two years of age].

    Science.gov (United States)

    Oliveira, Valterlinda Alves de; Assis, Ana Marlúcia Oliveira; Pinheiro, Sandra Maria Conceição; Barreto, Mauricio Lima

    2006-10-01

    To identify determinants of protein-energy malnutrition resulting in weight and linear growth deficits in children. A cross-sectional study was carried out among 1,041 children (under two years of age) from 10 municipalities in Bahia, Northeastern Brazil, during 1999-2000. Both logistic regression and a hierarchical approach were used to identify factors associated with the anthropometric measures. The basic determinant found in the final model for linear growth retardation was having up to two household appliances (OR=2.9; 95% CI: 1.74-4.90); as an underlying determinant, not attending prenatal visits (OR=2.7; 95% CI: 1.47-4.97); and, among immediate determinants were low birth weight (OR=3.6; 95% CI: 1.72-7.70) and reported hospitalization within 12 months before the interview (OR=2.4; 95% CI: 1.42-4.10). Determinants of weight deficit at the basic, underlying and immediate levels were: per capita monthly income of less than one-fourth of the minimum wage (OR=3.4; 95% CI: 1.41-8.16), not attending prenatal visits (OR=2.1; 95% CI: 1.03-4.35) and low birth weight (OR=4.8; 95% CI: 2.00-11.48) respectively. Children's weight and linear deficits were accounted for the overlapping of poor material living conditions, limited access to health care and disease burden. Interventions aimed at improving living conditions and better access to health care programs are strategies towards equity in children's health and nutrition.

  9. Determination of copper, zinc and iron in broncho-alveolar lavages by atomic absorption spectroscopy.

    Science.gov (United States)

    Harlyk, C; Mccourt, J; Bordin, G; Rodriguez, A R; van der Eeckhout, A

    1997-11-01

    Concentrations of Zn, Cu and Fe were measured in 157 broncho-alveolar lavages (BAL), before and after centrifugation, collected at the Leuven University Hospital (Belgium). Zn was measured by flame-atomic absorption spectroscopy, using direct calibration, while Cu and Fe were determined by electrothermal atomic absorption spectroscopy, using the method of standard additions. For Fe only 56 samples were measured. Most of the studied elements are present in the liquid phase (supernatant). About 90% of Cu concentrations lie between 0 and 15 micrograms/kg, while 90% of Zn concentrations are lower than 230 micrograms/kg, with 30% between 30 and 70 micrograms/kg, and 50% between 100 and 200 micrograms/kg. There seems to be a reverse relationship between Cu and Zn levels with high Cu going along with low Zn and vice versa.

  10. What does determine gonad weight in the wild kissing bug Mepraia spinolai

    Directory of Open Access Journals (Sweden)

    Carezza Botto-Mahan

    2007-03-01

    Full Text Available Female fecundity increases with body size in a variety of insects, but it is unknown if this generalization applies for kissing bugs. In this study, we evaluate whether gonad weight in the bloodsucking insect Mepraia spinolai correlates with body size, or determined by nutrition or developmental time. We found that the investment on reproductive tissue correlates positively and significantly with body size and with the amount of ingested blood by female insects along their lifespan. Total molting time did not significantly affect gonad weight. We suggest that under optimal feeding conditions M. spinolai females could express their maximum reproductive potential.

  11. Determinants of Successful Weight Loss After Using a Commercial Web-Based Weight Reduction Program for Six Months: Cohort Study

    Science.gov (United States)

    Postrach, Elisa; Aspalter, Rosa; Elbelt, Ulf; Koller, Michael; Longin, Rita; Schulzke, Jörg-Dieter

    2013-01-01

    Background The Internet is widely available and commonly used for health information; therefore, Web-based weight loss programs could provide support to large parts of the population in self-guided weight loss. Previous studies showed that Web-based weight loss interventions can be effective, depending on the quality of the program. The most effective program tools are visual progress charts or tools for the self-monitoring of weight, diet, and exercises. KiloCoach, a commercial program currently available in German-speaking countries, incorporates these features. A previous investigation showed that the program effectively supports users in losing weight. Objective We investigated weight loss dynamics stratified by weight loss success after 6-month use of KiloCoach. Furthermore, we analyzed possible associations between intensity of program use and weight loss. The results are intended for tailoring user recommendations for weight-loss Internet platforms. Methods Datasets of KiloCoach users (January 1, 2008 to December 31, 2011) who actively used the platform for 6 months or more were assigned to this retrospective analysis. Users (N=479) were 42.2% men, mean age of 44.0 years (SD 11.7), with a mean body mass index (BMI) of 31.7 kg/m2 (SD 3.2). Based on the weight loss achieved after 6 months, 3 success groups were generated. The unsuccessful group lost weight. At baseline, the unsuccessful (n=261, 54.5%), moderate success (n=133, 27.8%), and high success (n=85, 17.8%) groups were similar in age, weight, BMI, and gender distribution. Results After 6 months, the unsuccessful group lost 1.2% (SD 2.4), the moderate success group lost 7.4% (SD 1.5), and the high success group lost 14.2% (SD 3.8) of their initial weight (Pweight loss (weeks 3-4), the total number of dietary protocols, and the total number of weight entries were independent predictors for 6-month weight reduction (all Pweight reduction. Sensitivity analysis by baseline carried forward method confirmed

  12. Effect of Calcination Temperatures on Ratio of Atomic Weight of Al/O in Sol-Gel Method for Synthesis γ Al2O3 as a Buffer Catalyst

    Science.gov (United States)

    Suastiyanti, Dwita; Handayani, Sri; Manawan, Maykel T. E.

    2017-07-01

    The aim of this research was to determine the effect of calcination temperatures on the ratio of atomic weight of Al/O that could affect the formation of γ-Al2O3 phase. The novelty of this research is how to produce γ-Al2O3 in single phase and nanosize by simple method (sol-gel method).The calcination process was performed at a temperature which varied of 190°C, 275°C and 320°C for 4 hours respectively and sinter process carried out at a temperature of 420°C for 6 hours. Calcination process at temperature of 320°C for 4 hours produces powder with the ratio of atomic weight of Al/O in accordance with the ratio of atomic weight of Al/O in Al2O3 compound, 0.6667 (2/3). This ratio is as expected for a compound according to formula of Al2O3. This condition also produces alumina powder with the smallest particle size on the nanometer scale of 84.5 nm. SEM test results show that the grain is still heterogenous in size and shape. The results also show that the grain is still agglomerated.

  13. ISS Node 1 is readied for weight and center of gravity determination

    Science.gov (United States)

    1998-01-01

    Node 1, the first U.S. element for the International Space Station, and Pressurized Mating Adapter-1 (PMA-1) continue with prelaunch preparation activities at KSC's Space Station Processing Facility. The node and PMA-1 are seen here on a workstand getting ready to be moved the next day to a weight and balance stand for an interim weight and center of gravity determination. (The final determination is planned to be performed prior to transporting Node 1 to the launch pad.) Upon completing the interim determination, the node and PMA will be hoisted into the Shuttle payload transportation canister and the doors will be closed for a two-week leak check. Node 1 is a connecting passageway to the living and working areas of the space station. Node 1 is scheduled to fly on STS-88.

  14. New approach to determine common weights in DEA efficiency evaluation model

    Institute of Scientific and Technical Information of China (English)

    Feng Yang; Chenchen Yang; Liang Liang; Shaofu Du

    2010-01-01

    Data envelopment analysis(DEA)is a mathematical programming approach to appraise the relative efficiencies of peer decision-making unit(DMU),which is widely used in ranking DMUs.However,almost all DEA-related ranking approaches are based on the self-evaluation efficiencies.In other words,each DMU chooses the weights it prefers to most,so the resulted efficiencies are not suitable to be used as ranking criteria.Therefore this paper proposes a new approach to determine a bundle of common weights in DEA efficiency evaluation model by introducing a multi-objective integer programming.The paper also gives the solving process of this multi-objective integer programming,and the solution is proven a Paroto efficient solution.The solving process ensures that the obtained common weight bundle is acceptable by a groat number of DMUs.Finally a numeral example is given to demonstrate the approach.

  15. QSPR Calculation of Normal Boiling Points of Organic Molecules Based on the Use of Correlation Weighting of Atomic Orbitals with Extended Connectivity of Zero- and First-Order Graphs of Atomic Orbitals

    Directory of Open Access Journals (Sweden)

    Eduardo A. Castro

    2004-12-01

    Full Text Available We report the results of a calculation of the normal boiling points of a representative set of 200 organic molecules through the application of QSPR theory. For this purpose we have used a particular set of flexible molecular descriptors, the so called Correlation Weighting of Atomic Orbitals with Extended Connectivity of Zero- and First-Order Graphs of Atomic Orbitals. Although in general the results show suitable behavior to predict this physical chemistry property, the existence of some deviant behaviors points to a need to complement this index with some other sort of molecular descriptors. Some possible extensions of this study are discussed.

  16. A Experimental Determination of the Resonant Frequency of Atoms Moving in a Medium

    Science.gov (United States)

    Beary, Daniel Andrew

    The theory of the Doppler-Recoil effect is described. In contrast to previous theories, the theory proposed by Haugan and Kowalski suggests that the frequency of the electromagnetic wave that excites a transition in an atom is a function of the velocity of that atom and the index of refraction of the medium. Following the path of Haugan and Kowalski, the Doppler Recoil equation is derived under the conditions of a rarefied gas acting as a continuous medium. Next, the theory of saturation spectroscopy is revised. This method of spectroscopy uses a pump and probe beam traveling collinearly in opposite directions. Beams of equal frequency in the lab frame interact with the zero axial velocity population within the gas when the beams are on resonance. For pump and probe beams of different frequencies, the atoms that they interact with will have an axial velocity component such that the Doppler shift leads to resonance with both beams. The purpose of this work is to verify the Doppler -Recoil formula proposed by Haugan and Kowalski. In the experiment performed, the resonant frequency of the stationary and moving velocity groups is determined using saturation spectroscopy. The theory predicts an average frequency shift of 307 Hz/^circC. The data show a shift of 94 kHz/^circ C. Because of the unexpected result, possible sources of errors such as pressure broadening, power broadening, and potential for systematic errors were examined. No explanation was found for these shifts.

  17. Radiation trapping in atomic absorption spectroscopy at lead determination in different matricies

    Energy Technology Data Exchange (ETDEWEB)

    El-Gohary, Z. [Department of Physics, Faculty of Science, Menoufia University, Shebin El-Koom (Egypt)]. E-mail: zhelgohary@yahoo.com

    2005-08-15

    The determination of lead by flame atomic absorption analysis in the presence of Sn and Fe atoms and different matrices such as OH and SO{sub 3} was investigated with the objective of understanding the spectral interference processes at the analytical lines 283.31 nm for a wide range of concentration. The radiation trapping factor was interpreted and evaluated assuming Voigt distribution of the atomic and rotational lines in the flame. The radiation trapping factor was increased by increasing the number density (plasma of the absorbing medium is optically thick). In plasma, there is a certain point of equilibrium between the trapping and the escaping of radiation, which is relevant to 50% of absorption. The spectral background interference can cause a variation of the number density at equilibrium point as a result of the degree of overlap with the analytical line. The spectral background interference can be easily avoided by using another resonance absorption line for the analysis. The chemical modification of the matrix is applied to minimize the interference effect. Nitric acid, ammonium nitrate and magnesium nitrate are most commonly recommended as matrix modifiers.

  18. Radiation trapping in atomic absorption spectroscopy at lead determination in different matricies

    Science.gov (United States)

    El-Gohary, Z.

    2005-08-01

    The determination of lead by flame atomic absorption analysis in the presence of Sn and Fe atoms and different matrices such as OH and SO3 was investigated with the objective of understanding the spectral interference processes at the analytical lines 283.31 nm for a wide range of concentration. The radiation trapping factor was interpreted and evaluated assuming Voigt distribution of the atomic and rotational lines in the flame. The radiation trapping factor was increased by increasing the number density (plasma of the absorbing medium is optically thick). In plasma, there is a certain point of equilibrium between the trapping and the escaping of radiation, which is relevant to 50% of absorption. The spectral background interference can cause a variation of the number density at equilibrium point as a result of the degree of overlap with the analytical line. The spectral background interference can be easily avoided by using another resonance absorption line for the analysis. The chemical modification of the matrix is applied to minimize the interference effect. Nitric acid, ammonium nitrate and magnesium nitrate are most commonly recommended as matrix modifiers.

  19. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    Science.gov (United States)

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-06

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values.

  20. Influence and determinative factors of ion-to-atom arrival ratio in unbalanced magnetron sputtering systems

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Low pressure sputtering with a controlled ratio of ion flux to deposited atom flux at the condensing surface is one of the main directions of development of magnetron sputtering methods.Unbalanced magnetron sputtering,by producing dense secondary plasma around the substrate,provides a high ion current density.The closed-field unbalanced magnetron sputtering system (CFUBMS) has been established as a versatile technique for high-rate deposition high-quality metal,alloy,and ceramic thin films.The key factor in the CFUBMS system is the ability to transport high ion currents to the substrate,which can enhance the formation of full dense coatings at relatively low value homologous temperature.The investigation shows that the energy of ions incidenced at the substrate and the ratio of the flux of these ions to the flux of condensing atoms are the fundamental parameters in determining the structure and properties of films produced by ion-assisted deposition processes.Increasing ion bombardment during deposition combined with increasing mobility of the condensing atoms favors the formation of a dense microstructure and a smooth surface.

  1. Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

    Science.gov (United States)

    Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

    2004-01-01

    An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

  2. Molecular weight and helix conformation determine intestinal anti-inflammatory effects of exopolysaccharide from Schizophyllum commune.

    Science.gov (United States)

    Du, Bin; Yang, Yuedong; Bian, Zhaoxiang; Xu, Baojun

    2017-09-15

    Intestinal anti-inflammatory activities of exopolysaccharide from S. commune were assessed using dextran sulfate sodium (DSS)-induced colitis in mice model. The changes of molecular weight (MW), atomic force microscope morphology, X-ray diffraction, particle size distribution, and viscosity were recorded after sonication treatment. The results indicated that the triple helical structure of exopolysaccharide was dissociated into single helical structure and random coiled structure by ultrasonication via breaking of inter- and intramolecular hydrogen bonds. The medium (936kDa) and high MW (1437kDa) exopolysaccharide had the mixture of triple helix and single helix conformation, while the low MW (197kDa) exopolysaccharide exhibit random coiled conformation. The intestinal anti-inflammatory activity study showed that oral administration of medium and high MW (1437kDa) exopolysaccharide significantly recovered DSS-induced colitis in inflamed tissues and reduced inflammation induced infiltration of macrophages. These results showed that medium (936kDa) and high MW (1437kDa) exopolysaccharide had intestinal anti-inflammatory activity. The intestinal anti-inflammatory activity of exopolysaccharide was related to helical structure and molecular weight. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. DETERMINATION OF NICKLE CONTENTS IN SELECTED VANASPATI GHEE THROUGH ATOMIC ABSORPTION SPECTROPHOTOMETER

    Directory of Open Access Journals (Sweden)

    Waqas Ahmad

    2014-12-01

    Full Text Available To convert vegetable edible oils into vanaspati ghee, nickel is used as a catalyst in the hydrogenation process. A simple and fast method for the trace level determination of nickel in ghee is reported. In this different methods were applied for the extraction of residual nickel from ghee samples. Using toluene, as organic solvents, an acid mixture was used for the extraction of nickel. Extracted nickel was quantified with atomic absorption. Among the organic solvents, toluene proved to be the best solvent mediating a 95% extraction of nickel from ghee samples. Nickel was extracted and determined in ten different brands of ghee and in all samples its amount was well above the permissible limit of WHO (0.2 μg/g. Other metals like lead, zinc, copper, and cadmium were also determined and their concentrations were found to be much below the WHO permissible limits.

  4. Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol*L-1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0-12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg*L-1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

  5. Preconcentration and Determination of Chromium Species Using Octadecyl Silica Membrane Disks and Flame Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    MOGHIMI Ali; SABER-TEHRANI Mohammad; WAQIF-HUSAIN Syed; MOHAMMADHOSSEINI Majid

    2007-01-01

    A novel and selective method for the fast determination of trace amounts of chromium species in water samples has been developed.The procedure is based on the selective formation of chromium diethyldithiocarbamate complexes at different pH in the presence of Mn(Ⅱ) as an enhancement agent of chromium signals followed by elutionwith organic eluents and determination by atomic flame absorption spectrometry.The maximum capacity of the employed disks was found to be (3964±3) μg and (376±2) μg for Cr(Ⅲ) and Cr(Ⅵ),respectively.The detection limit of the proposed method is 49 and 43 ng·L-1 for Cr(Ⅲ) and Cr(Ⅵ),respectively.The proposed method was successfully applied for determination of chromium species Cr(Ⅲ) and Cr(Ⅵ) in different water samples.

  6. Application of atomic force microscopy on rapid determination of microorganisms for food safety.

    Science.gov (United States)

    Yang, H; Wang, Y

    2008-10-01

    Rapid detection and quantification of microorganisms is important for food quality, safety, and security. In this field, nanotechnology appears to be promising in its ability to characterize an individual microorganism and detect heterogeneous distribution of microbes in food samples. In this study, atomic force microscopy (AFM), a nanotechnology tool, was used to investigate Escherichia coli (E. coli) qualitatively and quantitatively. E. coli strains B and K12 were used as surrogates to represent pathogenic strains, such as E. coli O157: H7. The results from AFM were compared with those from scanning/transmission electron microscopy (SEM/TEM). The qualitative determination was obtained using morphology and characteristic parameters from AFM images, and the quantitative determination was obtained by calculating the microorganisms in AFM images. The results show that AFM provides a new approach for rapid determination of microorganisms for food safety.

  7. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of some fluoroquinolone antibacterials using ammonium reineckate

    Science.gov (United States)

    Al-Ghannam, Sheikha M.

    2008-04-01

    Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 μg mL -1 and 0.10-1.5 mg mL -1 using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 μg mL -1 using AAS method or 30-45 μg mL -1 using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.

  8. Determination of lead in fine particulates by slurry sampling electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Yu, J C; Ho, K F; Lee, S C

    2001-01-02

    A simple method for determining lead in fine particulates (PM2.5) by using electrothermal atomic absorption spectrometry (ETAAS) has been developed. Particulates collected on Nuclepore filter by using a dichotomous sampler were suspended in diluted nitric acid after ultrasonic agitation. The dislodging efficiency is nearly 100% after agitation for 5 min. In order to study the suspension behavior of PM2.5 in solvents, a Brookhaven ZetaPlus Particle Size Analyzer was used to determine the particle size distribution and suspension behavior of air particulates in the solvent. The pre-digestion and modification effect of nitric acid would be discussed. Palladium was added as a chemical modifier and the temperature program of ETAAS was changed in order to improve the recovery. The slurry was introduced directly into a graphite tube for atomization. The metal content in the sample was determined by the standard addition method. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling method. It offers a quick and efficient alternative method for heavy metal characterization in fine particulates.

  9. [Determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry].

    Science.gov (United States)

    Liu, Dong-yan; Zhang, Yuan-li

    2002-02-01

    A direct method was reported for the determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution conditions of coal samples as well as interference conditions of hydrochloric acid and matrix were studied. The recommended method not only proved to be simple and rapid than traditional gravimetric method but show satisfying precision and accuracy as well. The results of samples are as same as gravimetry. The recoveries are more than 96%, and the relative standard deviation of six samples are less than 3%.

  10. Local determination of the amount of integration of an atom into a crystal surface

    Science.gov (United States)

    Volgmann, K.; Gawronski, H.; Zaum, Ch; Rusina, G. G.; Borisova, S. D.; Chulkov, E. V.; Morgenstern, K.

    2014-10-01

    Collective vibrational modes of crystal lattices, called phonons, determine fundamental material properties, such as their thermal and electrical conductivities. Bulk phonon spectra are influenced by point defects. More recently, the importance of phonons on nanostructures has come into the focus of attention. Here we show a spatially resolved phonon spectra of point defects that reveal distinctly different signatures for a cavity alone and an impurity atom fully integrated into the surface as opposed to one placed into a cavity. The spectra are indicative for delocalized phonons and localized vibrations, respectively, as confirmed by theory.

  11. Iodine Determination by Microwave Plasma Torch Atomic Emission Spectrometer Coupled with Online Preconcentration Vapor Generation Technique

    Institute of Scientific and Technical Information of China (English)

    FEI Yan-qun; LUO Gui-min; FENG Guo-dong; CHEN Huan-wen; FEI Qiang; HUAN Yan-fu; JIN Qin-han

    2008-01-01

    This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry (MPT-AES) coupled with online preconcentration vapor generation method.A new desolvation device,multistrand Nation dryer,was used as the substitute for condenser desolvation system.Some experimental conditions,such as preconcentration time,acidity of sample solution,rinsing solution acidity and dynamic linear range were investigated and optimized.The new desolvation system eliminates the problem of decreasing emission intensity of I(I) 206.238 nm line with the increase of working time on a conventional condenser desolvation system,thus greatly improving the reproducibility.

  12. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed....../preconcentration procedures have been suggested and applied, such as liquid-liquid extraction, (co)precipitation with collection in knotted reactors, adsorption, hydride generation, or ion-exchange. Selected examples of some of these procedures will be discussed. Emphasis will be placed on the use of FI...

  13. Diet quality, social determinants, and weight status in Puerto Rican children aged 12 years.

    Science.gov (United States)

    Torres, Roxana; Santos, Elvia; Orraca, Luis; Elias, Augusto; Palacios, Cristina

    2014-08-01

    Diet quality may be influenced by social determinants and weight status. This has not been studied in Puerto Rico; therefore, our cross-sectional study examined whether diet quality, assessed by the Healthy Eating Index-2005 (HEI-2005), differs by social determinants (sex, school type, and region) and weight status in children in Puerto Rico. As part of an island-wide study to evaluate oral health in 1,550 children aged 12 years, dietary intake was assessed in a representative subset (n=796) using a 24-hour diet recall. Diet quality was evaluated from the diet recall results using the HEI-2005. Overall mean HEI-2005 score was 40.9, out of a total maximum score of 100. Girls had significantly higher scores for whole fruit, total vegetables, whole grains, and sodium but lower scores for total grains and milk compared with boys (Pdiet quality were associated with the social determinants studied and with weight status in our sample. Overall diet quality needs improvement in Puerto Rican children so that it is better aligned with dietary recommendations.

  14. Absolute number densities of helium metastable atoms determined by atomic absorption spectroscopy in helium plasma-based discharges used as ambient desorption/ionization sources for mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reininger, Charlotte; Woodfield, Kellie [Brigham Young University, Department of Chemistry and Biochemistry, Provo, UT 84602 (United States); Keelor, Joel D.; Kaylor, Adam; Fernández, Facundo M. [Georgia Institute of Technology, School of Chemistry and Biochemistry, Atlanta, GA 30332 (United States); Farnsworth, Paul B., E-mail: paul_farnsworth@byu.edu [Brigham Young University, Department of Chemistry and Biochemistry, Provo, UT 84602 (United States)

    2014-10-01

    The absolute number densities of helium atoms in the 2s {sup 3}S{sub 1} metastable state were determined in four plasma-based ambient desorption/ionization sources by atomic absorption spectroscopy. The plasmas included a high-frequency dielectric barrier discharge (HF-DBD), a low temperature plasma (LTP), and two atmospheric-pressure glow discharges, one with AC excitation and the other with DC excitation. Peak densities in the luminous plumes downstream from the discharge capillaries of the HF-DBD and the LTP were 1.39 × 10{sup 12} cm{sup −3} and 0.011 × 10{sup 12} cm{sup −3}, respectively. Neither glow discharge produced a visible afterglow, and no metastable atoms were detected downstream from the capillary exits. However, densities of 0.58 × 10{sup 12} cm{sup −3} and 0.97 × 10{sup 12} cm{sup −3} were measured in the interelectrode regions of the AC and DC glow discharges, respectively. Time-resolved measurements of metastable atom densities revealed significant random variations in the timing of pulsed absorption signals with respect to the voltage waveforms applied to the discharges. - Highlights: • We determine He metastable number densities for four plasma types • The highest number densities were observed in a dielectric barrier discharge • No helium metastable atoms were observed downstream from the exits of glow discharges.

  15. Heterogeneity of income and lifestyle determinants of body weight among adult women in Mexico, 2006.

    Science.gov (United States)

    Colchero, M A; Sosa-Rubí, S G

    2012-07-01

    In Mexico, the combined prevalence of overweight and obesity among Mexican women increased from 64% in 2000 to 72% in 2006. In this paper, we report our findings on the relation of women's body mass index (BMI) with income and lifestyles choices using data from a cross-sectional survey conducted in 2006. The two following approaches were executed. First, we estimated a two-stage least-squares regression to control for the potential endogeneity of income stratified by urban or rural residency. The second approach was aimed at exploring whether the determinants of weight varied among different weight levels using latent class models. Our findings from the two-stage least-squares regression show a positive non-significant association between income and BMI in the overall and urban samples but a significant positive relationship among rural women. Our results suggest that one unit increase in income is associated with 4.1% increase in body weight in rural areas. Estimates from the latent class model (LCM) show a positive but marginally significant association between income and BMI in the overall sample only in the class where there is a greater likelihood that women have normal weight or overweight compared to the class with a higher probability of being obese, but we also found a large association in rural areas for both classes. Lifestyle choices were associated with BMI. Results from the two-stage least-squares regressions reveal that more hours sitting per day and a higher percentage of expenditures in sugary beverages were associated with higher BMI levels. In the LCM, for women who eventually belong to the higher body weight class, lifestyles seem to matter more. Findings from this research suggest that policies to tackle the obesity epidemic among adult women should be different for women living in urban and rural areas and women with different weight levels.

  16. Node 1 and PMA-1 are moved for weight and center of gravity determination

    Science.gov (United States)

    1998-01-01

    Node 1, the first U.S. element for the International Space Station, and Pressurized Mating Adapter-1 (PMA-1) continue with prelaunch preparation activities at KSC's Space Station Processing Facility. Node 1 is a connecting passageway to the living and working areas of the space station. The node and PMA-1 are being moved to an element rotation stand, or test stand, where they will undergo an interim weight and center of gravity determination. The final determination is planned to be performed prior to transporting Node 1 to the launch pad. Node 1 is scheduled to fly on STS-88.

  17. Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

    Science.gov (United States)

    This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

  18. Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pasias, I.N.; Pappa, Ch.; Katsarou, V.; Thomaidis, N.S., E-mail: ntho@chem.uoa.gr; Piperaki, E.A.

    2014-02-01

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D{sub 2} background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during

  19. Slurry analysis after lead collection on a sorbent and its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baysal, Asli; Tokman, Nilgun [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey); Akman, Suleyman [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak-Istanbul (Turkey)], E-mail: akmans@itu.edu.tr; Ozeroglu, Cemal [Istanbul University, Department of Chemistry, Faculty of Engineering, 34320 Avcilar-Istanbul (Turkey)

    2008-02-11

    In this study, in order to eliminate the drawbacks of elution step and to reach higher enrichment factors, a novel preconcentration/separation technique for the slurry analysis of sorbent loaded with lead prior to its determination by electrothermal atomic absorption spectrometry was described. For this purpose, at first, lead was collected on ethylene glycol dimethacrylate methacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrolidine dithiocarbamate (APDC) by conventional batch technique. After separation of liquid phase, slurry of the sorbent was prepared and directly pipetted into graphite furnace of atomic absorption spectrophotometer. Optimum conditions for quantitative sorption and preparation of the slurry were investigated. A 100-fold enrichment factor could be easily reached. The analyte element in certified sea-water and Bovine-liver samples was determined in the range of 95% confidence level. The proposed technique was fast and simple and the risks of contamination and analyte loss were low. Detection limit (3{delta}) for Pb was 1.67 {mu}g l{sup -1}.

  20. [Studies on cold resistance of hazel determined and analyzed by atomic absorption spectrometry].

    Science.gov (United States)

    Li, Xiu-Xia; Liu, Cheng-Cai; Zhang, Wei-Dong; Shao, Hong; Wu, Heng-Mei; Wang, Zhong; Yang, Yong-Nian; Li, Ji-Lin

    2010-06-01

    Using annual branch of hazel as the experimental materials, the K(+)-leakage and relative electric conductivity of three hazel species (six hazel clones) which had been treated with different low temperature were determined by electro-conductivity gauge and atomic absorption spectrometry. Regression models were established for low temperature to the K(+)-leakage or the relative electric conductivity of six hazel clones. The results showed that there was the same result of cold resistance for all clones using the two methods of comprehensive evaluation, and the indicator of K(+)-leakage rate determined by atomic absorption spectrometry can be used as a means of early identification of cold resistance of hazel clones. There were obvious differences among the clones in the ability of cold resistance. The order of the ability of cold resistance for the six hazel clones was C7R7 > Z-9-40 > C6R1 > CS2R1 > Z-9-22 > Z-9-30, and the order of the ability of cold resistance for the three hazel species was C. heterophylla > C. heterophyllax X (C. heterophylla X C. avellana) > C. heterophylla X C. avellana. The median lethal temperature of tissue for all clones is -26(-)-40 degrees "C.

  1. Determinants of rapid weight gain during infancy: baseline results from the NOURISH randomised controlled trial

    Directory of Open Access Journals (Sweden)

    Mihrshahi Seema

    2011-11-01

    Full Text Available Abstract Background Rapid weight gain in infancy is an important predictor of obesity in later childhood. Our aim was to determine which modifiable variables are associated with rapid weight gain in early life. Methods Subjects were healthy infants enrolled in NOURISH, a randomised, controlled trial evaluating an intervention to promote positive early feeding practices. This analysis used the birth and baseline data for NOURISH. Birthweight was collected from hospital records and infants were also weighed at baseline assessment when they were aged 4-7 months and before randomisation. Infant feeding practices and demographic variables were collected from the mother using a self administered questionnaire. Rapid weight gain was defined as an increase in weight-for-age Z-score (using WHO standards above 0.67 SD from birth to baseline assessment, which is interpreted clinically as crossing centile lines on a growth chart. Variables associated with rapid weight gain were evaluated using a multivariable logistic regression model. Results Complete data were available for 612 infants (88% of the total sample recruited with a mean (SD age of 4.3 (1.0 months at baseline assessment. After adjusting for mother's age, smoking in pregnancy, BMI, and education and infant birthweight, age, gender and introduction of solid foods, the only two modifiable factors associated with rapid weight gain to attain statistical significance were formula feeding [OR = 1.72 (95%CI 1.01-2.94, P = 0.047] and feeding on schedule [OR = 2.29 (95%CI 1.14-4.61, P = 0.020]. Male gender and lower birthweight were non-modifiable factors associated with rapid weight gain. Conclusions This analysis supports the contention that there is an association between formula feeding, feeding to schedule and weight gain in the first months of life. Mechanisms may include the actual content of formula milk (e.g. higher protein intake or differences in feeding styles, such as feeding to schedule

  2. Determination of sodium in foods by flame atomic absorption spectrometry after microwave digestion: NMKL interlaboratory study.

    Science.gov (United States)

    Julshamn, Kaare; Lea, Per; Norli, Hilde Skaar

    2005-01-01

    Nine laboratories participated in an interlaboratory method performance (collaborative) study of a method for the determination of sodium in foods by flame atomic absorption spectrometry after wet digestion, using a microwave oven technique. Before the study, the laboratories were able to practice on samples with defined sodium levels (pretrial test). The method was tested on a total of 6 foods (broccoli, carrot, bread, saithe fillet, pork, and cheese) with sodium concentrations of 1480-8260 mg/kg. The materials were presented to the participants in the study as blind duplicates, and the participants were asked to perform single determinations for each sample. The repeatability relative standard deviations (RSDr) for sodium ranged from 1.9 to 6.5%. The reproducibility relative standard deviations (RSDR) ranged from 4.2 to 6.9%. The HorRat values ranged from 0.9 to 1.6.

  3. [Determination of trace elements in Aloe barbadensis Miller irrigated with seawater by atomic absorption spectrophotometry].

    Science.gov (United States)

    Liu, Chun-Hui; Wang, Chang-Hai; Liu, Zhao-Pu

    2008-03-01

    The dry leaves of Aloe barbadensis Miller irrigated with seawater were dissolved in nitric acid and then oxygenated by perchloric acid. Nine kinds of trace elements in the samples were determined by atomic absorption spectrophotometry, including calcium, potassium, magnesium, sodium, manganese, zinc, iron, copper and lead, with added lanthanum chloride as releaser to eliminate the interference of co-existent ions. The recoveries were 96.58%-104.31%, and the relative standard deviations of sample determination (10 times) were less than 2%. This method is simple, sensitive and rapid with satisfactory results and good reproducibility. The results indicated that there were rich Ca, Mg, K and Na, and moderate Mn, Zn and Fe elements in the Aloe barbadensis Miller irrigated with seawater. However, the concentrations of Cu and Pb were low. Therefore, Aloe barbadensis Miller irrigated with seawater has officinal and economic values. These results provide data for further research on Aloe barbadensis Miller irrigated with seawater.

  4. Bloch oscillations of ultracold atoms: a tool for a metrological determination of h/m Rb.

    Science.gov (United States)

    Battesti, Rémy; Cladé, Pierre; Guellati-Khélifa, Saïda; Schwob, Catherine; Grémaud, Benoît; Nez, François; Julien, Lucile; Biraben, François

    2004-06-25

    We use Bloch oscillations in a horizontal moving standing wave to transfer a large number of photon recoils to atoms with a high efficiency (99.5% per cycle). By measuring the photon recoil of 87Rb, using velocity-selective Raman transitions to select a subrecoil velocity class and to measure the final accelerated velocity class, we have determined h/m(Rb) with a relative precision of 0.4 ppm. To exploit the high momentum transfer efficiency of our method, we are developing a vertical standing wave setup. This will allow us to measure h/m(Rb) better than 10(-8) and hence the fine structure constant alpha with an uncertainty close to the most accurate value coming from the (g-2) determination.

  5. Determination of cyanide by a flow injection analysis-atomic absorption spectrometric method.

    Science.gov (United States)

    López Gómez, A V; Martínez Calatayud, J

    1998-10-01

    A new flow injection analysis (FIA) procedure is proposed for the indirect atomic absorption spectrometric determination of cyanide. The FIA manifold is based on the insertion of the sample into a distilled water carrier, then the sample flows through a solid-phase reactor filled with silver iodide entrapped in polymeric resin beads. The calibration graph is linear over the range 0.2-6.0 mg l-1 of cyanide (correlation coefficient 0.9974), the detection limit is 0.1 mg l-1, the sample throughput is 193 h-1 and the RSD is 0.8%. The method is simple, quick and more selective than other published FIA procedures. The reproducibility obtained by using different solid-phase reactors and solutions is in the range 2.2-3.1% (RSD). The method was applied to the determination of cyanide in commercial samples such as pharmaceutical formulations and industrial electrolytic baths.

  6. Determination of thallium in wine by electrothermal atomic absorption spectrometry after extraction preconcentration

    Science.gov (United States)

    Cvetković, Julijana; Arpadjan, Sonja; Karadjova, Irina; Stafilov, Trajče

    2002-06-01

    A simple method for extraction electrothermal atomic absorption spectroscopy (ETAAS) determination of Tl in wine is described. The wine sample is decomposed with a mixture of nitric acid and hydrogen peroxide and both thallium species Tl(I) and Tl(III) are extracted from 0.5 mol l -1 KI solution into iso-butyl methyl ketone (IBMK). Optimal parameters for ETAAS measurement of the iodide complexes extracted were defined for two different instruments: Perkin Elmer Zeeman 3030 (HGA 600) and Varian SpectrAA-880 (GTA-100). Modifiers of tartaric acid, Pd [ammoniumtetrachloropaladate (II)] or Ag (silver nitrate) were investigated for thermal stabilization of such extremely volatile species as iodide complexes of Tl. The analytical procedure developed permits 50-fold preconcentration and determination of 0.05 μg l -1 Tl in wine. The relative standard deviation ranges from 6 to 12% for the concentration range 0.2-1 μg l -1 Tl in wine.

  7. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization.

    Science.gov (United States)

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS.

  8. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  9. About One Approach to Determine the Weights of the State Space Method

    Directory of Open Access Journals (Sweden)

    I. K. Romanova

    2015-01-01

    Full Text Available The article studies methods of determining weight coefficients, also called coefficients of criteria importance in multiobjective optimization (MOO. It is assumed that these coefficients indicate a degree of individual criteria influence on the final selection (final or summary assessment: the more is coefficient, the greater is contribution of its corresponding criterion.Today in the framework of modern information systems to support decision making for various purposes a number of methods for determining relative importance of criteria has been developed. Among those methods we can distinguish a utility method, method of weighted power average; weighted median; method of matching clustered rankings, method of paired comparison of importance, etc.However, it should be noted that different techniques available for calculating weights does not eliminate the main problem of multicriteria optimization namely, the inconsistency of individual criteria. The basis for solving multicriteria problems is a fundamental principle of multi-criteria selection i.e. Edgeworth - Pareto principle.Despite a large number of methods to determine the weights, the task remains relevant not only for reasons of evaluations subjectivity, but also because of the mathematical aspects. Today, recognized is the fact that, for example, such a popular method as linear convolution of private criteria, essentially, represents one of the heuristic approaches and, applying it, you can have got not the best final choice. Carlin lemma reflects the limits of the method application.The aim of this work is to offer one of the methods to calculate the weights applied to the problem of dynamic system optimization, the quality of which is determined by the criterion of a special type, namely integral quadratic quality criterion. The main challenge relates to the method of state space, which in the literature also is called the method of analytical design of optimal controllers.Despite the

  10. 40 CFR Appendix A to Subpart Pppp... - Determination of Weight Volatile Matter Content and Weight Solids Content of Reactive Adhesives

    Science.gov (United States)

    2010-07-01

    ... as specified in ASTM E145-94 (Reapproved 2001), “Standard Specification for Gravity-Convection and... weight loss during baking may be calculated separately. These values may be useful for identifying sources of variation in the results obtained for different specimens of the same material. 2—For both...

  11. Socioeconomic and nutritional determinants of low birth weight babies: A hospital based study

    Directory of Open Access Journals (Sweden)

    Smiti Narain

    2014-12-01

    Full Text Available According to the World Health Organization (WHO definition, infants with birth weights of less than 2,500 grams are classified as low birth weight (LBW. LBW is a sensitive indicator for predicting the chances of both infant survival and healthy childhood growth and development, and it also reflects the present and past health status of the mother. LBW constitutes an important factor affecting neonatal mortality and morbidity.Objective: To find the incidence of low birth weight babies and its determinants Materials and methods: Present study was a cross sectional type. All mothers delivering live born singleton neonate in study place (Postnatal ward of Rohilkhand Medical College and hospital were interviewed with pretested, predesigned schedule. Statistical analysis was done using SPSS version 21software and chi square test, OR etc.Results: Overall incidence of LBW was 20% and mean birth weight was 2776.85 + 383.6 gm LBW was found to be more common in the rural population and poor educational status. A higher incidence of LBW was seen in mothers with inadequate diet and those who were anaemic. Conclusion: Low birth weight still poses a fair problem in our perspective, and when we cannot control ethnic factors like height, or do a drastic socio-economic upliftment, some basic factors, like good ANC care, correcting anemia, and above all motivating the mother to follow some habits in the ANC period like adequate consumption of food and adequate rest, institutional deliveries shall take a long way forward in addressing the problem.

  12. A rough set approach for determining weights of decision makers in group decision making

    Science.gov (United States)

    Yang, Qiang; Du, Ping-an; Wang, Yong; Liang, Bin

    2017-01-01

    This study aims to present a novel approach for determining the weights of decision makers (DMs) based on rough group decision in multiple attribute group decision-making (MAGDM) problems. First, we construct a rough group decision matrix from all DMs’ decision matrixes on the basis of rough set theory. After that, we derive a positive ideal solution (PIS) founded on the average matrix of rough group decision, and negative ideal solutions (NISs) founded on the lower and upper limit matrixes of rough group decision. Then, we obtain the weight of each group member and priority order of alternatives by using relative closeness method, which depends on the distances from each individual group member’ decision to the PIS and NISs. Through comparisons with existing methods and an on-line business manager selection example, the proposed method show that it can provide more insights into the subjectivity and vagueness of DMs’ evaluations and selections. PMID:28234974

  13. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Docekal, Bohumil [Institute of Analytical Chemistry, Academy of Sciences of the Czech Republic, Veveri 97, CZ-61142, Brno (Czech Republic)], E-mail: docekal@iach.cz; Vojtkova, Blanka [Institute of Materials Science, Faculty of Chemistry, Brno University of Technology, Purkynova 118, CZ-61200 Brno (Czech Republic)

    2007-03-15

    A true direct solid sampling electrothermal atomic absorption spectrometry method with Zeeman-effect background correction (Analytik Jena ZEEnit 60 AAS) was developed for the determination of As, Cd, Hg, Pb, Sb and Zn in powdered titanium dioxide of pharmaceutical, food and cosmetics grade. The interaction of the titanium matrix and graphite surface of the sample carrier boat in a transversely heated graphite tube atomizer was investigated. Conversion of titanium dioxide to interfering TiO{sub 2}-TiC-liquid phase, running out the sampling boat, was observed at temperatures above 2000 deg. C. The temperature program was optimized accordingly for these volatile analytes in atomization and cleaning steps in order to prevent this interference and to prolong significantly the analytical lifetime of the boat to more than one thousand runs. For all elements, calibration by aqueous standard addition method, by wet-chemically analyzed samples with different content of analytes and/or by dosing one sample in different amounts, were proved as adequate quantification procedures. Linear dynamic calibration working ranges can be considerably expanded up to two orders of magnitude within one measurement run by applying three-field dynamic mode of the Zeeman background correction system. The results obtained by true direct solid sampling technique are compared with those of other independent, mostly wet-chemical methods. Very low limits of detection (3{sigma} criterion) of true solid sampling technique of 21, 0.27, 24, 3.9, 6.3 and 0.9 ng g{sup -1} were achieved for As, Cd, Hg, Pb, Sb and Zn, respectively.

  14. Psychophysically determining the maximum acceptable weight of lift for polypropylene laminated bags.

    Science.gov (United States)

    Chen, Yi-Lang; Ho, Ting-Kuang

    2016-12-07

    The objective of this study was to psychophysically determine the maximum acceptable weight of lift (MAWL) for polypropylene (PP) laminated bags. Twelve men were requested to decide their MAWLs under various task combinations involving 3 lifting ranges, 3 lifting frequencies, and 2 hand conditions. The results revealed that the MAWL was significantly affected by the frequency and range variables (all plifts. The results of multiple stepwise regression revealed that certain anthropometric data (e.g., chest circumference, wrist circumference, and acromial height) accounted for the percentage of variance for the determined MAWLs, ranging from 56.2% to 83.4%. These data can be obtained simply and quickly, and are considered the superior predictors for MAWL determination when handling PP laminated bags.

  15. Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

    Science.gov (United States)

    Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

    2016-09-29

    Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg(-1); ICP-MS, 437ngg(-1)) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses.

  16. Determination of selenium in human spermatozoa and prostasomes using base digestion and electrothermal atomic absorption spectrophotometry.

    Science.gov (United States)

    Suistomaa, U; Saaranen, M; Vanha-Perttula, T

    1987-10-15

    A method for the determination of selenium in human spermatozoa and prostasomes is described. The samples were digested with 25% (w/v) tetramethylammonium hydroxide (TMAH) in methanol and analyzed by atomic absorption spectrometry with electrothermal atomization and Zeeman background correction (ET-AAS). Nickel was used as a matrix modifier. Calibration was performed using the matrix-based calibration curve. The TMAH-digestion method agreed well with a conventional digestion procedure using concentrated nitric acid. The TMAH-digestion does not require heating or strong acids and it was suitable for small biological samples. The average recovery of added selenium in spermatozoan digests was 95.1 +/- 5.2% (n = 5). The coefficient of variation was 9.1% (n = 21). The accuracy of the method tested with the NBS standard 1577 (bovine liver, certified at 1.1 +/- 0.1 micrograms Se/g) resulted in a value of 0.98 +/- 0.10 micrograms Se/g (n = 16). The method was further tested in an interlaboratory comparison study.

  17. Dynamic light scattering and atomic force microscopy techniques for size determination of polyurethane nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Giehl Zanetti-Ramos, Betina [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil)], E-mail: betinagzramos@pq.cnpq.br; Beddin Fritzen-Garcia, Mauricia [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil); Schweitzer de Oliveira, Cristian; Avelino Pasa, Andre [Laboratorio de Filmes Finos e Superficie, Departamento de Fisica (Brazil); Soldi, Valdir [Grupo de Estudos em Materiais Polimericos, Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borsali, Redouane [Centre de Recherche sur les Macromolecules Vegetales CERMAV/CNRS, 38041 - Grenoble (France); Creczynski-Pasa, Tania Beatriz [Laboratorio de Bioenergetica e Bioquimica de Macromoleculas, Departamento de Ciencias Farmaceuticas (Brazil)

    2009-03-01

    Nanoparticles have applications in various industrial fields principally in drug delivery. Nowadays, there are several processes for manufacturing colloidal polymeric systems and methods of preparation as well as of characterization. In this work, Dynamic Light Scattering and Atomic Force Microscopy techniques were used to characterize polyurethane nanoparticles. The nanoparticles were prepared by miniemulsion technique. The lipophilic monomers, isophorone diisocyanate (IPDI) and natural triol, were emulsified in water containing surfactant. In some formulations the poly(ethylene glycol) was used as co-monomer to obtain the hydrophilic and pegylated nanoparticles. Polyurethane nanoparticles observed by atomic force microscopy (AFM) were spherical with diameter around 209 nm for nanoparticles prepared without PEG. From AFM imaging two populations of nanoparticles were observed in the formulation prepared with PEG (218 and 127 nm) while dynamic light scattering (DLS) measurements showed a monodisperse size distribution around 250 nm of diameters for both formulations. The polydispersity index of the formulations and the experimental procedures could influence the particle size determination with these techniques.

  18. A new atomic absorption spectral assay for the determination of trace IgG using immunonanogold.

    Science.gov (United States)

    Tang, Yafang; Jiang, Caina; Liang, Aihui; Li, Jishun; Jiang, Zhiliang

    2011-05-01

    Nanogold in size of 10 nm was used to label goat anti-human IgG (GIgG) to obtain an immunonanogold probe (AuGIgG) for IgG. In pH 6.8 phosphate buffer solution and in the presence of immunoprecipitator polyethylene glycol 6000 (PEG 6000), IgG reacted with the probe (AuGIgG) to form AuGIgG-IgG-PEG immunocomplex. After the centrifugation to remove the immunocomplex, AuGIgG in the supernatant can be measured by atomic absorption spectrophotometry at gold absorption line 242.8 nm. The results showed that the absorption value decreased as the concentration of IgG increased, and the decreased absorption value was linear to IgG concentration in the range 0.025-0.375 μg/mL, with a detection limit of 0.008 μg/mL. On this base, a new nanogold-labeled atomic absorption spectral assay for IgG was established. The assay was applied to determine IgG in human serum sample with satisfactory results.

  19. Determination of metal concentration in fat supplements for swine nutrition by atomic absorption spectroscopy.

    Science.gov (United States)

    Cocchi, Marina; Faeti, Valerio; Manfredini, Matteo; Manzini, Daniela; Marchetti, Andrea; Sighinolfi, Simona

    2005-01-01

    The presence of some essential and toxic metals in fat supplements for swine diet was investigated. Collected samples represented a relevant production of the Italian industry. In particular, some samples were enriched with antioxidants or waste cooking oils. The method for the determination of Ca, Cu, Cd, Fe, Mg, Mn, Ni, Pb, and Zn in fat samples was developed by means of a certified reference material (CRM 186) and a representative fatty sample (RFS). All samples were digested in closed vessels in a microwave oven and then analyzed by flame atomic absorption or graphite furnace atomic absorption spectrometry. The entire analytical method provided a satisfactory repeatability and reproducibility confirmed by agreement between the experimental recovery data obtained for the CRM 186 sample and, with the method of standard additions, for the RFS material. The samples generally showed a small amount of metals compared with the recommended daily intake for the essential elements. On the other hand, some samples contained a significant concentration, from an analytical point of view, of Cd, Ni, and Pb. Principal component analysis (PCA) was applied to inspect the experimental data obtained from samples analysis. Basically no differences were detected in terms of metal concentration among the fat supplements analyzed.

  20. Use of flameless atomic absorption spectroscopy in immune cytolysis for nonradioactive determination of killer cell activity.

    Science.gov (United States)

    Borella, P; Bargellini, A; Salvioli, S; Cossarizza, A

    1996-02-01

    We describe here a novel method to evaluate natural killer (NK) cytolytic activity by use of flameless atomic absorption spectroscopy (GF-AAS). This technique may be adopted for use in laboratories equipped with electrothermal atomic absorption spectrometers. Nonradioactive Cr as Na2CrO4 was used to label target cells (K562), and cell lysis was evaluated by measuring Cr released after 4 h of incubation with the effectors. We selected 520 micrograms/L as the optimal dose for labeling targets, between 12 and 20 h as the optimal incubation time, and 10(4) cells as the optimal target size. Advantages of this method include: (a) exclusion of radioactive tracer, with no risk for workers; (b) limited costs; (c) high sensitivity and reproducibility; (d) possibility to store samples; and (e) better control of Cr used for labeling cells due to well-determined, fixed Cr concentrations in the range of nontoxic and linear cellular uptake. Comparison with data obtained by conventional 51Cr labeling of targets killed by the same effectors was excellent, yielding comparable results and corroborating the method.

  1. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

  2. Determination of nickel in active pharmaceutical ingredients by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Bubnič, Zoran; Urleb, Uroš; Kreft, Katjuša; Veber, Marjan

    2010-03-01

    An electrothermal atomic absorption spectrometric procedure for the determination of nickel in active pharmaceutical ingredients was developed. Since the recoveries of nickel by the direct dissolution of samples in diluted nitric acid were low and caused errors in the determination of Ni in pharmaceutical samples, different approaches for sample pre-treatment were examined. It was found that the microwave digestion was the most suitable way for sample preparation. Various combinations of digestion agents and different microwave conditions were tested. The combination of nitric acid and hydrogen peroxide was found to be the most appropriate. The validity of the method was evaluated by recovery studies of spiked samples and by the comparison of the results obtained by inductively coupled plasma mass spectrometry (ICP-MS). The recovery ranged from 87.5 to 104.0% and a good agreement was achieved between both methods. The detection limit and the limit of quantification were 0.6 and 2.1 µg g-1 respectively. The precision of the method was confirmed by the determination of Ni in the spiked samples and was below 4%, expressed in terms of a relative standard deviation. The method was applied to the determination of nickel in production samples of active pharmaceutical ingredients and intermediates.

  3. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

    Science.gov (United States)

    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

    2015-06-01

    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with

  4. Determining importance weighting functions for Contributon theory eigenvalue sensitivity coefficient methodologies

    Energy Technology Data Exchange (ETDEWEB)

    Perfetti, C.; Martin, W. [Univ. of Michigan, Dept. of Nuclear Engineering and Radiological Sciences, 2355 Bonisteel Boulevard, Ann Arbor, MI 48109-2104 (United States); Rearden, B.; Williams, M. [Oak Ridge National Laboratory, Reactor and Nuclear Systems Div., Bldg. 5700, P.O. Box 2008, Oak Ridge, TN 37831-6170 (United States)

    2012-07-01

    This study introduced two new approaches for calculating the F*(r) importance weighting function for Contributon and CLUTCH eigenvalue sensitivity coefficient calculations, and compared them in terms of accuracy and applicability. The necessary levels of F*(r) mesh refinement and mesh convergence for obtaining accurate eigenvalue sensitivity coefficients were determined for two preliminary problems through two parametric studies, and the results of these studies suggest that a sufficiently accurate F*(r) mesh for calculating eigenvalue sensitivity coefficients can be obtained for these problems with only a small increase in problem runtime. (authors)

  5. Determining Importance Weighting Functions for Contributon Theory Eigenvalue Sensitivity Coefficient Methodologies

    Energy Technology Data Exchange (ETDEWEB)

    Perfetti, Christopher M [ORNL; Martin, William R [University of Michigan; Rearden, Bradley T [ORNL; Williams, Mark L [ORNL

    2012-01-01

    This study introduced three approaches for calculating the importance weighting function for Contributon and CLUTCH eigenvalue sensitivity coefficient calculations, and compared them in terms of accuracy and applicability. The necessary levels of mesh refinement and mesh convergence for obtaining accurate eigenvalue sensitivity coefficients were determined through two parametric studies, and the results of these studies suggest that a sufficiently-accurate mesh for calculating eigenvalue sensitivity coefficients can be obtained for the Contributon and CLUTCH methods with only a small increase in problem runtime.

  6. Self-determinate evaluation method based on condition of weights non-dictatorial rate

    Institute of Scientific and Technical Information of China (English)

    Zhang Danning; Yi Pingtao; Guo Yajun

    2009-01-01

    The condition of weightes non-dictatorship is extended and a comprehensive evaluae method emboding self-determinate which is combined with competitive view optimization principles is built. The basic process includes simulating the model of economic man's self-benefit bahaviors, taking the place of experts to evaluate, bringing in the model of minimizing the sum of included angles to integrate the information of multiple objects and put the objects in order finally. The method has the advangtages of less dependendence on the subjective information, plenty of information, fair process and simple caculating. Finally, an application example is given to illustrate the effectiveness of the proposed method.

  7. Molecular weight determination of block copolymers by pulsed gradient spin echo NMR.

    Science.gov (United States)

    Barrère, Caroline; Mazarin, Michaël; Giordanengo, Rémi; Phan, Trang N T; Thévand, André; Viel, Stéphane; Charles, Laurence

    2009-10-01

    Matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS) is the technique of choice to achieve molecular weight data for synthetic polymers. Because the success of a MALDI-MS analysis critically depends on a proper matrix and cation selection, which in turn relates closely to the polymer chemical nature and size, prior estimation of the polymer size range strongly helps in rationalizing MALDI sample preparation. We recently showed how pulsed gradient spin echo (PGSE) nuclear magnetic resonance could be used as an advantageous alternative to size exclusion chromatography, to rationalize MALDI sample preparation and confidently interpret MALDI mass spectra for homopolymers. Our aim here is to extend this methodology to the demanding case of amphiphilic block copolymers, for which obtaining prior estimates on the Mw values appears as an even more stringent prerequisite. Specifically, by studying poly(ethylene oxide) polystyrene block copolymers of distinct molecular weights and relative block weight fractions, we show how PGSE data can be used to derive the block Mw values. In contrast to homopolymers, such determination requires not only properly recorded calibration curves for each of the polymers constituting the block copolymers but also an appropriate hydrodynamic model to correctly interpret the diffusion data.

  8. Determination of ionization potential of atomic gadolinium and its isotope effect. Analysis of unperturbed Rydberg series

    Energy Technology Data Exchange (ETDEWEB)

    Miyabe, Masabumi; Ohba, Masaki; Wakaida, Ikuo [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1997-10-01

    Autoionizing Rydberg series converging to six states (0, 261.841, 633.273, 3082.011, 3427.274, 3444.235 cm{sup -1}) of Gd ion have been observed by using three-color three-step photoionization via ten different 2nd-step levels of J=0 or 1. While the perturbations with interlopers become significant in the region of n=30-35 for most of the observed series, long and well-defined series structures appeared in higher energy region. From an analysis of such unperturbed structures, the first ionization potential of Gd atom was estimated to be 49601.45 (30) cm{sup -1}. This is in good agreement with the previous value, but the accuracy is improved by about one order of magnitude. In addition, isotope effect on the ionization potential was also determined by isotope shifts of some Rydberg series. (author)

  9. Determination of the actuator sensitivity of electromechanical polypropylene films by atomic force microscopy

    Science.gov (United States)

    Peltonen, Jouko; Paajanen, Mika; Lekkala, Jukka

    2000-10-01

    The actuator functionality of electromechanical polypropylene films was studied using atomic force microscopy. The film carries a permanent electric charge and includes microbubbles as a result of two-dimensional stretching of the film. The thickness change of various film structures covered with electrodes was measured as a function of external voltage. The dependence was found to be nonlinear, the thickness change in the range 0.001%-0.1% of the total film thickness and affected by the internal charge density of the film. Applying a capacitor model including an air gap within the polymer layer enabled the determination of the Young's modulus, the interfacial charge density and the actuator sensitivity of the studied structures.

  10. Study of effective atomic number of breast tissues determined using the elastic to inelastic scattering ratio

    Science.gov (United States)

    Antoniassi, M.; Conceição, A. L. C.; Poletti, M. E.

    2011-10-01

    In this work we have measured Compton and Rayleigh scattering radiation from normal (adipose and fibroglandular), benign (fibroadenoma) and malignant (ductal carcinoma) breast tissues using a monoenergetic beam of 17.44 keV and a scattering angle of 90° ( x=0.99 Å -1). A practical method using the area of Rayleigh and Compton scattering was used for determining the effective atomic number ( Zeff) of the samples, being validated through measurements of several reference materials. The results show that there are differences in the distributions of Zeff of breast tissues, which are mainly related to the elemental composition of carbon ( Z=6) and oxygen ( Z=8) of each tissue type. The results suggest that is possible to use the method to characterize the breast tissues permitting study histological features of the breast tissues related to their elemental composition.

  11. Determination of palladium by graphite furnace atomic absorption spectroscopy without matrix matching.

    Science.gov (United States)

    Jia, X; Wang, T; Wu, J

    2001-05-30

    A graphite furnace atomic absorption spectroscopy method for the analysis of the palladium (Pd) content in bulk pharmaceutical drug substances and their intermediates prepared in aqueous solutions is extended to samples prepared in acetonitrile (ACN) and ACN-water mixtures as well to samples prepared in dimethyl sulfoxide (DMSO) and DMSO-water mixtures. The Pd content in samples solubilized in these solvents can be accurately determined with calibration established with standards prepared in aqueous solutions without matrix matching or using the method of standard additions. The validity of this method is demonstrated by spike recovery studies and by the agreement with results for the same samples prepared in these solvents, in concentrated nitric acid, and prepared by a microwave digestion system.

  12. Determination of calcium, magnesium and zinc in unused lubricating oils by atomic absorption spectroscopy.

    Science.gov (United States)

    Udoh, A P

    1995-12-01

    Varying concentrations of lanthanum and strontium were added to solutions of ashed unused lubricating oils for the determination of calcium, magnesium and zinc content using flame atomic absorption spectrophotometry. At least 3000 mug g(-1) of lanthanum or strontium was required to completely overcome the interference of the phosphate ion, PO(3-)(4), and give peak values for calcium. The presence of lanthanum or strontium did not cause an appreciable increase in the amount of magnesium and zinc obtained from the analyses. The method is fast and reproducible, and the coefficients of variation calculated for the elements using one of the samples were 1.6% for calcium, 3.5% for magnesium and 0.2% for zinc. Results obtained by this method were better than those obtained by other methods for the same samples.

  13. Determination of barium in bottled drinking water by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Fagioli, F.; Locatelli, C.; Lanciotti, E.; Vallone, G.; Mazzotta, D.; Mugelli, A.

    1988-11-01

    In relation to the wide environmental spread of barium and to its cardiovascular effects, barium levels were determined by graphite furnace atomic absorption spectrometry in 60 different brands of bottled water marketed in Italy. Matrix interferences were investigated in order to evaluate the use of an analytical calibration function rather than the much more time consuming addition technique. The barium content ranged from limit of detection C/sub L/ (7.0 ..mu..g/1) up to 660 ..mu..g/1, the median value being 80 ..mu..g/l, while the recovery tests varied between 90 and 110% and the precision of the method (s/sub yx/) was 2.5%.

  14. Study of effective atomic number of breast tissues determined using the elastic to inelastic scattering ratio

    Energy Technology Data Exchange (ETDEWEB)

    Antoniassi, M.; Conceicao, A.L.C. [Departamento de Fisica e Matematica, Faculdade de Filosofia Ciencias e Letras de Ribeirao Preto, Universidade de Sao Paulo, Ribeirao Preto, Sao Paulo (Brazil); Poletti, M.E., E-mail: poletti@ffclrp.usp.br [Departamento de Fisica e Matematica, Faculdade de Filosofia Ciencias e Letras de Ribeirao Preto, Universidade de Sao Paulo, Ribeirao Preto, Sao Paulo (Brazil)

    2011-10-01

    In this work we have measured Compton and Rayleigh scattering radiation from normal (adipose and fibroglandular), benign (fibroadenoma) and malignant (ductal carcinoma) breast tissues using a monoenergetic beam of 17.44 keV and a scattering angle of 90{sup o} (x=0.99 A{sup -1}). A practical method using the area of Rayleigh and Compton scattering was used for determining the effective atomic number (Z{sub eff}) of the samples, being validated through measurements of several reference materials. The results show that there are differences in the distributions of Z{sub eff} of breast tissues, which are mainly related to the elemental composition of carbon (Z=6) and oxygen (Z=8) of each tissue type. The results suggest that is possible to use the method to characterize the breast tissues permitting study histological features of the breast tissues related to their elemental composition.

  15. Atomic site occupation determined by magnetism in the Heusler alloy Mn{sub 2}CoGa doped with Cr

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Y.J. [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China); School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300401 (China); Li, G.J.; Liu, E.K.; Chen, J.L.; Wang, W.H. [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China); Meng, F.B. [School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300401 (China); Wu, G.H., E-mail: ghwu@aphy.iphy.ac.cn [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China)

    2014-12-01

    The atomic configuration and magnetic properties of Mn{sub 2}CoM{sub x}Ga{sub 1−x} (M=Cr and Ni) Heusler alloys have been investigated by experiments and calculations. Doping with Ni leads to a magnetic moment change of 5.92 μ{sub B}/atom, giving rise to a local FM structure in the ferrimagnetic matrix. On the other hand, a moment change of 3.61 μ{sub B}/atom is experimentally observed in Cr-doped alloys, which is very large compared with the atomic moment of about 2 μ{sub B}/Cr atom in other Heusler alloys. Electronic-structure calculations are presented which indicate that, in contrast with Ni-doped alloys, the magnetism favors the doped Cr atoms to occupy unusual atomic sites. This is opposite to the effect of the covalent bonding in Ni-doped alloys and disobeys the empirical site-occupation rule for Heusler alloys. Due to the difference in electronegativity of the dopants, the covalent bonding in Mn{sub 2}CoGa doped with Ti, V and Cr is weaker than in alloys doped with Fe, Co and Ni. Because Cr has a higher magnetic moment than Ti and V, the magnetism determines, in this weak-covalent environment, an atomic site occupation by Cr which does not obey the empirical rule. This provides clear evidence for the impact of magnetism on the crystalline structure of Heusler alloys.

  16. Determination of diffusion, reflection and deexcitation coefficients of metastable excited Ne(3P2) atom

    Science.gov (United States)

    Suzuki, S.; Itoh, H.

    2016-05-01

    The diffusion coefficient of the metastable excited Ne(3P2) atom in neon, the reflection coefficient of Ne(3P2) at the surface of an electrode and the rate coefficient of Ne(3P2) for collisional quenching by Ne(1S0) were determined from the gas pressure dependence of the effective lifetime of Ne(3P2). The effective lifetime of Ne(3P2) was measured from the transient current after turning off the Ultraviolet (UV) light in a Townsend discharge. The observed transient current waveform was analysed by solving the diffusion equation for the metastable excited Ne(3P2) atom using the third kind of boundary condition. The rate coefficient of Ne(3P2) for collisional quenching by Ne(1S0) and the reflection coefficient were determined by a nonspectroscopic method for the first time in neon to the best of our knowledge and were (3.2  ±  0.4)  ×  10-16 cm3 s-1 and 0.10  ±  0.04, respectively. The obtained diffusion coefficient at 1 Torr was 177  ±  17 cm2 s-1, which is consistent with the value reported by Dixon and Grant. Moreover, the present results are compared with the results of Phelps and were found to be in good agreement. We also discuss the deexcitation rate of Ne(3P2) at pressures of up to 60 Torr in comparison with previously reported values.

  17. [Determination of nine mineral elements in hulless barley by ultraviolet spectrophotometry and flame atomic absorption spectrometry].

    Science.gov (United States)

    Liu, Jin; Zhang, Huai-Gang

    2010-04-01

    The contents of nine mineral elements, including sulphur, zinc, calcium, magnesium, potassium, sodium, iron, copper and manganese in five hulless barley (Hordeum vulgare L. var. nudum Hook. f.) lines were determined by ultraviolet spectrophotometry and flames atomic absorption spectrometry (FAAS). For the determination of sulphur, the samples were dissolved by magnesia and anhydrous sodium carbonate at 250 degrees C for 0. 5 h and at 550 degrees C for 3 h in the muffle furnace, and then a certain amount of barium chloride was put into the sample solution for colorimetry of the UV-Vs spectrophotometer. For the determination of other eight mineral elements, all of the samples were dissolved by a kind of incinerating method: first, the sample was put into the muffle furnace at 250 degrees C for 0. 5 h and at 550 degrees C for 2.5 h, then two droplets of 50%HNO3 were distributed into each sample, and the last step was putting the sample into the muffle furnace at 550 degrees C for 0.5 h. And then all of the ash was dissolved by 50%HNO3 to 50 milliliter and determined by flames atomic absorption spectrometry. The precision, accuracy, repeatability and stability of the method were discussed too. The results showed that the relative standard deviations (RSD) were between 1.2% and 3.7%; The average recoveries were 97.44%-101.52% and the relative standard deviations (RSD) of sample determination were 1.3%-3.8%. The repeatability experiment showed that the relative standard deviations (RSD) were 2.6%-6.1%. And the content of each mineral element was the same after 24 hours; All these showed that the method has a good precision, accuracy, repeatability and stability. In all the hulless barley samples, the average contents were in the order of K > S > Mg > Ca > Fe > Na > Zn > Mn > Cu, and the contents of zinc, iron and manganese closely related to people's health were relatively higher than other crops. The data of the experiment could provide an accurate and credible evidence

  18. Energy Intake and Energy Expenditure for Determining Excess Weight Gain in Pregnant Women

    Science.gov (United States)

    Gilmore, L. Anne; Butte, Nancy F.; Ravussin, Eric; Han, Hongmei; Burton, Jeffrey H.; Redman, Leanne M.

    2016-01-01

    Objective To conduct a secondary analysis designed to test whether gestational weight gain is due to increased energy intake or adaptive changes in energy expenditures. Methods In this secondary analysis, energy intake and energy expenditure of 45 pregnant women (BMI 18.5–24.9 kg/m2, n=33 and BMI ≥ 25, n=12) were measured preconceptionally 22, and 36 weeks of gestation. Energy intake was calculated as the sum of total energy expenditure measured by doubly labeled water and energy deposition determined by the 4-compartment body composition model. Weight, body composition, and metabolic chamber measurement were completed preconceptionally, 9, 22, and 36 weeks of gestation. Basal metabolic rate was measured by indirect calorimetry in a room calorimeter and activity energy expenditure by doubly labeled water. Results Energy intake from 22 to 36 weeks of gestation was significantly higher in high gainers (n=19) (3437 ± 99 kcal/d) versus low + ideal gainers (n=26) (2687 ± 110 pbody composition changes with gestational weight gain was not significantly different between high gainers and low + ideal gainers (151 ± 33 vs. 129 ± 36 kcal/d; p=.66). Activity energy expenditure decreased throughout pregnancy in both groups (low + ideal gainers: −150 ± 70 kcal/d; p=.04 and high gainers: −230 ± 92 kcal/day; p=.01), but there was no difference between high gainers and low + ideal gainers (p=.49). Conclusion Interventions designed to increase adherence to the IOM guidelines for weight gain in pregnancy may have increased efficacy if focused on limiting energy intake while increasing nutrient density and maintaining levels of physical activity. PMID:27054928

  19. Determination of Inorganic Arsenic Species by Electrochemical Hydride Generation Atomic Absorption Spectrometry with Selective Electrochemical Reduction

    Institute of Scientific and Technical Information of China (English)

    LI Xun; WANG Zheng-Hao

    2007-01-01

    A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As(Ⅲ) shows significantly higher absorbance at low electrolytic currents than As(Ⅴ) in 0.3 mol·L-1 H2SO4.The electrolytic current used for the determination of As(Ⅲ) without considerable interferences of As(V) was 0.4 A, whereas the current for the determination of As(Ⅲ)and As(V) was 1.2 A. For equal concentrations of As(Ⅲ) and As(V) in a sample, the interferences of As(V) during the As(Ⅲ) determination were smaller than 5%. The absorbance for As(V) could be calculated by subtracting that for As(Ⅲ) measured at 0.4 A from the total absorbance for As(Ⅲ) and As(V) measured at 1.2 A, and then the concentration of As(V) can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·ml-1 for As(Ⅲ) and As(V) respectively.The relative standrad deviations were of 3.5% for 20 ng·ml-1 As(Ⅲ) and 302% for 20 ng·ml-1 As(V).The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.

  20. [Determination of mercury in shark liver by cold atom fluorescence spectrometry after microwave dissolution].

    Science.gov (United States)

    Weng, Di

    2005-12-01

    The conditions for the determination of mercury in shark liver by cold atom fluorescence spectrometry (CAFS) with microwave dissolution were studied. After being dried completely, the method employed 2 mol x L(-1) HNO3-4 mol x L(-1) HCl as an oxidant, and with catalysis by V2O5, the samples were digested in a microwave oven. The mercury in absorption solution was reduced by SnCl2, and then was determined by CAFS at wavelength of 253.7 nm. 10% SnCl2 solution was used as a reductive agent for mercury. The linear range was 0-2.0 ng x mL(-1) mercury (r = 0.999 7). The detection limit was 0.05 ng x mL(-1), the relative standard deviation was 0.86%-2.22%, and the average recovery rate was 96.0%-108.5%. The method was suitable for the determination of mercury in shark liver.

  1. Novel Method for Indirect Determination of Iodine in Marine Products by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    LU Jian-ping; TAN Fang-wei; TANG Qiong; JIANG Tian-cheng

    2013-01-01

    A method for the determination of iodine based upon compound H2HgI4,formed between I-and Hg2+ in nitric acid and extracted in methyl isobutyl ketone(MIBK),was developed via atomic fluorescence spectrometry(AFS).After the compound is reduced with potassium borohydrid(KBH4),the resultant mercury vapor was injected into the instrument and iodine was,therefore,indirectly determined.Experimental parameters such as the conditions of extraction reagents,aqueous phase acidity,elemental mercury diffusion temperature in a vial and other factors were investigated and optimized.Under the optimum experimental conditions,this method shows a detection limit of 0.038 μg/L iodine and a linear relationship between 0.04-20 μg/L.The method was applied to determining the iodine content in marine duck eggs,kelps,laver and Ganoderma lucidum spirulina,showing a relative standard deviation(RSD) of 2.15% and the recoveries in the range of 98.1%-102.5%.

  2. [The determination of chromium in feeds by flame atomic absorption spectrophotometry].

    Science.gov (United States)

    Wang, Jian; Jia, Bin; Guo, Li-ping; Lin, Qiu-ping

    2005-07-01

    Chromium in feeds is regulated by China Standard GB 13078-2001. A method of flame atomic absorption spectrophotometry for the determination of Cr in feeds has been developed in allusion to shortage of China standard method. Several acetylene flow-rate, burner-high and the additive of interference suppressor NH4Cl were studied respectively on the effect of sensitivities of Cr(III) and Cr(VI). The two sets analytical average results of Cr in feed sample determined by calibration curves of Cr(III) and Cr(VI) were tested by t test, no marked discrepancy was found. Optimum instrumental conditions of Cr(III) and Cr(VI) with same sensitivity were confirmed. Sensitivity was 0.014 microg x mL(-1) with detection limit 0.70 mg x kg(-1). The recoveries were 94.4%-104.9%. Relative standard deviation of sample determination (5-6 times) was 1.90%-4.08%. This method is simply, fast and exact, the detection limit was answered for Cr limit in feeds regulated by GB 13078-2001, it can be applied to the analysis of Cr in feeds.

  3. Determination of myo-inositol hexakisphosphate (phytate) in urine by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grases, F.; Perello, J.; Isern, B.; Prieto, R.M

    2004-05-10

    Myo-inositol hexakisphosphate (phytate) is a substance present in urine with an important role in preventing calcium renal calculi development. In spite of this, the use of urinary phytate levels on stone-formers' evaluation and treatment is still notably restricted as a consequence of the enormous difficulty to analyze this substance in urine. In this paper, a simple procedure for routinary urinary phytate determination based on phosphorus determination through inductively coupled plasma atomic emission spectrometry is described. The method only requires a previous separation of phytate from other components by column anion exchange chromatography. The working linear range used was 0-2 mg l{sup -1} phosphorus (0-7 mg l{sup -1} phytate). The limit of detection was 64 {mu}g l{sup -1} of phytate and the limit of quantification was 213 {mu}g l{sup -1}. The relative standard deviation (R.S.D.) for 1.35 mg l{sup -1} phytate was 2.4%. Different urine samples were analyzed using an alternative analytical methodology based on gas chromatography (GC)/mass detection used for inositol determination (phytate was previously hydrolyzed), resulting both methods comparable using as criterion to assess statistical significance P<0.05.

  4. ALMOST: an all atom molecular simulation toolkit for protein structure determination.

    Science.gov (United States)

    Fu, Biao; Sahakyan, Aleksandr B; Camilloni, Carlo; Tartaglia, Gian Gaetano; Paci, Emanuele; Caflisch, Amedeo; Vendruscolo, Michele; Cavalli, Andrea

    2014-05-30

    Almost (all atom molecular simulation toolkit) is an open source computational package for structure determination and analysis of complex molecular systems including proteins, and nucleic acids. Almost has been designed with two primary goals: to provide tools for molecular structure determination using various types of experimental measurements as conformational restraints, and to provide methods for the analysis and assessment of structural and dynamical properties of complex molecular systems. The methods incorporated in Almost include the determination of structural and dynamical features of proteins using distance restraints derived from nuclear Overhauser effect measurements, orientational restraints obtained from residual dipolar couplings and the structural restraints from chemical shifts. Here, we present the first public release of Almost, highlight the key aspects of its computational design and discuss the main features currently implemented. Almost is available for the most common Unix-based operating systems, including Linux and Mac OS X. Almost is distributed free of charge under the GNU Public License, and is available both as a source code and as a binary executable from the project web site at http://www.open-almost.org. Interested users can follow and contribute to the further development of Almost on http://sourceforge.net/projects/almost.

  5. Determination of Anionic Surfactants Using Atomic Absorption Spectrometry and Anodic Stripping Voltammetry

    Science.gov (United States)

    John, Richard; Lord, Daniel

    1999-09-01

    An experiment has been developed for our undergraduate analytical chemistry course that demonstrates the indirect analysis of anionic surfactants by techniques normally associated with metal ion determination; that is, atomic absorption spectroscopy (AAS) and anodic stripping voltammetry (ASV). The method involves the formation of an extractable complex between the synthetic surfactant anion and the bis(ethylenediamine)diaqua copper(II) cation. This complex is extracted into chloroform and then back-extracted into dilute acid. The resulting Cu(II) ions are determined by AAS and ASV. Students are required to determine the concentration of a pre-prepared "unknown" anionic surfactant solution and to collect and analyze a real sample of their choice. After the two extraction processes, students typically obtain close to 100% analytical recovery. Correlation between student AAS and ASV results is very good, indicating that any errors that occur probably result from their technique (dilutions, extractions, preparation of standards, etc.) rather than from the end analyses. The experiment is a valuable demonstration of the following analytical principles: indirect analysis; compleximetric analysis; liquid-liquid (solvent) extraction; back-extraction (into dilute acid); analytical recovery; and metal ion analysis using flame-AAS and ASV.

  6. Hankel Determinant and Orthogonal Polynomials for a Gaussian Weight with a Discontinuity at the Edge

    Science.gov (United States)

    Bogatskiy, A.; Claeys, T.; Its, A.

    2016-10-01

    We compute asymptotics for Hankel determinants and orthogonal polynomials with respect to a discontinuous Gaussian weight, in a critical regime where the discontinuity is close to the edge of the associated equilibrium measure support. Their behavior is described in terms of the Ablowitz-Segur family of solutions to the Painlevé II equation. Our results complement the ones in [33]. As consequences of our results, we conjecture asymptotics for an Airy kernel Fredholm determinant and total integral identities for Painlevé II transcendents, and we also prove a new result on the poles of the Ablowitz-Segur solutions to the Painlevé II equation. We also highlight applications of our results in random matrix theory.

  7. Absolute number densities of helium metastable atoms determined by atomic absorption spectroscopy in helium plasma-based discharges used as ambient desorption/ionization sources for mass spectrometry

    Science.gov (United States)

    Reininger, Charlotte; Woodfield, Kellie; Keelor, Joel D.; Kaylor, Adam; Fernández, Facundo M.; Farnsworth, Paul B.

    2014-10-01

    The absolute number densities of helium atoms in the 2s 3S1 metastable state were determined in four plasma-based ambient desorption/ionization sources by atomic absorption spectroscopy. The plasmas included a high-frequency dielectric barrier discharge (HF-DBD), a low temperature plasma (LTP), and two atmospheric-pressure glow discharges, one with AC excitation and the other with DC excitation. Peak densities in the luminous plumes downstream from the discharge capillaries of the HF-DBD and the LTP were 1.39 × 1012 cm- 3 and 0.011 × 1012 cm- 3, respectively. Neither glow discharge produced a visible afterglow, and no metastable atoms were detected downstream from the capillary exits. However, densities of 0.58 × 1012 cm- 3 and 0.97 × 1012 cm- 3 were measured in the interelectrode regions of the AC and DC glow discharges, respectively. Time-resolved measurements of metastable atom densities revealed significant random variations in the timing of pulsed absorption signals with respect to the voltage waveforms applied to the discharges.

  8. Antiproton–to–electron mass ratio determined by two-photon laser spectroscopy of antiprotonic helium atoms

    Directory of Open Access Journals (Sweden)

    Sótér A.

    2014-03-01

    Full Text Available The ASACUSA collaboration of CERN has recently carried out two-photon laser spectroscopy of antiprotonic helium atoms. Three transition frequencies were determined with fractional precisions of 2.3–5 parts in 109. By comparing the results with three-body QED calculations, the antiproton-to-electron mass ratio was determined as 1836.1526736(23.

  9. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Alexandre de; Zmozinski, Ariane Vanessa [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Damin, Isabel Cristina Ferreira [Faculdade Dom Bosco de Porto Alegre, 90520-280, Porto Alegre, RS (Brazil); Silva, Marcia Messias, E-mail: mmsilva@iq.ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti Rodrigues [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2012-05-15

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 {mu}g kg{sup -1} for arsenic and 0.2 {mu}g kg{sup -1} for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a 'cold finger' was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis. - Highlights: Black-Right-Pointing-Pointer A direct sampling GF AAS method to determine As and Cd in crude oil was proposed. Black-Right-Pointing-Pointer The conventional chemical modifier Pd/Mg has been used to stabilize As and Cd. Black

  10. Determination of some antihistaminic drugs by atomic absorption spectrometry and colorimetric methods.

    Science.gov (United States)

    El-Kousy, N; Bebawy, L I

    1999-08-01

    Atomic absorption spectrometry (AAS) and colourimetric methods have been developed for the determination of pizotifen (I), ketotifen (II) and loratadine (III). The first method depends on the reaction of the three drugs (I); (II) and (III) with cobalt thiocyanate reagent at pH 2 to give ternary complexes. These complexes are readily extracted with organic solvent and estimated by indirect atomic absorption method via the determination of the cobalt content in the formed complex after extraction in 0.1 M hydrochloric acid. It was found that the three drugs can be determined in the concentration ranges from 10 to 74, 12 to 95 and 10 to 93 microg ml(-1) with mean percentage recovery of 99.71+/-0.87, 99.70+/-0.79 and 99.62+/-0.75%, respectively. The second method is based on the formation of orange red ion pairs as a result of the reaction between (I); (II) and (III) and molybdenum thiocyanate with maximum absorption at 469.5 nm in dichloromethane. Appropriate conditions were established for the colour reaction. Under the proposed conditions linearity was obeyed in the concentration ranges 3.5-25, 5-37.5 and 2.5-22.5 microg ml(-1) with mean percentage recovery of 99.60+/-0.41, 100.11+/-0.43 and 99.31+/-0.47% for (I): (II) and (III), respectively. The third method depends on the formation of radical ion using 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ). The colour formed was measured at 588 nm for the three drugs (I); (II) and (III), respectively. The method is valid in concentration range 10-80 microg ml(-1) with mean percentage recovery 99.75+/-0.44, 99.94+/-0.72 and 99.17+/-0.36% for (I); (II) and (III), respectively. The proposed methods were applied to the analysis of pharmaceutical preparations. The results obtained were statistically analysed and compared with those obtained by applying the official and reference methods.

  11. Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos; Silva, Erik G.P. da; Fernandes, Marcelo S.; Araujo, Rennan G.O.; Costa, Anto' ' enio C.S.; Ferreira, Sergio L.C. [Nucleo de Excelencia em Quimica Analitica da Bahia, Universidade Federal da Bahia, Instituto de Quimica, Salvador, Bahia (Brazil); Vale, M.G.R. [Instituto de Quimica, Universidade Federal da Bahia do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul (Brazil)

    2005-06-01

    Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L{sup -1} hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L{sup -1} hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 {mu}g g{sup -1} and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 {mu}g g{sup -1}, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 {mu}g g{sup -1}. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison. (orig.)

  12. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, Mariela N.M.; Cervera, Maria L.; Guardia, Miguel de la, E-mail: m.luisa.cervera@uv.e [University of Valencia, Valencia (Spain). Dept. of Analytical Chemistry

    2011-07-01

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L{sup -1} phosphoric acid, 1 mol L{sup -1} nitric acid, aqua regia, 1 mol L{sup -1} sulfuric acid and 6 mol L{sup -1} hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H{sub 2}SO{sub 4} the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g{sup -1} with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  13. An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    MAHMOUD MOHAMED ISSA

    2008-05-01

    Full Text Available A highly sensitive indirect atomic absorption spectrophotometric (AAS method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III. The excess of iron(III was extracted into diethyl ether and then the iron(II in the aqueous layer was aspirated into an air–acetylene flame and determined by AAS. The linear concentration ranges were 25–400, 50–500 and 60–600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

  14. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  15. Determination of firing distance. Lead analysis on the target by atomic absorption spectroscopy (AAS).

    Science.gov (United States)

    Gagliano-Candela, Roberto; Colucci, Anna P; Napoli, Salvatore

    2008-03-01

    This paper reports a method for the determination of the firing distance. Atomic absorption spectroscopy (AAS) was used to determine the lead (Pb) pattern around bullet holes produced by shots on test targets from the gun. Test shots were made with a Colt 38 Special at 5, 10, 20, 25, 30, 35, 40, 45, 50, 60, 80, and 100 cm target distance. The target was created with sheets of Whatman no. 1 paper on a polystyrene support. The target was subdivided into three carefully cut out rings (1, 2, and 3; with external diameters of 1.4 cm; 5 cm; 10.2 cm, respectively). Each sample was analyzed with graphite furnace AAS. Lead values analysis performed for each ring yielded a linear relation between the firing distance (cm) and the logarithm of lead amounts (microg/cm(2)) in definite target areas (areas 2 + 3): [ln dPb(2+3) = a(0) + a(1)l]; where dPb(2+3) = lead microg/cm(2) of area 2 + 3; a(0) and a(1) are experimentally calculated; l = distance in cm.

  16. Atomic charge transfer-counter polarization effects determine infrared CH intensities of hydrocarbons: a quantum theory of atoms in molecules model.

    Science.gov (United States)

    Silva, Arnaldo F; Richter, Wagner E; Meneses, Helen G C; Bruns, Roy E

    2014-11-14

    Atomic charge transfer-counter polarization effects determine most of the infrared fundamental CH intensities of simple hydrocarbons, methane, ethylene, ethane, propyne, cyclopropane and allene. The quantum theory of atoms in molecules/charge-charge flux-dipole flux model predicted the values of 30 CH intensities ranging from 0 to 123 km mol(-1) with a root mean square (rms) error of only 4.2 km mol(-1) without including a specific equilibrium atomic charge term. Sums of the contributions from terms involving charge flux and/or dipole flux averaged 20.3 km mol(-1), about ten times larger than the average charge contribution of 2.0 km mol(-1). The only notable exceptions are the CH stretching and bending intensities of acetylene and two of the propyne vibrations for hydrogens bound to sp hybridized carbon atoms. Calculations were carried out at four quantum levels, MP2/6-311++G(3d,3p), MP2/cc-pVTZ, QCISD/6-311++G(3d,3p) and QCISD/cc-pVTZ. The results calculated at the QCISD level are the most accurate among the four with root mean square errors of 4.7 and 5.0 km mol(-1) for the 6-311++G(3d,3p) and cc-pVTZ basis sets. These values are close to the estimated aggregate experimental error of the hydrocarbon intensities, 4.0 km mol(-1). The atomic charge transfer-counter polarization effect is much larger than the charge effect for the results of all four quantum levels. Charge transfer-counter polarization effects are expected to also be important in vibrations of more polar molecules for which equilibrium charge contributions can be large.

  17. Ultratrace determination of lead by hydride generation in-atomizer trapping atomic absorption spectrometry: Optimization of plumbane generation and analyte preconcentration in a quartz trap-and-atomizer device

    Energy Technology Data Exchange (ETDEWEB)

    Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz

    2012-05-15

    A compact trap-and-atomizer device and a preconcentration procedure based on hydride trapping in excess of oxygen over hydrogen in the collection step, both constructed and developed previously in our laboratory, were employed to optimize plumbane trapping in this device and to develop a routine method for ultratrace lead determination subsequently. The inherent advantage of this preconcentration approach is that 100% preconcentration efficiency for lead is reached in this device which has never been reported before using quartz or metal traps. Plumbane is completely retained in the trap-and-atomizer device at 290 Degree-Sign C in oxygen-rich atmosphere and trapped species are subsequently volatilized at 830 Degree-Sign C in hydrogen-rich atmosphere. Effect of relevant experimental parameters on plumbane trapping and lead volatilization are discussed, and possible trapping mechanisms are hypothesized. Plumbane trapping in the trap-and-atomizer device can be routinely used for lead determination at ultratrace levels reaching a detection limit of 0.21 ng ml{sup -1} Pb (30 s preconcentration, sample volume 2 ml). Further improvement of the detection limit is feasible by reducing the blank signal and increasing the trapping time. - Highlights: Black-Right-Pointing-Pointer In-atomizer trapping HG-AAS was optimized for Pb. Black-Right-Pointing-Pointer A compact quartz trap-and-atomizer device was employed. Black-Right-Pointing-Pointer Generation, preconcentration and atomization steps were investigated in detail. Black-Right-Pointing-Pointer 100% preconcentration efficiency for lead was reached. Black-Right-Pointing-Pointer Routine analytical method was developed for Pb determination (LOD of 0.2 ng ml{sup -1} Pb).

  18. Determination of zinc in serum, blood, and ultrafiltrate fluid from patients on hemofiltration by graphite furnace/atomic absorption spectroscopy or flow injection analysis/atomic absorption spectroscopy.

    Science.gov (United States)

    de Blas, O J; Rodriguez, R S; Mendez, J H; Tomero, J A; Gomez, B de L; Gonzalez, S V

    1994-01-01

    Two methods were optimized for the determination of zinc in samples of blood, serum, and ultrafiltrate fluid from patients with chronic renal impairment undergoing hemofiltration. In the first procedure, after acid digestion of the samples, Zn in blood and serum is determined by a system coupled to flow injection analysis and atomic absorption spectroscopy. The method is rapid, automated, simple, needs small amounts of sample, and has acceptable analytical characteristics. The analytical characteristics obtained were as follows: determination range of method, 0.05-2.0 ppm of Zn; precision as coefficient of variation (CV), 5.3%; recovery, 95-105%; and detection limit (DL), 0.02 ppm. The second method is optimized for ultrafiltrate fluid because the sensitivity of the first procedure is not suitable for the levels of Zn (ppb or ng/mL) in these samples. The technique chosen was atomic absorption spectroscopy with electrothermal atomization in a graphite furnace. The analytical characteristics obtained were as follows: determination range of method, 0.3-2.0 ppb Zn; CV, 5.7%; recovery, 93-107%; and DL, 0.12 ppb. The methods were used to determine zinc in samples of blood, serum, and ultrafiltrate fluid from 5 patients with chronic renal impairment undergoing hemofiltration to discover whether there were significant differences in the zinc contents of blood, serum, and ultrafiltrate fluid after the hemofiltration process. An analysis of variance of the experimental data obtained from a randomly selected group of 5 patients showed that zinc concentrations in the ultrafiltrate fluid, venous blood, and venous serum do not vary during hemofiltration (p < 0.05), whereas in arterial blood and serum, the time factor has a significant effect.

  19. Determining resource intensity weights in ambulatory chemotherapy related to nursing workload.

    Science.gov (United States)

    Green, Esther; Preyra, Colin; Stewart, Janice; McLennan, Cindy; Bland, Rosemary; Dus, Tamara; Langhorn, Marcia; Beattie, Kathy; Cheung, Annie; Hertz, Sherrie; Sechter, Haim; Burns, Judy; Angus, Helen; Sawka, Carol

    2012-01-01

    Ontario cancer programs aim to deliver high-quality nursing care and treatment that is safe for patients and staff. The reality of health care is that financial constraints, inherent in the delivery of care, require that funding mechanisms count not only the cost of drugs, but factors such as pharmacy and nursing human resource costs. While some organizations have developed patient classification systems to measure nursing intensity and workload, these systems apply primarily to inpatient populations, and are fraught with numerous challenges, such as the need for nurses to document to justify the workload required for care. The purpose of this paper is to outline the methodology and engagement of nurses to develop regimen-based resource intensity weights that can be applied to ambulatory chemotherapy suites. The methodology included determination of workload related to nursing time to prepare, teach, counsel and assess patients, as well as time to gather supplies, access lines, monitor, manage adverse reactions, manage symptoms and document care. Resource intensity weights provide better measures of the complexity of care required by cancer patients in ambulatory settings.

  20. Understanding the Determinants of Weight-Related Quality of Life among Bariatric Surgery Candidates

    Directory of Open Access Journals (Sweden)

    Annie Tessier

    2012-01-01

    Full Text Available Obesity and its relation to quality of life are multifaceted. The purpose of this paper was to contribute evidence to support a framework for understanding the impact of obesity on quality of life in 42 morbidly obese subjects considering a wide number of potential determinants. A model of weight-related quality of life (WRQL was developed based on the Wilson-Cleary model, considering subjects' weight characteristics, arterial oxygen pressure (PaO2, walking capacity (6-minute walk test, 6MWT, health-related quality of life (HRQL; Physical and Mental Component Summaries of the SF-36 PCS/MCS, and WRQL. The model of WRQL was tested with linear regressions and a path analysis, which showed that as PaO2 at rest increased 6MWT increased. 6MWT was positively associated with the PCS, which in turn was positively related to WRQL along with the MCS. The model showed good fit and explained 38% of the variance in WRQL.

  1. Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Bruhn, C G; Huerta, V N; Neira, J Y

    2004-01-01

    Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 microg) and Rh (2.0 microg) modifiers and in the digest solutions of the study matrices, Rh (2.0 microg) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25-100 microg L(-1)) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3 sigmablank/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300-400 firings. Validation was by determination of As in the certified reference material (CRM) of "Oyster tissue" solution with a percentage relative error (Erel%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94 +/- 8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h(-1)), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers.

  2. Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    de Jesus, Robson M; Silva, Laiana O B; Castro, Jacira T; de Azevedo Neto, Andre D; de Jesus, Raildo M; Ferreira, Sergio L C

    2013-03-15

    In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 μg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 μg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method.

  3. Determination of a high spatial resolution geopotential model using atomic clock comparisons

    Science.gov (United States)

    Lion, G.; Panet, I.; Wolf, P.; Guerlin, C.; Bize, S.; Delva, P.

    2017-01-01

    Recent technological advances in optical atomic clocks are opening new perspectives for the direct determination of geopotential differences between any two points at a centimeter-level accuracy in geoid height. However, so far detailed quantitative estimates of the possible improvement in geoid determination when adding such clock measurements to existing data are lacking. We present a first step in that direction with the aim and hope of triggering further work and efforts in this emerging field of chronometric geodesy and geophysics. We specifically focus on evaluating the contribution of this new kind of direct measurements in determining the geopotential at high spatial resolution (≈ 10 km). We studied two test areas, both located in France and corresponding to a middle (Massif Central) and high (Alps) mountainous terrain. These regions are interesting because the gravitational field strength varies greatly from place to place at high spatial resolution due to the complex topography. Our method consists in first generating a synthetic high-resolution geopotential map, then drawing synthetic measurement data (gravimetry and clock data) from it, and finally reconstructing the geopotential map from that data using least squares collocation. The quality of the reconstructed map is then assessed by comparing it to the original one used to generate the data. We show that adding only a few clock data points (less than 1% of the gravimetry data) reduces the bias significantly and improves the standard deviation by a factor 3. The effect of the data coverage and data quality on the results is investigated, and the trade-off between the measurement noise level and the number of data points is discussed.

  4. High performance liquid chromatography--atomic fluorescence spectrometric determination of arsenic species in beer samples

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, N.M.; Parrilla, Carmen; Cervera, M.L.; Pastor, A.; Guardia, M. de la

    2003-04-10

    A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation--atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH{sub 2}PO{sub 4}/K{sub 2}HPO{sub 4} as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 {mu}l, a 4.0% (m/v) solution of sodium tetrahydroborate and 2.0 mol l{sup -1} hydrochloric acid with flow rates of 2.7 and 1.7 ml min{sup -1}, respectively and a flow rate of 500 ml min{sup -1} for the argon carrier gas. Under the best experimental conditions, the detection limit was found to be 0.12, 0.20, 0.27 and 0.39 {mu}g l{sup -1} for As(III), DMA, MMA and As(V), respectively. The relative standard deviation for eight independent determinations varied from 3.9 till 8.9% for species considered at a concentration level of 10.0 {mu}g l{sup -1}. Recovery and comparative studies evidenced that the method is suitable for the accurate determination of arsenic species in water and beer samples.

  5. Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bruhn, C.G.; Huerta, V.N.; Neira, J.Y. [Departamento de Analisis Instrumental, Facultad de Farmacia, Universidad de Concepcion, P.O. Box 237, Concepcion (Chile)

    2004-01-01

    Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 {mu}g) and Rh (2.0 {mu}g) modifiers and in the digest solutions of the study matrices, Rh (2.0 {mu}g) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25-100 {mu}g L{sup -1}) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3{sigma}{sub blank}/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300-400 firings. Validation was by determination of As in the certified reference material (CRM) of ''Oyster tissue'' solution with a percentage relative error (E{sub rel}%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94{+-}8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h{sup -1}), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers. (orig.)

  6. Determination of a high spatial resolution geopotential model using atomic clock comparisons

    Science.gov (United States)

    Lion, G.; Panet, I.; Wolf, P.; Guerlin, C.; Bize, S.; Delva, P.

    2017-06-01

    Recent technological advances in optical atomic clocks are opening new perspectives for the direct determination of geopotential differences between any two points at a centimeter-level accuracy in geoid height. However, so far detailed quantitative estimates of the possible improvement in geoid determination when adding such clock measurements to existing data are lacking. We present a first step in that direction with the aim and hope of triggering further work and efforts in this emerging field of chronometric geodesy and geophysics. We specifically focus on evaluating the contribution of this new kind of direct measurements in determining the geopotential at high spatial resolution (≈ 10 km). We studied two test areas, both located in France and corresponding to a middle (Massif Central) and high (Alps) mountainous terrain. These regions are interesting because the gravitational field strength varies greatly from place to place at high spatial resolution due to the complex topography. Our method consists in first generating a synthetic high-resolution geopotential map, then drawing synthetic measurement data (gravimetry and clock data) from it, and finally reconstructing the geopotential map from that data using least squares collocation. The quality of the reconstructed map is then assessed by comparing it to the original one used to generate the data. We show that adding only a few clock data points (less than 1% of the gravimetry data) reduces the bias significantly and improves the standard deviation by a factor 3. The effect of the data coverage and data quality on the results is investigated, and the trade-off between the measurement noise level and the number of data points is discussed.

  7. [Study on determination of eight metal elements in Hainan arecanut leaf by flame atomic absorption spectrophotometry].

    Science.gov (United States)

    Liu, Li-yun; Wang, Ping; Feng, Mei-li; Dong, Zhi-guo; Li, Jie

    2008-12-01

    Arecanut is a sort of palm that is important economic crop for the farmers in Hainan province of China, wherein there are many kinds of metal elements such as K, Ca, Na, Mg, Fe, Mn, Cu, Zn etc. These elements are important nutrition for the growth of arecanut. It is very valuable to study on the content of these metal elements in arecanut leaf in terms of plant nutriology of arecanut. The arecanut leaf in Wangling county, Hainan province of China was sampled by diagonal-field-sampling method. Refering to other plant sample determination by FAAS, the detailed studies are done with different digestion and determination methods. In the present paper the effects of mixed acid of HNO3-HClO4 digestion method on determining the amount of metal elements in the arecanut leaf by FAAS is reported, and another one is incineration digestion method. FAAS method was established for the determination of K, Ca, Mg, Na, Fe, Mn, Cu and Zn The samples were incinerated or heated with HNO3-HClO4 (4:1). In the meantime, the optimum parameters of FAAS and effects of different digestion methods on the results were discussed. The recovery rate of standard addition is 98.36%-102.38% in the first method; RSD is 0.42%-2.328% (n=6); The recovery rate of standard addition is 99.22%-103.72% in the second method; RSD is 0.58%-1.283 (n=6). The metal amount determined by the first method is lower than the second method, the ratio is 0.9703-0.9934. The two methods are satisfied, but the latter is better. It is precise enough to common experiment to use flame atomic absorption spectrophotometry with digestion by incineration If the especially precise experiment is required, the digestion methods with mixed acid of HNO3-HClO4 may be introduced. The paper introduced methods dependable for determination of some metal elements in order to study on some nutrient effects of these metal elements in arecanut.

  8. The Proposal of Key Performance Indicators in Facility Management and Determination the Weights of Significance

    Science.gov (United States)

    Rimbalová, Jarmila; Vilčeková, Silvia

    2013-11-01

    The practice of facilities management is rapidly evolving with the increasing interest in the discourse of sustainable development. The industry and its market are forecasted to develop to include non-core functions, activities traditionally not associated with this profession, but which are increasingly being addressed by facilities managers. The scale of growth in the built environment and the consequential growth of the facility management sector is anticipated to be enormous. Key Performance Indicators (KPI) are measure that provides essential information about performance of facility services delivery. In selecting KPI, it is critical to limit them to those factors that are essential to the organization reaching its goals. It is also important to keep the number of KPI small just to keep everyone's attention focused on achieving the same KPIs. This paper deals with the determination of weights of KPI of FM in terms of the design and use of sustainable buildings.

  9. The criteria weight determination of factors impacting the melt flow index of degradable plastics using Lambda-Max method

    Science.gov (United States)

    Dom, Rosma Mohd; Saadon, Nurul Adzlyana; Mohamad, Daud

    2013-09-01

    Three common methods of determining criteria weights using the Analytic Hierarchy Process (AHP) are extent analysis, logarithmic least square method (LLSM) and Lambda-Max. Lambda-Max criteria weights determination method uses pair wise comparison of criteria considered. Studies have shown that Lambda-Max is a preferred criteria weight determination method since it involves lesser computation with consistent results of precise criteria weights generated. In this paper the criteria weights of four factors impacting the Melt Flow Index of degradable plastics are calculated using Lambda-Max method. The input factors (criteria) are the percentages by mass of polyethylene, oil palm biomass, palm olein and starch used in the formulation of degradable plastics. The criteria weights are calculated using Lambda-Max based on input given by four experts. The finding indicates the feasibility of using Lambda-Max method in criteria weight determination for determining the impact of four factors in the formulation of degradable plastics as reflected by the consistency control index value calculated.

  10. Determination of the weighted CT dose index in modern multi-detector CT scanners.

    Science.gov (United States)

    Perisinakis, K; Damilakis, J; Tzedakis, A; Papadakis, A; Theocharopoulos, N; Gourtsoyiannis, N

    2007-11-07

    The aim of the present study was to (a) evaluate the underestimation in the value of the free-in-air (CTDI(air)) and the weighted CT dose index (CTDI(w)) determined with the standard 100 mm pencil chamber, i.e. the CTDI(100) concept, for the whole range of nominal radiation beam collimations selectable in a modern multi-slice CT scanner, (b) estimate the optimum length of the pencil-chamber and phantoms for accurate CTDI(w) measurements and (c) provide CTDI(w) values normalized to free-in-air CTDI for different tube-voltage, nominal radiation beam collimations and beam filtration values. The underestimation in the determination of CTDI(air) and CTDI(w) using the CTDI(100) concept was determined from measurements obtained with standard polymethyl-methacrylate (PMMA) phantoms and arrays of thermoluminescence dosimeters. The Monte Carlo N-Particle transport code was used to simulate standard CTDI measurements on a 16-slice CT scanner. The optimum pencil-chamber length for accurate determination of CTDI(w) was estimated as the minimum chamber length for which a further increase in length does not alter the value of the CTDI. CTDI(w)/CTDI(air) ratios were determined using Monte Carlo simulation and the optimum detector length for all selectable tube-voltage values and for three different values of beam filtration. To verify the Monte Carlo results, measured values of CTDI(w)/CTDI(air) ratios using the standard 100 mm pencil ionization chamber were compared with corresponding values calculated with Monte Carlo experiments. The underestimation in the determination of CTDI(air) using the 100 mm pencil chamber was less than 1% for all beam collimations. The underestimation in CTDI(w) was 15% and 27% for head and body phantoms, respectively. The optimum detector length for accurate CTDI(w) measurements was found to be 50 cm for the beam collimations commonly employed in modern multi-detector (MD) CT scanners. The ratio of CTDI(w)/CTDI(air) determined using the optimum

  11. Comparison of simple additive weighting (SAW) and composite performance index (CPI) methods in employee remuneration determination

    Science.gov (United States)

    Karlitasari, L.; Suhartini, D.; Benny

    2017-01-01

    The process of determining the employee remuneration for PT Sepatu Mas Idaman currently are still using Microsoft Excel-based spreadsheet where in the spreadsheet there is the value of criterias that must be calculated for every employee. This can give the effect of doubt during the assesment process, therefore resulting in the process to take much longer time. The process of employee remuneration determination is conducted by the assesment team based on some criterias that have been predetermined. The criteria used in the assessment process are namely the ability to work, human relations, job responsibility, discipline, creativity, work, achievement of targets, and absence. To ease the determination of employee remuneration to be more efficient and effective, the Simple Additive Weighting (SAW) method is used. SAW method can help in decision making for a certain case, and the calculation that generates the greatest value will be chosen as the best alternative. Other than SAW, also by using another method was the CPI method which is one of the calculating method in decision making based on performance index. Where SAW method was more faster by 89-93% compared to CPI method. Therefore it is expected that this application can be an evaluation material for the need of training and development for employee performances to be more optimal.

  12. Intramuscular adipose tissue determined by T1-weighted MRI at 3T primarily reflects extramyocellular lipids.

    Science.gov (United States)

    Akima, Hiroshi; Hioki, Maya; Yoshiko, Akito; Koike, Teruhiko; Sakakibara, Hisataka; Takahashi, Hideyuki; Oshida, Yoshiharu

    2016-05-01

    The purpose of this study was to assess relationships between intramuscular adipose tissue (IntraMAT) content determined by MRI and intramyocellular lipids (IMCL) and extramyocellular lipids (EMCL) determined by (1)H magnetic resonance spectroscopy ((1)H MRS) or echo intensity determined by B-mode ultrasonography of human skeletal muscles. Thirty young and elderly men and women were included. T1-weighted MRI was taken from the right mid-thigh to measure IntraMAT content of the vastus lateralis (VL) and biceps femoris (BF) using a histogram shape-based thresholding technique. IMCL and EMCL were measured from the VL and BF at the right mid-thigh using (1)H MRS. Ultrasonographic images were taken from the VL and BF of the right mid-thigh to measure echo intensity based on gray-scale level for quantitative analysis. There was a significant correlation between IntraMAT content by MRI and EMCL of the VL and BF (VL, r=0.506, Plipids, not intramyocellular lipids, in human skeletal muscles. Copyright © 2016 Elsevier Inc. All rights reserved.

  13. Determinants of survival in very low birth weight neonates in a public sector hospital in Johannesburg

    Directory of Open Access Journals (Sweden)

    Cooper Peter A

    2010-05-01

    Full Text Available Abstract Background Audit of disease and mortality patterns provides essential information for health budgeting and planning, as well as a benchmark for comparison. Neonatal mortality accounts for about 1/3 of deaths Methods This was a retrospective chart review of 474 VLBW infants admitted within 24 hours of birth, between 1 July 2006 and 30 June 2007, to the neonatal unit of Charlotte Maxeke Johannesburg Academic Hospital (CMJAH in Johannesburg, South Africa. Binary outcome logistic regression on individual variables and multiple logistic regression was done to identify those factors determining survival. Results Overall survival was 70.5%. Survival of infants below 1001 grams birth weight was 34.9% compared to 85.8% for those between 1001 and 1500 grams at birth. The main determinant of survival was birth weight with an adjusted survival odds ratio of 23.44 (95% CI: 11.22 - 49.00 for babies weighing between 1001 and 1500 grams compared to those weighing below 1001 grams. Other predictors of survival were gender (OR 3. 21; 95% CI 1.6 - 6.3, birth before arrival at the hospital (BBA (OR 0.23; 95% CI: 0.08 - 0.69, necrotising enterocolitis (NEC (OR 0.06; 95% CI: 0.02 - 0.20, hypotension (OR 0.05; 95% CI 0.01 - 0.21 and nasal continuous positive airways pressure (NCPAP (OR 4.58; 95% CI 1.58 - 13.31. Conclusions Survival rates compare favourably with other developing countries, but can be improved; especially in infants

  14. Spatial and temporal behavior of atomic oxygen determined by Ogo 6 airglow observations

    Science.gov (United States)

    Donahue, T. M.; Guenther, B.; Thomas, R. J.

    1974-01-01

    Maps are produced of the atomic oxygen density near 97 km showing a strong variation in latitude, longitude, universal time, and time of year. These densities are deduced from atomic oxygen green nightglow observations carried out from Ogo 6. Meridional wind patterns needed to support the asymmetries observed in local oxygen production and loss rates are deduced.

  15. Determination of Aluminum Concentration in Seawater by Colorimetry and Atomic Absorption Spectroscopy.

    Science.gov (United States)

    1972-11-30

    this was also high. 5 . ,Irj ~ - • lri*; llo. TALLE 2 ATOMIC ABSORPTION SPECTROSCOPY DETEPIJINATION OF ALUMINU1 CONCENTRATIO11 OF SEAWATER OCEAN...Concentration in Seawater by Colorimetr-y and Atomic Absorption Spectroscopy Charles A. Greene, Jr. and Everett N. Jones Ocean Science Department T14

  16. [Determination of chlorine in gasoline by inductively coupled plasma atomic emission spectrometry].

    Science.gov (United States)

    Zhao, Yan; Chen, Xiao-yan; Xu, Dong-yu; Zhang, Shi-yuan; Chen, Ze-yong

    2014-12-01

    A new method was studied for the analysis of chlorine in gasoline by inductively coupled plasma atomic emission spectrometry (ICP-AES). Samples werediluted 1+4(φ) with kerosene. The intense spectral line for chlorine (134.724 nm) was used. In order to eliminate carbon and maintain stable plasma, small amounts of oxygen (0.050 L · min(-1)) were added to the auxiliary gas. The instrumental main condition was optimized in terms of effects of generator power, nebulizer gas flow, auxiliary gas flow, and oxygen flow on SBR for chlorine. Standard addition method was used to compensate matrix effect and signal drift. The recovery for spiking gasoline samples and the limit of detection were in the range of 96.6%~103.9% and 0.27 mg · L(-1) respectively. The relative standard deviation (RSD) was between 1.57% and 4.49%. Compared with microcoulometry, the analysis results of organic chlorine were basically the same. Moreover, chlorine content, including organic chlorine and inorganic chloride was determined by ICP-AES. The proposed method had the advantages of simplicity, speediness and sensitivity, and expanded the ICP-AES application in non-metals especially halogen elements. It can be used for the analysis of chlorine in gasoline and provides technical support for quality evaluation.

  17. Determination of the Elastic Properties of Tomato Fruit Cells with an Atomic Force Microscope

    Directory of Open Access Journals (Sweden)

    Andrzej Kurenda

    2013-09-01

    Full Text Available Since the mechanical properties of single cells together with the intercellular adhesive properties determine the macro-mechanical properties of plants, a method for evaluation of the cell elastic properties is needed to help explanation of the behavior of fruits and vegetables in handling and food processing. For this purpose, indentation of tomato mesocarp cells with an atomic force microscope was used. The Young’s modulus of a cell using the Hertz and Sneddon models, and stiffness were calculated from force-indentation curves. Use of two probes of distinct radius of curvature (20 nm and 10,000 nm showed that the measured elastic properties were significantly affected by tip geometry. The Young’s modulus was about 100 kPa ± 35 kPa and 20 kPa ± 14 kPa for the sharper tip and a bead tip, respectively. Moreover, large variability regarding elastic properties (>100% among cells sampled from the same region in the fruit was observed. We showed that AFM provides the possibility of combining nano-mechanical properties with topography imaging, which could be very useful for the study of structure-related properties of fruits and vegetables at the cellular and sub-cellular scale.

  18. [Determination of trace elements in new food sources by flame atomic absorption spectrophotometry].

    Science.gov (United States)

    Liu, Li E; Ding, Li; Qi, Min; Han, Xiu Li; Zhang, Hong-Quan

    2007-07-01

    Samples were digested by HNO3 + HClO4. Flame atomic absorption spectrophotometry (FAAS) was successfully used to determine copper, zinc and iron in new resource food. Under our experimental conditions, the recovery ratio was 94.66%-108.80%; the precision was 0.71%-4.78%. This method of measuring elements is convenient, rapid and accurate. The results showed that there are profitable elements, such as copper, zinc and iron in new resourse food in Henan province. By F test and SNK test, the content sequence of metal elements was found as follows: copper, Chrysanthemum morifolium Ramat = Silkworm pupa > flowers of Pueraria lobata Ohwin = Wheat germ = Codonopsis lanceolata = roots of Pueraria lobata Ohwi > Opuntia dillenii Haw. Zinc, Opuntia dillenii Haw > Silkworm pupa = flowers of Pueraria lobata Ohwi = roots of Pueraria lobata Ohwi = Wheat germ = Codonopsis lanceolata = Chrysanthemum morifolium Ramat. Iron, Silkworm pupa = C hrysanthemum morifolium Ramat = roots of Pueraria lobata Ohwi > flowers of Pueraria lobata Ohwi = Wheat germ = Codonopis lanceolata = Opuntia dillenii Haw.

  19. Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Maria Jose da [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Paim, Ana Paula S. [Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Pimentel, Maria Fernanda [Departamento de Engenharia Quimica, Universidade Federal de Pernambuco, Recife, PE (Brazil); Cervera, M. Luisa, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Guardia, Miguel de la [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain)

    2010-05-14

    A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g{sup -1} concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO{sub 3} and H{sub 2}O{sub 2} followed by dilution with water containing KBr/KBrO{sub 3} and hydroxylamine and reduction with SnCl{sub 2} in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g{sup -1} with a recovery percentage of 95 {+-} 4% at an added concentration of 5 ng g{sup -1}. The concentration level of Hg found in 24 natural rice samples from different origin ranged between 1.3 and 7.8 ng g{sup -1}.

  20. Determination of additives in PVC material by UV laser ablation inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Hemmerlin, M.; Mermet, J. M.; Bertucci, M.; Zydowicz, P.

    1997-04-01

    UV laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES) has been applied to the direct determination of additives in solid poly(vinyl chloride) materials. A Nd:YAG laser, operating at its fourth harmonic (266 nm), was used with a beam masking device, in the most reproducible conditions, to introduce solid particles into the plasma torch of a simultaneous ICP-AES system. Emphasis was placed on both precision and accuracy in the analysis of PVC materials by LA-ICP-AES. A series of six in-house PVC reference materials was prepared by incorporating several additives in increasing concentrations. Three alternative methods were evaluated to certify the amount of incorporated elements: ICP-AES with sample dissolution, NAA and XRF. Satisfactory results and good agreement were obtained for seven elements (Al, Ca, Cd, Mg, Sb, Sn and Ti) among the ten incorporated. Sample homogeneity appeared to be satisfactory, and calibration graphs obtained by LA-ICP-AES for several elements are presented. Finally, the performance of the technique in terms of repeatability (1.6-5%), reproducibility (2-5%), and limits of detection was investigated.

  1. Determination of calcium and magnesium in hydroethanolic extracts of propolis by atomic absorption flame spectrophotometry

    Directory of Open Access Journals (Sweden)

    E. Q. SANTANA

    2009-01-01

    Full Text Available

    Propolis is a natural product collected by honeybees and has a large range of pharmacological activity, including antimicrobial, antitumoral, antioxidant and anti-inflammatory. Its use as a popular medicine is increasing all over the world, creating a need for quality control of the commercial products. In this study the levels of calcium and magnesium in commercial hydroalcoholic propolis extracts from varios states of Brazil were determined by atomic absorption flame spectrophotometry and different values were obtained for northern and southern states. This study can be extended to the analysis of metals that are harmful to health. The results showed that the calibration curves were linear over a wide concentration range (0.5-4.0 µg.mL-1 for calcium and 0.05-0.4 µg.mL-1 for magnesium with good correlation coefficients (0.999 and 0.988, respectively. Good analytical recovery (94% was obtained. The proposed method showed adequate precision and relative standard deviation lower than 2 %. The method is accurate and precise as well as having advantages such as simplicity and speed. Keywords: hydroalcoholic propolis extract; mineralization; analysis; calcium; magnesium.

  2. Determination of arsenic in a nickel alloy by flow injection hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Hanna, C. P.; Tyson, J. F.; Offley, S. G.

    1992-08-01

    The development of a method for the direct determination of trace arsenic quantities in nickel alloy digests, by flow injection hydride generation atomic absorption spectrometry, is described. An optimization study of the manifold and chemical parameters produced system performance, in terms of tolerance of the nickel matrix and sensitivity, such that matrix removal and pre-reduction of As(V) to As (III) prior to arsine generation were eliminated. Full recovery of the As(V) signal from a solution containing 5 ng ml -1 in the presence of 60 μg ml -1 nickel was obtained. Validation of the method was achieved by analyzing a British Chemical Standard (BCS) Certified Reference Material (CRM) #346 IN nickel alloy containing arsenic at a concentration of 50 μg g -1. Following dissolution in nitric and hydrofluoric acids by a microwave assisted procedure, the only subsequent preparation required was dilution by the appropriate factor. Up to 60 injections h -1 may be made, with a detection limit of 0.5 ng ml -1 arsenic (250 pg absolute) as As(V) in a 500 μl sample. The peak height characteristic concentration is 0.46 ng ml -1, with a relative standard deviation of 3.5% for a 10 ng ml -1 As(V) standard ( n = 6).

  3. [Determination of thirteen metal elements in the plant Foeniculum vulgare Mill. by flame atomic absorption spectrophotometry].

    Science.gov (United States)

    Xue, Guo-qing; Liu, Qing; Han, Yu-qi; Wei, Hui-guang; Dong, Ting

    2006-10-01

    The objective of the paper is to determine the amount of metal elements of Na, K, Mg, Ca, Cu, Zn, Mn, Fe, Co, Ni, Cd, Cr and Pb in the planted Foeniculum vulgare Mill. by flame atomic absorption spectrophotometry (FAAS), after the cinefaction and the digestion with HNO3-HClO4 (phi 4:1) at 90-95 degrees C and normal pressure. The optimum parameters of FAAS and the effects of solution medium on the results were investigated. The analytical results show that the amount of Na, K, Mg, Ca, Mn, Fe, Cu, Zn and Pb was 1508.7, 27653.0, 2036.0, 4848.1, 24.8, 323.5, 15.2, 23.7 and 10.8 microg x g(-1), respectively, and that of Co, Ni, Cd and Cr was not checked out in the samples. The recovery of standard addition is 97.45%-102.50%, the relative standard deviation (n=9) was 0.34%-2.77%. The characteristic method is quick, simple and convenient and the results are satisfactory.

  4. Ion-exchange preconcentration and determination of vanadium in milk samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    López-García, Ignacio; Viñas, Pilar; Romero-Romero, Rafael; Hernández-Córdoba, Manuel

    2009-06-15

    A new method for the electrothermal atomic absorption spectrometric determination of vanadium in milk and infant formulas using suspensions to avoid the need for previous dissolution of samples is described. Sensitivity is improved by a procedure based on preconcentration and removal of the matrix, using ion-exchange (Dowex 1X8-100). Suspensions of 15% (m/v) infant formula samples were prepared in a medium containing 0.05M sodium citrate (pH 7.2) and passed through the ion exchange column. Vanadium was eluted from the column using 1M hydrochloric acid and injected in the graphite furnace using a mixture of hydrofluoric acid plus magnesium nitrate as chemical modifiers. Calibration was carried out using multiple injection and aqueous standards prepared in the same medium. Detection limits were 0.2 ng g(-1) for infant formulas and 0.02 microg L(-1) for cow milk samples. The reliability of the procedure was checked by comparing the results obtained with those found using a previous mineralization stage and by analyzing five certified reference materials.

  5. Separate determination of the amplitude of thermal vibrations and static atomic displacements in titanium carbide by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Khidirov, I., E-mail: khidirov@inp.uz; Parpiev, A. S. [Uzbekistan Academy of Sciences, Institute of Nuclear Physics (Uzbekistan)

    2011-05-15

    The amplitude of thermal (dynamic) atomic vibrations and meansquare static atomic displacements in titanium carbide TiC{sub x} (x = 0.97, 0.88, 0.70) have been separately determined by measuring neutron diffraction patterns at two temperatures (T{sub 1} = 300 K and T{sub 2} = 80 K). The static lattice distortions in stoichiometric titanium carbide are experimentally found to be negligible. In the TiC{sub x} homogeneity range, the amplitude {radical}u{sup 2}{sub dyn} of thermal atomic vibrations significantly increases with a decrease in the carbon concentration. The Debye temperature has been determined for the first time in the TiC{sub x} homogeneity range at both room and liquid-nitrogen temperatures.

  6. Determination of effective atomic numbers, effective electrons numbers, total atomic cross-sections and buildup factor of some compounds for different radiation sources

    Science.gov (United States)

    Levet, A.; Özdemir, Y.

    2017-01-01

    The photon interaction parameters such as mass attenuation coefficient, effective atomic number, effective electron density, buildup factor have been measured for Fe(NO3)3, V4O2, NaCO3·H2O, C6H5FeO7·H2O and CuCI compounds using 137Ba, 157Gd and 241Am γ-rays sources in stable geometry. The mass attenuation coefficients have been determined experimentally via Energy Dispersive X-ray Fluorescence Spectroscopy (EDXRF) system and theoretically by using WinXCom computer program. Then, effective atomic numbers, Zeff, and electron densities, Neff, have been calculated by using the mass attenuation coefficients. The obtained values of effective atomic numbers have been compared with the ones calculated according to a different approach proposed by Hine and the calculated ones from theory. Also, photon buildup factors were obtained by changing collimator diameters in the different photon energies. We observed that the buildup factor increased as the collimator diameter increased for all sources used.

  7. Comparisons of selected methods for the determination of kinetic parameters from electrothermal atomic absorption data

    Science.gov (United States)

    Fonseca, Rodney W.; Pfefferkorn, Lisa L.; Holcombe, James A.

    1994-12-01

    Three of the methods available for the determination of kinetic parameters for atom formation in ETAAS were compared. In the approach of mcnally and holcombe [ Anal. Chem. 59, 1015 (1987)], Arrhenius-type plots are used to extract activation energy values while an approximation of the order of release is obtained by studying the alignment of the absorption maxima at increasing analyte concentrations. In the method of rojas and olivares [ Spectrochim. Acta47B, 387 (1992)], plots are prepared for different orders of release, with the correct order yielding a longer linear region from whose slope the activation energy is calculated. The method of yan et al. [ Spectrochim. Acta48B, 605 (1993)] uses a single absorption profile for the calculations. Activation energy and the order of release are obtained from the slope and intercept, respectively, on their graph. All three methods assume linear heating rate, constant activation energies, and furnace isothermality. The methods were tested with the same experimental data sets for Cu, Au and Ni using a spatially isothermal cuvette. Since intensive mathematical treatments commonly have deleterious effects on the uncertainty of the final result, the methods were compared using both the original data and a smoothed version of it. In general, the three methods yielded comparable results for the metals studied. However, choosing the most linear plot to determine the correct order of release when using Rojas and Olivares' method was sometimes subjective, and McNally and Holcombe's method provided only estimates for the orders of release that were neither zero nor unity.

  8. Atomic absorption techniques for determining vanadium and nickel in crude oil

    Energy Technology Data Exchange (ETDEWEB)

    Grizzle, P.L.; Wilson, C.A.; Ferrero, E.P.; Coleman, H.J.

    1977-05-01

    Four different techniques for sample preparation were evaluated for determining vanadium and nickel in crude oils by atomic absorption (AA) spectroscopy: (1) The flame-analyzed dilution method which consists of direct-flame AA analysis after diluting the sample with a suitable organic solvent; (2) the flame-analyzed, wet-ashing method in which the sample is combusted and the residue is then dissolved before flame analysis; (3) the flameless, dilution method which involves flameless AA analysis of the sample following dilution with a suitable organic solvent; and (4) the direct, flameless method in which the crude oil or residue is directly analyzed by flameless AA. The flame-analyzed dilution method yielded erratic and inaccurate analytical results for samples of crude oils as well as for a residual sample containing standard amounts of vanadium and nickel; hence, it is unsatisfactory for oil-identification. Similarly, the direct, flameless method is unsatisfactory owing to the small concentration range available for analysis (less than approximately 15 ppM). Both the flame-analyzed, wet-ashing and flameless-dilution methods yield reliable and reproducible (better than 10%) quantitative data for nickel and vanadium in crude oils and crude oil residues. Results demonstrate that the error associated with the loss of volatile metal containing compounds upon wet-ashing is within the reproducibility of the technique. Although wet-ashing may be slightly more reproducible, the flameless-dilution method is much simpler and faster and is recommended as the better of the two procedures for routine determinations of trace metals for oil identification.

  9. [Determination of Trace Germanium in Plant Samples by Dry Ashing-Atomic Fluorescence Spectrometry].

    Science.gov (United States)

    Chen, Hai-jie; Yu, Zhao-shui; Bai, Jin-feng; Li, Qing-xia; Liu, Ya-xuan; Bo, Wei; Zhang, Qin

    2015-04-01

    To reduce the limit of detection (LOD) and allow the accurate determination of Ge, a dry ashing method was performed to enrich the Ge in plant samples. A method for the determination.of trace Ge in plant samples by HG-AFS was established. Study of the effect of temperature on the ashing of plant samples showed that no volatile loss of Ge occurred even at 900 °C. Additional experiments indicated that a 4 h burning process at 600 °C would be sufficient to fully ash the plant samples. Various digestion methods (involving nitric acid, hydrofluoric acid, and sulfuric acid digestion methods) for ashed samples were investigated. High-temperature ashing with large sample weights was used, which could reduce the reagent doses and the method's LOD effectively and simultaneously, the precision of the method was improved. The method's LOD was 0.27 ng · g(-1), and the relative standard deviation was 3.99%-6.81%. Verified with national biological reference materials (grade I), the proposed method was accurate and reliable.

  10. Weighted least-squares solver for determining pressure from particle image velocimetry data

    Science.gov (United States)

    de Kat, Roeland

    2016-11-01

    Currently, most approaches to determine pressure from particle image velocimetry data are Poisson approaches (e.g.) or multi-pass marching approaches (e.g.). However, these approaches deal with boundary conditions in their specific ways which cannot easily be changed-Poisson approaches enforce boundary conditions strongly, whereas multi-pass marching approaches enforce them weakly. Under certain conditions (depending on the certainty of the data or availability of reference data along the boundary) both types of boundary condition enforcement have to be used together to obtain the best result. In addition, neither of the approaches takes the certainty of the particle image velocimetry data (see e.g.) within the domain into account. Therefore, to address these shortcomings and improve upon current approaches, a new approach is proposed using weighted least-squares. The performance of this new approach is tested on synthetic and experimental particle image velocimetry data. Preliminary results show that a significant improvement can be made in determining pressure fields using the new approach. RdK is supported by a Leverhulme Trust Early Career Fellowship.

  11. Socio-economic and nutritional determinants of low birth weight in India

    Directory of Open Access Journals (Sweden)

    Manzur Kader

    2014-01-01

    Full Text Available Background: Low birth weight (LBW is an important risk factor for childhood morbidity and mortality, consequently an important public health concern. Aim: This study aims to identify significant socio-economic and nutritional determinants associated with LBW in India. Materials and Methods: Data from 2005 to 2006 National Family Health Survey-3 (NFHS-3 of India was analyzed. A total of 20,946 women (15-49 years who gave birth at least once 5 years preceding the NFHS-3 were included in this study. Infant′s LBW (<2500 grams as outcome variable was examined in association with all independent predictors as infant′s sex, maternal household wealth status, caste, age, education, body mass index (BMI, stature, anemia level, parity, inter-pregnancy interval, antenatal care received, and living place. Results: Almost 20% of the infants were born with LBW. Mother′s low education level, BMI <18.5, short stature (height <145 centimeters and lack of antenatal visits (<4 visits were significant predictors of LBW. Male gender has a protective effect against LBW. Conclusion: Maternal education, nutritional status and antenatal care received are key determinants that need to be addressed to reduce prevalence of LBW in India. Continue implementation of multifaceted health promotion interventions are needed to address these factors effectively.

  12. Direct atomic absorption determination of cadmium and lead in strongly interfering matrices by double vaporization with a two-step electrothermal atomizer

    Science.gov (United States)

    Grinshtein, Ilia L.; Vilpan, Yuri A.; Saraev, Alexei V.; Vasilieva, Lubov A.

    2001-03-01

    Thermal pretreatment of a sample using double vaporization in a two-step atomizer with a purged vaporizer makes possible the direct analysis of samples with strongly interfering matrices including solids. A porous-graphite capsule or a filter inserted into the vaporizer is used for solid sample analysis. The technique was used for the direct determination of Cd and Pb in human urine, potatoes, wheat, bovine liver, milk powder, grass-cereal mixtures, caprolactam, bituminous-shale and polyvinyl chloride plastic without chemical modification or any other sample pretreatment.

  13. C12/C13-ratio determination in nanodiamonds by atom-probe tomography.

    Science.gov (United States)

    Lewis, Josiah B; Isheim, Dieter; Floss, Christine; Seidman, David N

    2015-12-01

    The astrophysical origins of ∼ 3 nm-diameter meteoritic nanodiamonds can be inferred from the ratio of C12/C13. It is essential to achieve high spatial and mass resolving power and minimize all sources of signal loss in order to obtain statistically significant measurements. We conducted atom-probe tomography on meteoritic nanodiamonds embedded between layers of Pt. We describe sample preparation, atom-probe tomography analysis, 3D reconstruction, and bias correction. We present new data from meteoritic nanodiamonds and terrestrial standards and discuss methods to correct isotopic measurements made with the atom-probe tomograph.

  14. Influence of matrix effects on determination of the trace element content in zirconium by the atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    A.N. Kulik

    2009-01-01

    Full Text Available The influence of sample matrix prepared on the basis of hydrofluoric acid on the measured content of trace elements in zirconium was studied. The accuracy of determination of the trace element content was verified by the “introduced-found” method. Based on verification results the temperature regime of electrothermal atomizer was optimized.

  15. Influence of phosphorus and calcium on flame atomic absorption spectrophotometric determination of lead in canned fish products.

    Science.gov (United States)

    Serra, T M; Serrano, J F

    1984-01-01

    Lead was determined in the presence of whole multiples of the P/Ca ratio found in Portuguese canned fish by flame atomic absorption spectrophotometry with and without using an ashing aid. Under our experimental conditions, use of the ashing aid eliminates P and Ca interference. Results with real samples, spiked with 1, 2, 3, and 4 ppm lead, are presented and statistically treated.

  16. Determination of nickel by flame atomic-absorption spectrophotometry after separation by adsorption of its nioxime complex on microcrystalline naphthalene.

    Science.gov (United States)

    Nagahiro, T; Puri, B K; Katyal, M; Satake, M

    1984-11-01

    A method has been developed for the determination of nickel in alloys by flame atomic-absorption spectrophotometry after formation of a water-insoluble complex, its adsorption on microcrystalline naphthalene, and dissolution of the complex and naphthalene in nitric acid and xylene.

  17. A COMPARISON OF A SPECTROPHOTOMETRIC (QUERCETIN) METHOD AND AN ATOMIC-ABSORPTION METHOD FOR DETERMINATION OF TIN IN FOOD

    DEFF Research Database (Denmark)

    Engberg, Å

    1973-01-01

    Procedures for the determination of tin in food, which involve a spectrophotometric method (with the quercetin-tin complex) and an atomic-absorption method, are described. The precision of the complete methods and of the individual analytical steps required is evaluated, and the parameters...

  18. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    Science.gov (United States)

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  19. Child weight growth trajectory and its determinants in a sample of Iranian children from birth until 2 years of age

    Directory of Open Access Journals (Sweden)

    Sayed-Mohsen Hosseini

    2014-01-01

    Full Text Available Background: Growth is one of the most important indices in child health. The best and most effective way to investigate child health is measuring the physical growth indices such as weight, height and head circumference. Among these measures, weight growth is the simplest and the most effective way to determine child growth status. Weight trend at a given age is the result of cumulative growth experience, whereas growth velocity represents what is happening at the time. Methods: This longitudinal study was conducted among 606 children repeatedly measured from birth until 2 years of age. We used linear mixed model to analyze repeated measures and to determine factors affecting the growth trajectory. LOWESS smooth curve was used to draw velocity curves. Results: Gender, child rank, birth status and feeding mode had a significant effect on weight trajectory. Boys had higher weight during the study. Infants with exclusive breast feeding had higher weight than other infants. Boys had higher growth velocity up to age 6 month. Breast fed infants had higher growth velocity up to 6 month, but thereafter the velocity was higher in other infants. Conclusions: Many of the studies have investigated child growth, but most of them used cross-sectional design. In this study, we used longitudinal method to determine effective factors on weight trend in children from birth until 2-year-old. The effects of perinatal factors on further growth should be considered for prevention of growth disorders and their late complications.

  20. Correlates of antenatal body mass index (bmi as a determinant of birth weight – a longitudinal study

    Directory of Open Access Journals (Sweden)

    Saurabh Rambiharilal Shrivastava

    2012-09-01

    Full Text Available Objectives: To study the correlation between Body Mass Index (BMI in antenatal period and birth weight of child, along with the socio-demographic determinants of birth weight. Methods: A longitudinal study of one-year duration, from June 2010 to May 2011, was conducted in an urban slum of Mumbai, India. Universal sampling method was employed, including as subjects all pregnant women with minimum two Antenatal Care (ANC visits - and at least one in the third trimester - registered at an urban health centre from June to August 2010. Subjects with any pre-existing co-morbid illness or with past history of giving birth to twins or to any congenitally malformed child, or else, with outcome of still births or home delivery, were excluded. These women were followed up for the next months until delivery. Maternal weight was recorded at each visit and BMI was calculated, or the average BMI, in case of more than one visit in any trimester. Birth weight was recorded using hospital or maternity home records. Results: Prevalence of low birth weight was 26.7%. Correlation between maternal BMI of third trimester and neonatal birth weight was moderately positive. 60.8% of variability in birth weight can be predicted by maternal BMI in third trimester. Conclusions: Third trimester BMI can be used as a predictor of neonatal birth weight. Information, Education and Counseling (IEC activities regarding utilization of Antenatal Care (ANC services can help reducing the incidence of Low Birth Weight (LBW.

  1. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  2. Determination of urinary manganese by the direct chelation-extraction method and flameless atomic absorption spectrophotometry.

    Science.gov (United States)

    Watanabe, T; Tokunaga, R; Iwahana, T; Tati, M; Ikeda, M

    1978-01-01

    The direct chelation-extraction method, originally developed by Hessel (1968) for blood lead analysis, has been successfully applied to urinalysis for manganese. The analyses of 35 urine samples containing up to 100 microgram/1 of manganese from manganese-exposed workers showed that the data obtained by this method agree well with those by wet digestion-flame atomic absorption spectrophotometry and also by flameless atomic absorption spectrophotometry. PMID:629893

  3. Determination of cadmium and lead in edible oils by electrothermal atomic absorption spectrometry after reverse dispersive liquid-liquid microextraction.

    Science.gov (United States)

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2014-06-01

    The dispersive liquid-liquid microextraction of edible oils with a low volume of an acidic solution in the presence of isopropyl alcohol allows cadmium and lead to be completely separated into the aqueous phase. After centrifugation, the metals are determined by electrothermal atomization atomic absorption spectrometry using a palladium salt for chemical modification in the heating cycle. Using a 10 g oil sample, the enrichment factor is 140, which permits detection limits of 0.6 and 10 ng kg(-1) for cadmium and lead, respectively. The results agree with those obtained after sample mineralization. Data for the cadmium and lead levels for 15 samples of different characteristics are given.

  4. Determination of cadmium in rice and water by tungsten coil electrothermal vaporization-atomic fluorescence spectrometry and tungsten coil electrothermal atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wen Xiaodong [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Wu Peng [Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Chen Li [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Hou Xiandeng, E-mail: houxd@scu.edu.cn [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China)

    2009-09-14

    In this work, the microsampling nature of tungsten coil electrothermal vaporization Ar/H{sub 2} flame atomic fluorescence spectrometry (W-coil ETV-AFS) as well as tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) was used with cloud point extraction (CPE) for the ultrasensitive determination of cadmium in rice and water samples. When the temperature of the extraction system is higher than the cloud point temperature of the selected surfactant Triton X-114, the complex of cadmium with dithizone can be quantitatively extracted into the surfactant-rich phase and subsequently separated from the bulk aqueous phase by centrifugation. The main factors affecting the CPE, such as concentration of Triton X-114 and dithizone, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimal conditions, the limits of detection for cadmium by W-coil ETV-AFS and W-coil ET-AAS were 0.01 and 0.03 {mu}g L{sup -1}, with sensitivity enhancement factors of 152 and 93, respectively. The proposed methods were applied to the determination of cadmium in certified reference rice and water samples with analytical results in good agreement with certified values.

  5. Ecological, historical and evolutionary determinants of modularity in weighted seed-dispersal networks

    DEFF Research Database (Denmark)

    Schleuning, Matthias; Ingmann, Lili; Strauß, Rouven

    2014-01-01

    algorithm to detect modularity in weighted bipartite networks in a global analysis of avian seed-dispersal networks. We define roles of species, such as connector values, for weighted and binary networks and associate them with avian species traits and phylogeny. The weighted, but not binary, analysis...... demonstrates the dominating impact of ecological factors on the structure of seed-dispersal networks, but also underscores the relevance of evolutionary history in shaping species roles in ecological communities....

  6. Laser-Excited Atomic Fluorescence and Ionization in a Graphite Furnace for the Determination of Metals and Nonmetals

    Science.gov (United States)

    Butcher, David James

    1990-01-01

    Here is reported novel instrumentation for atomic spectrometry that combined the use of a pulsed laser system as the light source and an electrothermal atomizer as the atom cell. The main goal of the research was to develop instrumentation that was more sensitive for elemental analysis than commercially available instruments and could be used to determine elements in real sample matrices. Laser excited atomic fluorescence spectrometry (LEAFS) in an electrothermal atomizer (ETA) was compared to ETA atomic absorption spectrometry (AAS) for the determination of thallium, manganese, and lead in food and agricultural standard reference materials (SRMs). Compared to ETA AAS, ETA LEAFS has a longer linear dynamic range (LDR) (5-7 orders of magnitude compared to 2-3 orders of magnitude) and higher sensitivity (10 ^{-16} to 10^{ -14} g as compared to 10^{ -13} to 10^{-11} g). Consequently, ETA LEAFS allows elemental analysis to be done over a wider range of concentrations with less dilution steps. Thallium was accurately determined in biological samples by ETA LEAFS at amounts five to one hundred times below the ETA AAS detection limit. ETA AAS and ETA LEAFS were compared for the determination of lead and manganese, and in general, the accuracies and precisions of ETA AAS were the same, with typical precisions between 3% and 6%. Fluorine was determined using laser excited molecular fluorescence spectrometry (LEMOFS) in an ETA. Molecular fluorescence from magnesium fluoride was collected, and the detection limit of 0.3 pg fluorine was two to six orders of magnitude more sensitive than other methods commonly used for the determination of fluorine. Significant interferences from ions were observed, but the sensitivity was high enough that fluorine could be determined in freeze dried urine SRMs by diluting the samples by a factor of one hundred to remove the interferences. Laser enhanced ionization (LEI) in an ETA was used for the determination of metals. For thallium, indium

  7. Hazards Forecasting and Weights Determination during Operation and Maintenance of Petrol Fuel Station

    Directory of Open Access Journals (Sweden)

    M.M. Ahmed

    2013-06-01

    Full Text Available Petrol Fuel Stations (PFS is the most commonly available hazardous facility within urban and rural areas. Hazardous materials such as petrol, diesel, Compressed Natural Gas (CNG and kerosene oil normally sell and stores at PFS. PFS can be considered as small refinery within the city. A 3.5 year study conducted and 3216 non-compliances were recorded from PFS located in various cities of Pakistan. The operating company was ISO 14001 and OHSAS 18001 certified. The recorded non-compliances during study period were categorized into 8 potential factors. These were Housekeeping (HK, Transportation Hazard (TH, Slips, Trips and Falls (STF, Carelessness (C, Fire Risks (FR, Electrical Fault (EF, Miscellaneous Cases (MC and Medical Treatment Cases (MTC. Analytical Hierarchy Process (AHP was used and categorized 8 factors were prioritized. The same data was further classified based upon to cause fatality, accident, incident and near miss cases. A total numbers of 14, 426, 975 and 1804, fatality, accident, incident and near miss cases were recorded. With application of Exponential Smoothing method the fatalities, accident, incident and near miss cases for the years 2011, 2012 and 2013 were forecasted. The results of AHP and forecasted hazards will be presented and discussed in this study. It is hope that the both approaches will assist health and safety professionals for future hazards predictions and hazards weights determinations. Health and safety practitioners can take remedial and preventative measures by using past data with utilization of proposed techniques.

  8. Obtaining Arbitrary Prescribed Mean Field Dynamics for Recurrently Coupled Networks of Type-I Spiking Neurons with Analytically Determined Weights

    Directory of Open Access Journals (Sweden)

    Wilten eNicola

    2016-02-01

    Full Text Available A fundamental question in computational neuroscience is how to connect a network of spiking neurons to produce desired macroscopic or mean field dynamics. One possible approach is through the Neural Engineering Framework (NEF. The NEF approach requires quantities called decoders which are solved through an optimization problem requiring large matrix inversion. Here, we show how a decoder can be obtained analytically for type I and certain type II firing rates as a function of the heterogeneity of its associated neuron. These decoders generate approximants for functions that converge to the desired function in mean-squared error like 1/N, where N is the number of neurons in the network. We refer to these decoders as scale-invariant decoders due to their structure. These decoders generate weights for a network of neurons through the NEF formula for weights. These weights force the spiking network to have arbitrary and prescribed mean field dynamics. The weights generated with scale-invariant decoders all lie on low dimensional hypersurfaces asymptotically. We demonstrate the applicability of these scale-invariant decoders and weight surfaces by constructing networks of spiking theta neurons that replicate the dynamics of various well known dynamical systems such as the neural integrator, Van der Pol system and the Lorenz system. As these decoders are analytically determined and non-unique, the weights are also analytically determined and non-unique. We discuss the implications for measured weights of neuronal networks

  9. Determination of solute site occupancies within γ' precipitates in nickel-base superalloys via orientation-specific atom probe tomography.

    Science.gov (United States)

    Meher, S; Rojhirunsakool, T; Nandwana, P; Tiley, J; Banerjee, R

    2015-12-01

    The analytical limitations in atom probe tomography such as resolving a desired set of atomic planes, for solving complex materials science problems, have been overcome by employing a well-developed unique and reproducible crystallographic technique, involving synergetic coupling of orientation microscopy with atom probe tomography. The crystallographic information in atom probe reconstructions has been utilized to determine the solute site occupancies in Ni-Al-Cr based superalloys accurately. The structural information in atom probe reveals that both Al and Cr occupy the same sub-lattice within the L12-ordered γ' precipitates to form Ni3(Al,Cr) precipitates in a Ni-14Al-7Cr (at%) alloy. Interestingly, the addition of Co, which is a solid solution strengthener, to a Ni-14Al-7Cr alloy results in the partial reversal of Al site occupancy within γ' precipitates to form (Ni,Al)3(Al,Cr,Co) precipitates. This unique evidence of reversal of Al site occupancy, resulting from the introduction of other solutes within the ordered structures, gives insights into the relative energetics of different sub-lattice sites when occupied by different solutes.

  10. Determination of atomic number and composition of human enamel; Determinacao da composicao e numero atomico efetivo do esmalte humano

    Energy Technology Data Exchange (ETDEWEB)

    Nogueira, M.S. [Centro Regional de Ciencias Nucleares (CRCN), Recife, PE (Brazil); Rodas Duran, J.E. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Filosofia, Ciencias e Letras. Dept. de Fisica e Matematica

    2001-07-01

    The teeth are organs of complicated structure that consist, partly, of hard tissue containing in its interior the dental pulp, rich in vases and nerves. The main mass of the tooth is constituted by the dentine, which is covered with hard tissues and of epithelial origin called enamel. The dentine of the human teeth used in this work were completely removed and the teeth were cut with a device with a diamond disc. In this work the chemical composition of the human enamel was determined, which showed a high percentage of Ca and P, in agreement with the results found in the literature. The effective atomic number of the material and the half-value layer in the energy range of diagnostic X-ray beams were determined. Teeth could be used to evaluated the public's individual doses as well as for retrospective dosimetry what confirms the importance of their effective atomic number and composition determination. (author)

  11. Matrix effects on the determination of manganese in geological materials by atomic-absorption spectrophotometry under different flame conditions

    Science.gov (United States)

    Sanzolone, R.F.; Chao, T.T.

    1978-01-01

    Suppression caused by five of the seven matrix elements studied (Si, Al, Fe, Ca and Mg) was observed in the atomic-absorption determination of manganese in geological materials, when synthetic solutions and the recommended oxidizing air-acetylene flame were used. The magnitude of the suppression effects depends on (1) the kind and concentration of the interfering elements, (2) the type of acid medium, and (3) the concentration of manganese to be determined. All interferences noted are removed or alleviated by using a reducing nitrous oxide-acetylene flame. The atomic-absorption method using this flame can be applied to the determination of total and extractable manganese in a wide range of geological materials without interferences. Analyses of six U.S. Geological Survey rock standards for manganese gave results in agreement with the reported values. ?? 1978.

  12. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  13. Determinants of relative weight and body fat distribution in an international perspective

    NARCIS (Netherlands)

    A. Molarius (Anu)

    1999-01-01

    textabstractOverweight can be defined as excess storage of body fat in an individual. In adult men with a "normal" weight, the percentage of body fat is about 15-20%. In women this percentage is higher, about 25-30%. In spite of the fact that differences in weight between individuals are only partly

  14. Extraction and preconcentration of selenium from aqueous solutions and its determination in water and hair samples by atomic-absorption spectrophotometry.

    Science.gov (United States)

    Ejaz, M; Qureshi, M A

    1987-03-01

    Several organic solvents, including benzene, xylene, toluene, nitrobenzene, chloroform, carbon tetrachloride, chlorobenzene and high molecular-weight pyridines such as 4-(5-nonyl)pyridine, 2-hexyl-pyridine and benzylpyridine have been investigated as components of systems for the extraction and preconcentration of selenium from nitric acid solutions containing iodide. The results are discussed in terms of choice of reagents and the acid and iodide concentrations, and of several other parameters affecting the extraction. The utility of the method for separation of selenium from aqueous solution has been evaluated. The method has been used for preconcentration of trace levels of selenium from water and hair samples for determination by atomic-absorption spectrophotometry.

  15. Simultaneous determination of arsenic, cadmium, copper, chromium, nickel, lead and thallium in total digested sediment samples and available fractions by electrothermal atomization atomic absorption spectroscopy (ET AAS).

    Science.gov (United States)

    Álvarez, María Á; Carrillo, Génesis

    2012-08-15

    This study describes the optimization and validation of a quick and simple method for the simultaneous determination of total content and available fractions of As, Cr, Cu, Ni, Pb and Tl in sediments by ET AAS, which has been proved to be useful for environmental research. The optimization was carried out using a 3(3) Box-Behnken factorial design which was applied to matrices of total digestion and to stages 1 and 2 of the modified BCR sequential extraction scheme for sediments in order to determine the appropriate atomization temperatures and masses for the chemical modifiers: Pd(NO(3))(2) and Mg(NO(3))(2). The simultaneous determination of the elements in all matrices considered was performed, without the use of chemical modifiers at atomization temperatures of 1700 °C for Cd and Tl, and 2100 °C for As, Cu, Cr, Ni and Pb, using a standard calibration curve for calibration purposes. The characteristic masses and limits of detection obtained were 36.5, 1.8, 6.5, 28, 34, 46.5 and 48 ρg and 0.11, 0.001, 0.022, 0.04, 0.2, 0.03 and 0.003 μg g(-1) for As, Cd, Cr, Cu, Ni, Pb and Tl, respectively. The analytical procedure was validated by analyzing three sediment certified reference materials (CRM NCS DC 73315 and LKSD-4 for total content and BCR 701 for available fractions). Good accuracy was obtained (tested statistically, P=0.05, and shown by the high recovery for each element in each matrix), except for total As in the matrix of total digestion, where losses of the analyte could be attributed to sample treatment with HNO(3). The precision of the procedure was between 0.6% and 6%.

  16. On the determination of the pion effective mass in nuclei from pionic atoms

    Science.gov (United States)

    Friedman, E.; Gal, A.

    1998-07-01

    The binding energies of the deeply bound 1s and 2p states in pionic atoms of 207Pb, recently established experimentally in the 208Pb(d,3He) reaction, have been used by several groups to derive the pion effective mass in nuclear matter. We show that these binding energies are fully consistent with `normal' pionic atoms and that the real part of the pion-nucleus potential at the center of 207Pb is 28+/-3 MeV and not 20 MeV as suggested previously.

  17. Time course and determinants of leptin decline during weight loss in obese boys and girls

    DEFF Research Database (Denmark)

    Holm, Jens-Christian; Gamborg, Michael; Kaas-Ibsen, Karsten;

    2007-01-01

    OBJECTIVE: To investigate whether changes in leptin concentrations during weight loss can be explained by gender, puberty, baseline adiposity and changes in adiposity, body composition, rate of weight loss, physical activity and insulin concentrations. DESIGN: A longitudinal study with 9 repeated...... size, physical activity scores, blood leptin (ng/ml) and insulin concentrations (pmol/l) were measured at baseline, and except for Tanner stage and testicular size, repeated regularly during the programme. RESULTS: The weight loss was accompanied by a steep decline in leptin concentrations during......, puberty, baseline adiposity or concomitant changes in BMI SDS, fat mass percentage, rate of weight loss, physical activity scores or insulin concentrations. CONCLUSION: The biphasic leptin decline, which exceeded the level expected, was independent of puberty, baseline adiposity and changes in adiposity...

  18. Important factors influencing molecular weight cut-off determination of membranes in organic solvents

    NARCIS (Netherlands)

    Zwijnenberg, Harmen Jan; Dutczak, S.M.; Boerrigter, M.E.; Hempenius, Mark A.; Luiten-Olieman, Maria W.J.; Benes, Nieck Edwin; Wessling, Matthias; Stamatialis, Dimitrios

    2012-01-01

    In solvent resistant nanofiltration (SRNF), sensible selection of a membrane for a particular solvent/solute system is recognized as challenging. Prospective methods for suitability analysis of membranes include molecular weight cut off (MWCO) characterization. However, insufficient understanding of

  19. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    Science.gov (United States)

    Ball, J.W.; Nordstrom, D.K.

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

  20. Predicting actual weight loss: A review of the determinants according to the theory of planned behaviour

    OpenAIRE

    Louisa Ming Yan Chung; Shirley Siu Ming Fong

    2015-01-01

    Weight reduction that corresponds with lifestyle modification is difficult to foster. The theory of planned behaviour has been actively cited in explaining health-related behaviour. This review evaluated the application of the theory of planned behaviour to weight-loss behaviour. Among the three reviewed papers, cross-sectional survey designs and subjective outcome measurements were commonly applied. All of the studies recruited obese female adults as participants, limiting the generalisabili...

  1. Predicting actual weight loss: A review of the determinants according to the theory of planned behaviour

    OpenAIRE

    Louisa Ming Yan Chung; Shirley Siu Ming Fong

    2015-01-01

    Weight reduction that corresponds with lifestyle modification is difficult to foster. The theory of planned behaviour has been actively cited in explaining health-related behaviour. This review evaluated the application of the theory of planned behaviour to weight-loss behaviour. Among the three reviewed papers, cross-sectional survey designs and subjective outcome measurements were commonly applied. All of the studies recruited obese female adults as participants, limiting the generalisabili...

  2. Conditions for Statistical Determination of the Neutrino Mass Spectrum in Radiative Emission of Neutrino Pairs in Atoms

    CERN Document Server

    Song, Ningqiang; Gomez-Cadenas, J J; Gonzalez-Garcia, M C; Conde, A Peralta; Taron, Josep

    2015-01-01

    The photon spectrum in macrocoherent atomic de-excitation via radiative emission of neutrino pairs (RENP) has been proposed as a sensitive probe of the neutrino mass spectrum, capable of competing with conventional neutrino experiments. In this paper we revisit this intriguing technique in order to quantify the requirements for statistical determination of some of the properties of the neutrino spectrum, in particular the neutrino mass scale and the mass ordering. Our results are sobering. We find that, even under ideal conditions, the determination of neutrino parameters needs experimental live times of the order of days to years for several laser frequencies, assuming a target of volume of order 100 cm3 containing about 10^21 atoms per cubic centimeter in a totally coherent state with maximum value of the electric field in the target. Such conditions seem to be, as of today, way beyond the reach of our current technology.

  3. EM-fold: de novo atomic-detail protein structure determination from medium-resolution density maps.

    Science.gov (United States)

    Lindert, Steffen; Alexander, Nathan; Wötzel, Nils; Karakaş, Mert; Stewart, Phoebe L; Meiler, Jens

    2012-03-07

    Electron density maps of membrane proteins or large macromolecular complexes are frequently only determined at medium resolution between 4 Å and 10 Å, either by cryo-electron microscopy or X-ray crystallography. In these density maps, the general arrangement of secondary structure elements (SSEs) is revealed, whereas their directionality and connectivity remain elusive. We demonstrate that the topology of proteins with up to 250 amino acids can be determined from such density maps when combined with a computational protein folding protocol. Furthermore, we accurately reconstruct atomic detail in loop regions and amino acid side chains not visible in the experimental data. The EM-Fold algorithm assembles the SSEs de novo before atomic detail is added using Rosetta. In a benchmark of 27 proteins, the protocol consistently and reproducibly achieves models with root mean square deviation values <3 Å.

  4. Determination of cadmium by electrothermal atomic absorption spectrometry after microwave-assisted digestion of animal tissues and sewage sludges.

    Science.gov (United States)

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-04-01

    The determination of cadmium in different sample types has been carried out by electrothermal atomization atomic absorption spectrometry with D(2)-background correction using a unpyrocoated graphite tube, after pressurized microwave-assisted digestion. Five chemical modifiers [(NH(4))(2)HPO(4), Pd(NO)(3))(2), Ni(NO(3))(2), thiourea and Triton X-100] have been assayed and nickel nitrate has been found to be most effective for an accurate determination of cadmium in mussel tissue, pig kidney and sewage sludge. The characteristic mass of the method is of the order of 1 pg and the limit of detection is lower than 0.1 ng/ml.

  5. Application of methane as a gaseous modifier for the determination of silicon using electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Heinrich, Hans-Joachim, E-mail: hans-joachim.heinrich@bam.de; Kipphardt, Heinrich

    2012-04-15

    For determination of silicon in aqueous solutions by electrothermal atomic absorption spectrometry methane/argon mixtures as a gaseous modifier were applied during the pyrolysis step to improve the analytical performance. The beneficial effects observed on thermal stabilization, signal enhancement and shape of absorbance signals were attributed to the thermal decomposition products of methane, which were hydrogen and carbon black (soot). Using a 5% CH{sub 4} mixture with argon, the optimized pyrolysis and atomization temperatures were 1350 Degree-Sign C and 2450 Degree-Sign C, respectively. A flushing step following the pyrolysis was mandatory to avoid background absorption and accelerated deposition of pyrolytic graphite. Characteristic masses of 50 and 30 pg were obtained for standard transversely heated graphite atomizer (THGA) tubes and end-capped THGA tubes, respectively, which were lower than with other previously applied modifiers. A limit of detection of 0.2 {mu}g L{sup -1} (3 s, n = 10) has been obtained. In addition, this gaseous modifier did not contribute to contamination which often was significant when a liquid modifier solution was co-injected. The proposed method has been applied to the determination of silicon in ultrapure water, nitric and hydrochloric acids. - Highlights: Black-Right-Pointing-Pointer CH{sub 4}/Ar gas mixtures act as new modifier in the determination of Si using ET AAS. Black-Right-Pointing-Pointer CH{sub 4} improved thermal stabilization, atomization efficiency and signal shape of Si. Black-Right-Pointing-Pointer Optimum performance by addition of 5% CH{sub 4} during pyrolysis at 1350 Degree-Sign C. Black-Right-Pointing-Pointer Gaseous modifier does not contribute to blank values. Black-Right-Pointing-Pointer Optimized method suitable for determination of Si in ultrapure reagents.

  6. Determination of the total iron content of used lubricating oils by atomic-absorption with use of emulsions.

    Science.gov (United States)

    Salvador, A; de la Guardia, M; Berenguer, V

    1983-12-01

    A new method is proposed for the determination of the total iron content of used lubricating oils. It is based on treatment of the samples with a mixture of hydrofluoric and nitric acids (without destruction of the organic matter) and emulsification, followed by atomic-absorption measurement. This allows the use of aqueous standards and provides a simple, rapid, inexpensive and accurate method, that is not affected by the particle size of the solids in the oil.

  7. Determination of Mercury in an Assortment of Dietary Supplements Using an Inexpensive Combustion Atomic Absorption Spectrometry Technique

    OpenAIRE

    Levine, Keith E.; Levine, Michael A.; Weber, Frank X.; Hu, Ye; Perlmutter, Jason; Grohse, Peter M.

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a res...

  8. Atom-chip-based quantum gravimetry for the precise determination of absolute gravity

    Science.gov (United States)

    Abend, Sven; Schubert, Christian; Ertmer, Wolfgang; Rasel, Ernst

    2017-04-01

    We present a novel technique for the precise measurement of absolute local gravity with a quantum gravimeter based on an atom chip. Atom interferometry utilizes the interference of matter waves interrogated by laser light to read out inertial forces. Today's generation of these devices typically operate with test mass samples, that consists of ensembles of laser cooled atoms. Their performance is limited by the velocity spread and finite-size of the test masses that impose systematic uncertainties at the level of a few μGal [1]. Rather than laser cooled atoms we employ quantum degenerate ensembles, so called Bose-Einstein condensates [2], as ultra-sensitive probes for gravity. These sources offer unique properties that will allow to overcome the current limitations in the next generation of sensors. Furthermore, atom-chip technology offers the possibility to generate Bose-Einstein condensates in a fast and reliable way. We present a lab-based prototype that uses the atom chip itself to retro-reflect the interrogation laser and thus serves as inertial reference inside the vacuum [3]. With this setup, it is possible to demonstrate all necessary steps to measure gravity, including the preparation of the source, spanning an interferometer as well as the detection of the output signal. All steps are pursued on a baseline of 1 cm right below the atom chip and to analyze relevant systematic effects. In the framework of the center of excellence geoQ a next generation device is under construction at the Institut für Quantenoptik, that will target for in-field measurements. This device will feature a state-of-the-art atom-chip source with a high-flux of ultra-cold atoms at a repetition rate of 1-2 Hz [4]. The device will be characterized in cooperation with the Müller group at the Institut für Erdmessung the sensor and finally employed in a campaign to measure the Fennoscandian uplift at the level of 1 μGal. The presented work is supported by the CRC 1227 DQ-mat, the

  9. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation.

  10. Lifetime determination of the 5d$^{2}$~$^{3}$F$_{2}$ state in barium using trapped atoms

    CERN Document Server

    De, S; Willmann, L

    2015-01-01

    Magneto-optically trapped atoms enable the determination of lifetimes of metastable states and higher lying excited states like the $\\rm{5d^{2}~^{3}F_{2}}$ state in barium. The state is efficiently populated by driving strong transitions from metastable states within the cooling cycle of the barium MOT. The lifetime is inferred from the increase of MOT fluorescence after the transfer of up to $30\\,\\%$ of the trapped atoms to this state. The radiative decay of the $\\rm{5d^{2}~^{3}F_{2}}$ state cascades to the cooling cycle of the MOT with a probability of $96.0(7)\\,\\%$ corresponding to a trap loss of $4.0(7)\\,\\%$ and its lifetime is determined to $\\rm{160(10)~\\mu s}$. This is in good agreement with the theoretically calculated lifetime of $\\rm{190~\\mu s}$ [J. Phys. B, {\\bf 40}, 227 (2007)]. The determined loss of $4.0(7)\\,\\%$ from the cooling cycle is compared with the theoretically calculated branching ratios. This measurement extends the efficacy of trapped atoms to measure lifetimes of higher, long-lived st...

  11. Adequate weight gain in pregnancy: An analysis of its determinants in a cross-sectional study

    Directory of Open Access Journals (Sweden)

    Popa Alina Delia

    2014-01-01

    Full Text Available Introduction. Prenatal care is considered an important tool for promoting a healthy lifestyle, but has not been studied as a predictor for maternal weight gain during pregnancy, especially in Romania, where evidence about pregnancy and nutrition is scarce. Objective. This study has aimed to explore the relationship between pre-gestational body mass index (BMI, adequacy of prenatal care and weight gain during pregnancy. Methods. We carried a cross-sectional study on a sample of 400 pregnant women admitted at the “Cuza Voda” Obstetrics and Gynecology Hospital in Iasi. Information regarding demographic characteristics, number of prenatal visits, date of the initial hospital record, nutritional education during pregnancy were registered throughout a questionnaire filled out by means of a direct interview. The anthropometric indicators analyzed were the pre-gestational BMI and the pregnancy weight gain. Data on caloric intake were obtained using a food frequency questionnaire. Results. Weight gain within the limits of the Institute of Medicine recommendations was noticed at 44.35% of the women who declared that they received nutritional advice compared to 40.7% of those who did not receive advice regarding diet during pregnancy. Overweight (53.1% and obese women (66.7% had a larger weight gain than those with a normal pre-pregnancy BMI (29.8% (p<0.001. The variables that were identified with an effect on weight gain in this sample of pregnant women were: inadequate prenatal care, pre-gestational BMI and energy intake. Conclusion. Identifying the pre-gestational BMI and diet changes as predictors of weight gain underline the importance of an individualized prenatal care.

  12. Atomically resolved structural determination of graphene and its point defects via extrapolation assisted phase retrieval

    Energy Technology Data Exchange (ETDEWEB)

    Latychevskaia, Tatiana; Fink, Hans-Werner [Physics Department, University of Zurich, Winterthurerstrasse 190, 8057 Zurich (Switzerland)

    2015-01-12

    Previously reported crystalline structures obtained by an iterative phase retrieval reconstruction of their diffraction patterns seem to be free from displaying any irregularities or defects in the lattice, which appears to be unrealistic. We demonstrate here that the structure of a nanocrystal including its atomic defects can unambiguously be recovered from its diffraction pattern alone by applying a direct phase retrieval procedure not relying on prior information of the object shape. Individual point defects in the atomic lattice are clearly apparent. Conventional phase retrieval routines assume isotropic scattering. We show that when dealing with electrons, the quantitatively correct transmission function of the sample cannot be retrieved due to anisotropic, strong forward scattering specific to electrons. We summarize the conditions for this phase retrieval method and show that the diffraction pattern can be extrapolated beyond the original record to even reveal formerly not visible Bragg peaks. Such extrapolated wave field pattern leads to enhanced spatial resolution in the reconstruction.

  13. Determination of Optimum Conditions for Distinguishing the Pulse Height Distributions of Atomic and Polyatomic Ions

    Energy Technology Data Exchange (ETDEWEB)

    Kristo, M J

    2006-12-12

    This work explored the use of pulse height distributions (PHD) from multiplier-type detectors as a means of detecting and eliminating the effects of polyatomic interferences in secondary ion mass spectrometry (SIMS). We explored the behavior of PHD for {sup 235}U{sup +}, {sup 208}Pb{sup 27}Al{sup +} and {sup 207}Pb{sup 28}Si{sup +}, all with a nominal mass-to-charge ratio of 235. In every case, the distribution for the atomic ion ({sup 235}U{sup +}) was clearly shifted relative to the distributions for {sup 208}Pb{sup 27}Al{sup +} and {sup 207}Pb{sup 28}Si{sup +}. When the first surface of the detector is metallic in character, the polyatomic ions are shifted to larger pulse heights relative to the atomic ion. When the first surface of the detector is oxide in character, the atomic ion is shifted to larger pulse heights relative to the polyatomic ions. The relative positioning appear to be stable for a given detector over time at the same secondary ion impact energy. Consequently, it appears to be feasible to use PHD data to detect interfering polyatomic ions and eliminate their deleterious effects using peak deconvolution techniques. Consequently, the updated Ultrafast RAE detector will be designed to make the pulse height information available to the data acquisition system.

  14. Cooking fuel choices and garbage burning practices as determinants of birth weight: a cross-sectional study in Accra, Ghana

    Directory of Open Access Journals (Sweden)

    Amegah Adeladza K

    2012-10-01

    Full Text Available Abstract Background Effect of indoor air pollution (IAP on birth weight remains largely unexplored but yet purported as the most important environmental exposure for pregnant women in developing countries due to the effects of second-hand smoke. We investigated the associations between the determinants of indoor air quality in households and birth weight. Methods A cross-sectional study of 592 mothers and their newborns using postnatal services at the Korle Bu Teaching Hospital located in Accra, Ghana was conducted in 2010 to collect information on characteristics of indoor environment and other potential determinants of fetal growth. Birth weight was recorded from hospital records. Results Household cooking fuel choices and garbage burning practices were determinants of birth weight. Multivariate linear regression analysis adjusting for age, social class, marital status and gravidity of mothers, and sex of neonate resulted in a 243g (95% CI: 496, 11 and 178g (95% CI: 421, 65 reduction in birth weight for use of charcoal, and garbage burning respectively compared with use of LPG only. The estimated reductions in birth weight was not statistically significant. Applying the ordinal scale exposure parameter nonetheless revealed a significant exposure-response relationship between maternal exposures from charcoal use and garbage burning, and birth weight. Generalized linear models adjusting for confounders resulted in a 41% (risk ratio [RR] = 1.41; 95% CI: 0.62, 3.23 and 195% (RR=2.95; 95% CI: 1.10, 7.92 increase in the risk of low birth weight (LBW for use of charcoal, and garbage burning respectively compared with use of LPG only. A combination of charcoal use and household garbage burning during pregnancy on fetal growth resulted in a 429g (95% CI: 259, 599 reduction in birth weight and 316% (RR=4.16; 95% CI: 2.02, 8.59 excess risk of LBW. Sensitivity analysis performed by restricting the analysis to term births produced similar results

  15. Calculation of the weighting function and determination of the depth of correlation in micro-PIV from experimental particle images

    Science.gov (United States)

    Hein, M.; Wieneke, B.; Seemann, R.

    2014-08-01

    Micro-particle image velocimetry (µPIV) uses volume-illumination and imaging of particles through a single microscope objective. Displacement fields are obtained by image correlation and depend on all imaged particles, including defocused particles. The measured in-plane displacement is a weighted spatial average of the true displacement, with a weighting function W(z) that depends on the optical system and flow-gradients. The characteristic width of the weighting function W(z) is also referred to as depth of correlation (DOC) and is a measure up to which distance from the focal plane particles influence the measurement, which is crucial for the interpretation of measured flow fields. We present procedures to determine the W(z) from which the DOC can be derived and to directly determine the DOC from PIV double images, generated from experimentally recorded particle images. Both procedures provide comparable DOC results. Our approach allows determination of the DOC and W(z)as a function of out of plane gradients, optical setup parameters and PIV-analysis parameters. Experimental results for different objectives and particle sizes are discussed, revealing substantial deviations from theoretical predictions for high NA air-objectives. Moreover, using the determined weighting function W(z), the correction of measured flow profiles for errors introduced by the spatial averaging is demonstrated.

  16. Dietary protein-to-carbohydrate ratio and added sugar as determinants of excessive gestational weight gain

    DEFF Research Database (Denmark)

    Maslova, Ekaterina; Halldorsson, Thorhallur I; Astrup, Arne;

    2015-01-01

    OBJECTIVE: To examine the relation between the protein:carbohydrate (P/C) ratio and added sugar intake in pregnancy and gestational weight gain (GWG). DESIGN: A prebirth cohort including 103 119 pregnancies enrolled between 1996 and 2003. SETTING: All women in Denmark were eligible to participate...... and defined as gain in g/week. We used multivariable linear regression, including adjusting for pre-pregnancy body mass index, to calculate relative change in GWG and 95% CI. RESULTS: Average GWG was 471(224) g/week. The adjusted weight gain was 16 g/week lower (95% CI 9 to 22, p for trend ....001) in the highest (Q5) versus lowest (Q1) quintile of the P/C ratio (∼3% average reduction across the entire pregnancy). Weight gain for those with >20%E vs

  17. Dietary protein-to-carbohydrate ratio and added sugar as determinants of excessive gestational weight gain

    DEFF Research Database (Denmark)

    Maslova, Ekaterina; Halldorsson, Thorhallur I; Astrup, Arne

    2015-01-01

    OBJECTIVE: To examine the relation between the protein:carbohydrate (P/C) ratio and added sugar intake in pregnancy and gestational weight gain (GWG). DESIGN: A prebirth cohort including 103 119 pregnancies enrolled between 1996 and 2003. SETTING: All women in Denmark were eligible to participate...... for the analysis. EXPOSURE: Macronutrient intake was quantified using a validated food frequency questionnaire administered in the 25th week of gestation. The P/C ratio and added sugar intake were examined in quintiles. PRIMARY OUTCOME MEASURES: GWG was based on self-reported weight in gestational weeks 12 and 30.......001) in the highest (Q5) versus lowest (Q1) quintile of the P/C ratio (∼3% average reduction across the entire pregnancy). Weight gain for those with >20%E vs reduction). A high P/C ratio was inversely related to intake of added...

  18. Predicting actual weight loss: A review of the determinants according to the theory of planned behaviour

    Directory of Open Access Journals (Sweden)

    Louisa Ming Yan Chung

    2015-01-01

    Full Text Available Weight reduction that corresponds with lifestyle modification is difficult to foster. The theory of planned behaviour has been actively cited in explaining health-related behaviour. This review evaluated the application of the theory of planned behaviour to weight-loss behaviour. Among the three reviewed papers, cross-sectional survey designs and subjective outcome measurements were commonly applied. All of the studies recruited obese female adults as participants, limiting the generalisability of the studies’ findings. The theory of planned behaviour can be effectively applied in weight-reduction programmes targeting female obese patients. This review confirmed critiques citing the limitations of experimental studies, the subjective measurement of behaviour and short follow-up periods.

  19. Predicting actual weight loss: A review of the determinants according to the theory of planned behaviour.

    Science.gov (United States)

    Chung, Louisa Ming Yan; Fong, Shirley Siu Ming

    2015-01-01

    Weight reduction that corresponds with lifestyle modification is difficult to foster. The theory of planned behaviour has been actively cited in explaining health-related behaviour. This review evaluated the application of the theory of planned behaviour to weight-loss behaviour. Among the three reviewed papers, cross-sectional survey designs and subjective outcome measurements were commonly applied. All of the studies recruited obese female adults as participants, limiting the generalisability of the studies' findings. The theory of planned behaviour can be effectively applied in weight-reduction programmes targeting female obese patients. This review confirmed critiques citing the limitations of experimental studies, the subjective measurement of behaviour and short follow-up periods.

  20. Predicting actual weight loss: A review of the determinants according to the theory of planned behaviour

    Directory of Open Access Journals (Sweden)

    Louisa Ming Yan Chung

    2015-01-01

    Full Text Available Weight reduction that corresponds with lifestyle modification is difficult to foster. The theory of planned behaviour has been actively cited in explaining health-related behaviour. This review evaluated the application of the theory of planned behaviour to weight-loss behaviour. Among the three reviewed papers, cross-sectional survey designs and subjective outcome measurements were commonly applied. All of the studies recruited obese female adults as participants, limiting the generalisability of the studies’ findings. The theory of planned behaviour can be effectively applied in weight-reduction programmes targeting female obese patients. This review confirmed critiques citing the limitations of experimental studies, the subjective measurement of behaviour and short follow-up periods.

  1. Genetic determinism for within-litter birth weight variation and its relationship with litter weight and litter size in the Ripollesa ewe breed.

    Science.gov (United States)

    Casellas, J; Caja, G; Piedrafita, J

    2007-06-01

    Birth weight plays a central role in lamb survival and growth, and the knowledge of its genetic determinism has become essential in worldwide selection programmes. Within this context, within-litter birth weight variation (BWV) has been suggested as an attractive trait to homogenise litters in prolific species, although it has not been analysed in sheep. The objective of this study was to ascertain whether maternal additive genetic variance exists for BWV in Ripollesa ewes, and to study its genetic, permanent environmental and residual relationships with litter weight (LW) and litter size (LS) at birth. Data were recorded in the Ripollesa experimental flock of the Universitat Autònoma of Barcelona, between 1986 and 2005, and included 1 662 litters from 380 ewes, with 712 records of BWV and 1 530 records of LW. Traits were analysed with a multivariate animal model solved through Bayesian methodologies, and with a threshold characterisation of LS. Additionally, the effect of BWV on lamb survival was studied. Additive genetic variance was observed for BWV (h2 = 0.061), as well as for LW (h2 = 0.200) and LS (h2 = 0.141). Nevertheless, genetic correlations among those traits were not substantial (BWV and LW = 0.151; BWV and LS = - 0.219; LW and LS = - 0.320) and suffered from a high degree of uncertainly, with the null correlation included within the highest posterior interval at 95%. Within-litter birth weight variation and LS showed a negative and large permanent environmental correlation ( - 0.872), and LW and LS were negatively correlated due to residual ( - 0.762) and permanent environmental ( - 0.449) random sources of variation. Within-litter birth weight variation influenced lamb mortality during the first 7 days of life (P 0.05). The low heritability found indicates that slow genetic progress may be expected from selecting for BWV. Close to zero genetic correlations suggest that this selection will probably not affect LS and LW, although

  2. Determination of gold in copper-bearing sulphide ores and metallurgical flotation products by atomic-absorption spectrometry.

    Science.gov (United States)

    Strong, B; Murray-Smith, R

    1974-12-01

    A method is described which is specific for the determination of gold in sulphide copper ores and concentrates. Direct decomposition with aqua regia was found to be incomplete. A carefully controlled roasting stage followed by treatment with hydrochloric acid and then aqua regia was effective for dissolving all the gold. The gold is extracted into 4-methylpentan-2-one (methyli-sobutylketone) then aspirated into a very lean air-acetylene flame and the gold determined by atomic-absorption spectrometry. No interferences were observed from large concentrations of copper, iron or nickel.

  3. Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

    Science.gov (United States)

    Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

    1971-01-01

    A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

  4. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    Science.gov (United States)

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection.

  5. Determination of Ultratrace Amounts of Copper(Ⅱ) in Water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction (CPE). 1-( 2-Pyridylazo)-2-naphthol was used as the chelating reagent and Triton X-114 as the micellar-forming surfactant. CPE was conducted in a pH 8.0 medium at 40 ℃ for 10 min. After the separation of the phases by centrifugation, the surfactant-rich phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20 μL of the diluted surfactant-rich phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconcentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0ng/mL, and the relative standard deviation was found to be less than 3.1% for a sample containing 1.0 ng/mL Cu(Ⅱ). This developed method was successfully applied to the determination of ultratrace amounts of Cu in drinking water, tap water, and seawater samples.

  6. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu Qingyang, E-mail: liuqingyang0807@yahoo.com.c [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2010-07-15

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg{sup 0}, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL{sup -1} for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  7. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Science.gov (United States)

    Liu, Qingyang

    2010-07-01

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg 0, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL -1 for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury ( n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  8. Atomic spectroscopy and highly accurate measurement: determination of fundamental constants; Spectroscopie atomique et mesures de grande precision: determination de constantes fonfamentales

    Energy Technology Data Exchange (ETDEWEB)

    Schwob, C

    2006-12-15

    This document reviews the theoretical and experimental achievements of the author concerning highly accurate atomic spectroscopy applied for the determination of fundamental constants. A pure optical frequency measurement of the 2S-12D 2-photon transitions in atomic hydrogen and deuterium has been performed. The experimental setting-up is described as well as the data analysis. Optimized values for the Rydberg constant and Lamb shifts have been deduced (R = 109737.31568516 (84) cm{sup -1}). An experiment devoted to the determination of the fine structure constant with an aimed relative uncertainty of 10{sup -9} began in 1999. This experiment is based on the fact that Bloch oscillations in a frequency chirped optical lattice are a powerful tool to transfer coherently many photon momenta to the atoms. We have used this method to measure accurately the ratio h/m(Rb). The measured value of the fine structure constant is {alpha}{sub -1} = 137.03599884 (91) with a relative uncertainty of 6.7*10{sup -9}. The future and perspectives of this experiment are presented. This document presented before an academic board will allow his author to manage research work and particularly to tutor thesis students. (A.C.)

  9. Determination of low molecular weight thiols using monobromobimane fluorescent labeling and high-performance liquid chromatography

    Science.gov (United States)

    Fahey, Robert C.; Newton, Gerald L.

    1988-01-01

    Methods are described for the preparation and high-performance liquid chromatography (HPLC) analysis of monobromobimane derivatives of low molecular weight thiols in extracts of biological samples. Typical problems encountered in the development and application of these methods are discussed. Analysis of mung bean extract is used as an example.

  10. Weight-based determination of spinal canal depth for paediatric lumbar punctures.

    Science.gov (United States)

    Bailie, Helen C; Arthurs, Owen J; Murray, Matthew J; Kelsall, A Wilf

    2013-11-01

    The aim of this study was to evaluate whether spinal canal depth (SCD), measured using ultrasound, could be estimated from simple body measurements in a sample of children. We measured SCD in a group of 225 children aged 0-18 years in the curved left lateral position using ultrasound. Statistical analysis was performed using Pearson's correlation coefficient at the 5% level of significance. We also performed linear regression analyses (analysis of variance) for mid-spinal canal depth (MSCD), including five potential predictors of age, gender, height, weight and body surface area, in each model. The mean MSCD was 33.0 mm (18.1-56.4) across the whole cohort. The best linear correlation of MSCD (mm) was found with weight (W; kg), approximating the formula MSCD=0.4W+20 (R(2)=0.72). Body weight accounted for 85% of the variance in the data (adjusted R(2)=0.72). Our formula gives values outside of the actual measured SCD range in 23/225 (10.2%) of cases and estimates MSCD at 24 mm at 10 kg, 32 mm at 30 kg and 40 mm at 50 kg. We demonstrate a good correlation between weight and MSCD in a large group of children. Use of the simple formula MSCD (mm)=0.4 W+20 could improve the success rates of lumbar puncture in the paediatric population, but remains to be validated.

  11. Energy intake and energy expenditure for determining excess weight gain in pregnant women

    Science.gov (United States)

    To conduct a secondary analysis designed to test whether gestational weight gain is the result of increased energy intake or adaptive changes in energy expenditures. In this secondary analysis, energy intake and energy expenditure of 45 pregnant women (body mass index [BMI] 18.5-24.9 [n=33] and BMI ...

  12. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Energy Technology Data Exchange (ETDEWEB)

    Angeli, Valeria [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Biagi, Simona [National Research Council of Italy, C.N.R., Istituto per i Processi Chimico-Fisici - IPCF-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ghimenti, Silvia [University of Pisa, Department of Chemistry and Industrial Chemistry, Via Risorgimento 35, 56126 Pisa (Italy); Onor, Massimo; D' Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2011-11-15

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H{sub 2} miniaturized flame after sodium borohydride reduction to Hg{sup 0}, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H{sub 2} microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10{sup -5} mol L{sup -1}), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L{sup -1} (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 {mu}mol L{sup -1} were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were

  13. Microwave-assisted extraction and ultrasonic slurry sampling procedures for cobalt determination in geological samples by electrothermal atomic absorption spectroscopy.

    Science.gov (United States)

    Felipe-Sotelo, M; Carlosena, A; Fernández, E; López-Mahía, P; Muniategui, S; Prada, D

    2004-06-17

    Slurry sampling is compared to microwave-assisted acid digestion for cobalt determination in soil/sediment samples by electrothermal atomic absorption spectrometry (ETAAS). Furnace temperature programs and appropriate amounts of three chemical modifiers were optimised in order to get the highest signals and good separations between the atomic and background signals. Using nitric acid (0.5% (v/v)) as liquid medium, no chemical modifier was needed. The detection limit, based on integrated absorbance, was 0.04mugg(-1) for digests and slurries. Within-batch precision and analytical recoveries were satisfactory for both procedures. Accuracy was tested by analysing a reference soil and a sediment from IRMM. The methods were further compared employing a set of roadside soils and estuarine sediments. As no significant differences (95% confidence) were found, practical analytical properties were suggested in order to select one of them.

  14. Childhood Excess Weight in Spain From 2006 to 2012. Determinants and Parental Misperception.

    Science.gov (United States)

    Ramiro-González, María D; Sanz-Barbero, Belén; Royo-Bordonada, Miguel Ángel

    2017-08-01

    Due to the high prevalence of childhood obesity in Spain, we analyzed changes in its prevalence from 2006 to 2007 and from 2011 to 2012, as well as diet, sleep, and sedentary habits in 5- to 14-year-olds and parental misperceptions about their children's excess weight. The sample was from the Spanish National Health Surveys for 2006 to 2007 (n=5590) and for 2011 to 2012 (n=3601). Data were collected by trained personnel through telephone interviews with parents/guardians. Weight and height were self-reported and the International Obesity Task Force cutpoints were used to define overweight and obesity. The prevalence of childhood excess weight was 30.1% from 2006 to 2007 and 29.7% from 2011 to 2012, while that of childhood obesity was 9.6% and 9%, respectively. Parental misperception of childhood excess weight increased from 60.8% to 71.4% (P<.001). Daily consumption of vegetables increased by 7.8%, while that of soft drinks and snacks decreased. This decrease was greatest in children from families with a low socioeconomic status, who also decreased their consumption of sweets and fast food. Adherence to sleep recommendations decreased by 5%, but adherence to recommended sedentary time did not change. High childhood overweight and obesity rates remained stable in Spain from 2006 to 2007 and from 2011 to 2012, but there was an increase in parental misperception of childhood excess weight. Despite reduced consumption of soft drinks and snacks, there was low adherence to dietary recommendations, hours of sleep, and sedentary habits. Copyright © 2016 Sociedad Española de Cardiología. Published by Elsevier España, S.L.U. All rights reserved.

  15. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  16. Entropy method for determination of weight of evaluating indicators in fuzzy synthetic evaluation for water quality assessment

    Institute of Scientific and Technical Information of China (English)

    ZOU Zhi-hong; YUN Yi; SUN Jing-nan

    2006-01-01

    Considering the difficulty of fuzzy synthetic evaluation method in calculation of the multiple factors and ignorance of the relationship among evaluating objects, a new weight evaluation process using entropy method was introduced. This improved method for determination of weight of the evaluating indicators was applied in water quality assessment of the Three Gorges reservoir area.The results showed that this method was favorable for fuzzy synthetic evaluation when there were more than one evaluating objects.One calculation was enough for calculating every monitoring point. Compared with the original evaluation method, the method predigested the fuzzy synthetic evaluation process greatly and the evaluation results are more reasonable.

  17. Influence of supersaturated carbon on the diffusion of Ni in ferrite determined by atom probe tomography

    KAUST Repository

    Kresse, T.

    2013-09-01

    In patented and cold-drawn pearlitic steel wires dissociation of cementite occurs during mechanical deformation. In this study the influence of the carbon decomposition on the diffusion of nickel in ferrite is investigated by means of atom probe tomography. In the temperature range 423-523 K we observed a much smaller activation energy of Ni diffusion than for self-diffusion in body-centered cubic iron, indicating an increased vacancy density owing to enhanced formation of vacancy-carbon complexes. © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  18. A precision analysis and determination of the technical requirements of an atom interferometer for gravity measurement

    Institute of Scientific and Technical Information of China (English)

    Zhao-ying WANG; Tao CHEN; Xiao-long WANG; Zhang ZHANG; Yun-fei XU; Qiang LIN

    2009-01-01

    The influence of the wave-front curvature of Raman pulses on the measurement precision of gravitational acceleration in atom interferometry is analysed by the method of a transmission matrix. It is shown that the measurement precision of gravitational acceleration is largely dependent on the spot size of the Raman pulse, the temporal interval between Raman pulses and the optical path difference of the two counter-propagating Raman pulses. Moreover, the influence of Doppler frequency shift on the precision is discussed. In order to get a certain measurement precision, the requirement for the accuracy of frequency scanning of the Raman pulse to compensate for the Doppler frequency shift is obtained.

  19. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively.

  20. Comparison of Adsorbed Mercury Screening Method With Cold-Vapor Atomic Absorption Spectrophotometry for Determination of Mercury in Soil

    Science.gov (United States)

    Easterling, Donald F.; Hovanitz, Edward S.; Street, Kenneth W.

    2000-01-01

    A field screening method for the determination of elemental mercury in environmental soil samples involves the thermal desorption of the mercury from the sample onto gold and then the thermal desorption from the gold to a gold-film mercury vapor analyzer. This field screening method contains a large number of conditions that could be optimized for the various types of soils encountered. In this study, the conditions were optimized for the determination of mercury in silty clay materials, and the results were comparable to the cold-vapor atomic absorption spectrophotometric method of determination. This paper discusses the benefits and disadvantages of employing the field screening method and provides the sequence of conditions that must be optimized to employ this method of determination on other soil types.

  1. Contents of cadmium, mercury and lead in fish from the Atlantic sea (Morocco) determined by atomic absorption spectrometry.

    Science.gov (United States)

    Chahid, Adil; Hilali, Mustapha; Benlhachimi, Abdeljalil; Bouzid, Taoufiq

    2014-03-15

    As a part of a specific monitoring program, lead (Pb) cadmium (Cd) and mercury (Hg) concentrations in important species of fish from various fishing ports of the southern Kingdom of Morocco (Sardina pilchardus, Scomber scombrus, Plectorhinchus mediterraneus, Trachurus trachurus, Octopus vulgaris, Boops boops, Sarda sarda, Trisopterus capelanus, and Conger conger) were investigated by the Moroccan Reference Laboratory (NRL) for trace elements in foodstuffs of animal origin. The samples were analysed for lead and cadmium by a graphite furnace atomic absorption spectrometry (GFAAS); and for mercury by cold vapour atomic absorption spectrometry (CVAAS). The results were expressed as μg/g of wet weight (w/w). The levels of Cd, Pb and Hg in muscles of fish were 0.009-0.036, 0.013-0.114 and 0.049-0.194 μg/g, respectively. The present study showed that different metals were present in the sample at different levels but within the maximum residual levels prescribed by the EU for the fish and shellfish from these areas, in general, should cause no health problems for consumers.

  2. Atomic structures suggest determinants of transmission barriers in mammalian prion disease.

    Science.gov (United States)

    Apostol, Marcin I; Wiltzius, Jed J W; Sawaya, Michael R; Cascio, Duilio; Eisenberg, David

    2011-04-05

    Prion represents a unique class of pathogens devoid of nucleic acid. The deadly diseases transmitted by it between members of one species and, in certain instances, to members of other species present a public health concern. Transmissibility and the barriers to transmission between species have been suggested to arise from the degree to which a pathological protein conformation from an individual of one species can seed a pathological conformation in another species. However, this hypothesis has never been illustrated at an atomic level. Here we present three X-ray atomic structures of the same segment from human, mouse, and hamster PrP, which is critical for forming amyloid and confers species specificity in PrP seeding experiments. The structures reveal that different sequences encode different steric zippers and suggest that the degree of dissimilarity of these zipper structures gives rise to transmission barriers in prion disease, such as those that protect humans from acquiring bovine spongiform encephalopathy (BSE) and chronic wasting disease (CWD).

  3. Determination of Elements by Atomic Absorption Spectrometry in Medicinal Plants Employed to Alleviate Common Cold Symptoms

    Institute of Scientific and Technical Information of China (English)

    F Zehra Küçükbay; Ebru Kuyumcu

    2014-01-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of com-mon cold have been studied for their mineral contents .Eleven minor and major elements (essential ,non-essen-tial and toxic) were identified in the Asplenium adiantum-nigrum L .,Althaea of ficinalis L .,Verbascum phlomoides L .,Euphorbiachamaesyce L .,Zizyphus jujube Miller ,Peganum harmala L .,Arum dioscori-dis Sm .,Sambucus nigra L .,Piper longum L .,Tussilago farfara L .and Elettariacardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrom-etry .Microwave digestion procedure for total concentration was applied under optimized conditions for dissolu-tion of medicinal plants .Plant based biological certified reference materials (CRMs) served as standards for quantification .These elements are found to be present in varying concentrations in the studied plants .The baseline data presented in this work can be used in understanding the role of essential ,non-essential and toxic elements in nutritive ,preventive and therapeutic properties of medicinal plants .

  4. Simple Atomic Absorption Spectroscopic and Spectrophotometric Methods for Determination of Pioglitazone Hydrochloride and Carvedilol in Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    Afaf A. Abdelmonem

    2014-01-01

    Full Text Available This study represents simple atomic absorption spectroscopic and spectrophotometric methods for determination of pioglitazone hydrochloride (PGZ-HCl and carvedilol (CRV based on formation of ion-pair associates between drugs and inorganic complex, bismuth(III tetraiodide (Method A and between drugs and organic acidic dyes, fast green and orange G (Method B. Method A is based on formation of ion-pair associate between drugs and bismuth(III tetraiodide in acidic medium to form orange-red ion-pair associates, which can be quantitatively determined by two different procedures. The formed ion-pair associate is extracted by methylene chloride, dissolved in acetone, dried, and then decomposed by hydrochloric acid, and bismuth content is determined by direct atomic absorption spectrometric technique (Procedure 1 or extracted by methylene chloride, dissolved in acetone, and quantified spectrophotometrically at 490 nm (Procedure 2. Method B is based on formation of ion-pair associate between drugs and either fast green dye or orange G dye in acidic medium to form ion-pair associates. The formed ion-pair associate is extracted by methylene chloride and quantified spectrophotometrically at 630 nm (for fast green dye method or 498 nm (for orange G dye method. Optimal experimental conditions have been studied. Both methods are applied for determination of the drugs in tablets without interference.

  5. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  6. Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

    Science.gov (United States)

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

  7. Determining an Appropriate Weight attribute in Fraud Call Rate Data Using Case Based Reasoning

    Directory of Open Access Journals (Sweden)

    Musa Bala Shuaibu

    2014-03-01

    Full Text Available Fraud cases are significantly causing huge revenue losses in telecommunication companies around the world. Although previous cases are very important data in dealing with fraud patterns, there are variations in the dataset of different fraud case scenarios which in turns need specific detection system without necessarily involving the domain expert directly. This paper investigates the appropriate weight values for attributes using fraud Call Rate Data that is based on Artificial Intelligence technique (Case Based Reasoning with a meaningful confidence in telecommunication data. The experimental result on the fraud data reports that the weight for all attribute used in this study needs to be set at 0.9 in order to get the best performance of 98.33%.

  8. The lancet weight determines wheal diameter in response to skin prick testing with histamine

    DEFF Research Database (Denmark)

    Andersen, Hjalte Holm; Lundgaard, Anna Charlotte; Sohrt Petersen, Anne

    2016-01-01

    BACKGROUND: Skin prick test (SPT) is a common test for diagnosing immunoglobulin E-mediated allergies. In clinical routine, technicalities, human errors or patient-related biases, occasionally results in suboptimal diagnosis of sensitization. OBJECTIVE: Although not previously assessed...... with potential diagnostic implications. This warrants additional research of the optimal lancet weight in relation to SPT-guidelines to improve the specificity and sensitivity of the procedure....

  9. Lab-on-a-Chip method uncertanties in determination of high-molecular-weight glutenin subunits

    Directory of Open Access Journals (Sweden)

    Živančev Dragan R.

    2013-01-01

    Full Text Available Polymeric wheat endosperm proteins, especially the high-molecular-weight glutenin subunits (HMW-GS, are probably the most interesting protein fraction giving the essential information about bread-making quality of wheat flour. A relatively new method that shows a great potential for a fast, reliable and automatable analysis of protein purity, sizing and quantification is microfluidic or Lab-on-a-Chip (LoaC capillary electrophoresis. This work was aimed to explore the possibilities of implementation of LoaC method to analysis of protein samples isolated from a Serbian common wheat variety, emphasizing the steps that might bring uncertainties and affect reproducibility of obtained glutenin subunits quantitation results. A good resolution of protein bands in a molecular weight range of 14.0 to 220.0 kDa was achieved. The reproducibility of HMW-GS sizing and quantitation were good, with the average coefficient of variation values of 1.2% and 12.2%. The ratio of HMW-GS to low-molecular-weight glutenin subunits (LMW-GS was about 20%. The investigation ruled out influences of the extract solution addition and the buffer addition steps of the applied method, as well as the individual chip influence on GS quantitation results. However, there was statistically significant difference between HMW-GS quantitation results of multi-step and one-step extraction procedures applied prior to glutenin subunits extraction step.

  10. Noise variance estimation and optimal weight determination for GOCE gravity recovery­

    Directory of Open Access Journals (Sweden)

    J. Kusche

    2003-01-01

    Full Text Available In the course of level 2 data processing for the GOCE (Gravity Field and Steady–State Ocean Circulation Explorer satellite mission different streams of level 1b data will be merged in a single solution providing the Earth’s gravity field, but also state-vector parameters and other quantities. A proper weighting of orbit tracking data, gravity gradiometry data and certain a priori information, usually considered as ‘solution constraints’, can be expected as crucial for the solution quality. But the a priori stochastic models, based on pre–mission assessment of the expected instrument behaviour, may be over–optimistic or even too pessimistic since they refer to an unprecedented mission with scientific payload never tested in space. One way to derive an optimal weighting scheme on a statistically sound basis while simultaneously validating the stochastic noise levels of the data is by including variance component estimation as a part of the level 1b to level 2 data analysis process. The idea is that by applying Monte-Carlo techniques this method can be extended to a large-scale problem like GOCE data analysis, using software modules that already exist or are currently under development. The proposed method has been tested using simulated GOCE orbit trajectories as well as gravity gradiometry data corrupted by colored random noise.Key words. GOCE, gravity field modelling, combination solutions, weight estimation, variance component estimation

  11. Determination of dextrose equivalent value and number average molecular weight of maltodextrin by osmometry.

    Science.gov (United States)

    Rong, Y; Sillick, M; Gregson, C M

    2009-01-01

    Dextrose equivalent (DE) value is the most common parameter used to characterize the molecular weight of maltodextrins. Its theoretical value is inversely proportional to number average molecular weight (M(n)), providing a theoretical basis for correlations with physical properties important to food manufacturing, such as: hygroscopicity, the glass transition temperature, and colligative properties. The use of freezing point osmometry to measure DE and M(n) was assessed. Measurements were made on a homologous series of malto-oligomers as well as a variety of commercially available maltodextrin products with DE values ranging from 5 to 18. Results on malto-oligomer samples confirmed that freezing point osmometry provided a linear response with number average molecular weight. However, noncarbohydrate species in some commercial maltodextrin products were found to be in high enough concentration to interfere appreciably with DE measurement. Energy dispersive spectroscopy showed that sodium and chloride were the major ions present in most commercial samples. Osmolality was successfully corrected using conductivity measurements to estimate ion concentrations. The conductivity correction factor appeared to be dependent on the concentration of maltodextrin. Equations were developed to calculate corrected values of DE and M(n) based on measurements of osmolality, conductivity, and maltodextrin concentration. This study builds upon previously reported results through the identification of the major interfering ions and provides an osmolality correction factor that successfully accounts for the influence of maltodextrin concentration on the conductivity measurement. The resulting technique was found to be rapid, robust, and required no reagents.

  12. Technical Note: On methodologies for determining the size-normalised weight of planktic foraminifera

    Directory of Open Access Journals (Sweden)

    C. J. Beer

    2010-07-01

    Full Text Available The size-normalised weight (SNW of planktic foraminifera, a measure of test wall thickness and density, is potentially a valuable palaeo-proxy for marine carbon chemistry. As increasing attention is given to developing this proxy it is important that methods are comparable between studies. Here, we compare SNW data generated using two different methods to account for variability in test size, namely (i the narrow (50 μm range sieve fraction method and (ii the individually measured test size method. Using specimens from the 200–250 μm sieve fraction range collected in multinet samples from the North Atlantic, we find that sieving does not constrain size sufficiently well to isolate changes in weight driven by variations in test wall thickness and density from those driven by size. We estimate that the SNW data produced as part of this study are associated with an uncertainty, or error bar, of about ±11%. Errors associated with the narrow sieve fraction method may be reduced by decreasing the size of the sieve window, by using larger tests and by increasing the number tests employed. In situations where numerous large tests are unavailable, however, substantial errors associated with this sieve method remain unavoidable. In such circumstances the individually measured test size method provides a better means for estimating SNW because, as our results show, this method isolates changes in weight driven by variations in test wall thickness and density from those driven by size.

  13. Low birth weight at term and its determinants in a tertiary hospital of Nepal: a case-control study.

    Directory of Open Access Journals (Sweden)

    Sudesh Raj Sharma

    Full Text Available Birth weight of a child is an important indicator of its vulnerability for childhood illness and chances of survival. A large number of infant deaths can be averted by appropriate management of low birth weight babies and prevention of factors associated with low birth weight. The prevalence of low birth weight babies in Nepal is estimated to be about 12-32%.Our study aimed at identifying major determinants of low birth weight among term babies in Nepal. A hospital-based retrospective case control study was conducted in maternity ward of Tribhuvan University Teaching Hospital from February to July 2011. A total of 155 LBW babies and 310 controls were included in the study. Mothers admitted to maternity ward during the study period were interviewed, medical records were assessed and anthropometric measurements were done. Risk factors, broadly classified into proximal and distal factors, were assessed for any association with birth of low-birth weight babies. Regression analysis revealed that a history of premature delivery (adjusted odds ratio; aOR5.24, CI 1.05-26.28, hard physical work during pregnancy (aOR1.48, CI 0.97-2.26, younger age of mother (aOR1.98, CI 1.15-3.41, mothers with haemoglobin level less than 11gm/dl (aOR0.51, CI0.24-1.07 and lack of consumption of nutritious food during pregnancy (aOR1.99, CI 1.28-3.10 were significantly associated with the birth of LBW babies. These factors should be addressed with appropriate measures so as to decrease the prevalence of low birth weight among term babies in Nepal.

  14. An objective approach to determining the weight ranges of prey preferred by and accessible to the five large African carnivores.

    Directory of Open Access Journals (Sweden)

    Hayley S Clements

    Full Text Available Broad-scale models describing predator prey preferences serve as useful departure points for understanding predator-prey interactions at finer scales. Previous analyses used a subjective approach to identify prey weight preferences of the five large African carnivores, hence their accuracy is questionable. This study uses a segmented model of prey weight versus prey preference to objectively quantify the prey weight preferences of the five large African carnivores. Based on simulations of known predator prey preference, for prey species sample sizes above 32 the segmented model approach detects up to four known changes in prey weight preference (represented by model break-points with high rates of detection (75% to 100% of simulations, depending on number of break-points and accuracy (within 1.3±4.0 to 2.7±4.4 of known break-point. When applied to the five large African carnivores, using carnivore diet information from across Africa, the model detected weight ranges of prey that are preferred, killed relative to their abundance, and avoided by each carnivore. Prey in the weight ranges preferred and killed relative to their abundance are together termed "accessible prey". Accessible prey weight ranges were found to be 14-135 kg for cheetah Acinonyx jubatus, 1-45 kg for leopard Panthera pardus, 32-632 kg for lion Panthera leo, 15-1600 kg for spotted hyaena Crocuta crocuta and 10-289 kg for wild dog Lycaon pictus. An assessment of carnivore diets throughout Africa found these accessible prey weight ranges include 88±2% (cheetah, 82±3% (leopard, 81±2% (lion, 97±2% (spotted hyaena and 96±2% (wild dog of kills. These descriptions of prey weight preferences therefore contribute to our understanding of the diet spectrum of the five large African carnivores. Where datasets meet the minimum sample size requirements, the segmented model approach provides a means of determining, and comparing, the prey weight range preferences of any carnivore

  15. Determinants of Weight Loss following Laparoscopic Sleeve Gastrectomy: The Role of Psychological Burden, Coping Style, and Motivation to Undergo Surgery

    Directory of Open Access Journals (Sweden)

    Andrea Figura

    2015-01-01

    Full Text Available Background. The amount of excess weight loss (%EWL among obese patients after bariatric surgery varies greatly. However, reliable predictors have not been established yet. The present study evaluated the preoperative psychological burden, coping style, and motivation to lose weight as factors determining postoperative treatment success. Methods. The sample included 64 morbidly obese patients with a preoperative BMI of 51±8 kg/m2 who had undergone laparoscopic sleeve gastrectomy (LSG. Well-established questionnaires were applied before surgery to assess the psychological burden in terms of “perceived stress” (PSQ-20, “depression” (PHQ-9, “anxiety” (GAD-7, and “mental impairment” (ISR as well as coping style (Brief COPE and motivation to lose weight. %EWL as an indicator for treatment success was assessed on average 20 months after surgery. Results. Based on the %EWL distribution, patients were classified into three %EWL groups: low (14–39%, moderate (40–59%, and high (60–115%. LSG patients with high %EWL reported significantly more “active coping” behavior prior to surgery than patients with moderate and low %EWL. Patients’ preoperative psychological burden and motivation to lose weight were not associated with %EWL. Conclusion. An “active coping” style might be of predictive value for better weight loss outcomes in patients following LSG intervention.

  16. Rapid determination of lead and cadmium in sewage sludge samples using electrothermal atomic absorption spectrometry with slurry sample introduction

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Vinas, P.; Arroyo-Cortez, J.; Hernandez-Cordoba, M. [Dept. of Analytical Chem., Univ. of Murcia (Spain)

    2000-08-01

    Lead and cadmium concentrations in sewage sludge samples are determined by suspending the ground samples in a solution containing 10% (v/v) concentrated hydrofluoric acid, 1% (v/v) concentrated nitric acid, 0.5% (m/v) dihydrogen ammonium phosphate and 0.1% (m/v) sodium hexametaphosphate. Aliquots of 20 {mu}L of these suspensions (4 mg/mL) are diluted to 1000 {mu}L with the same solution and then injected into the electrothermal atomizer. The drying stage is performed by programming a 400 C temperature, a ramp time of 20 s and a hold time of 15 s on the power supply of the atomizer. No ashing step is used. Platform atomization is carried out at 1600 and 1800 C for Pb and Cd, respectively. Calibration is performed using aqueous standards in the 5-75 and 0.2- 5 {mu}g/L Pb and Cd ranges, respectively. Results obtained for three certified reference materials and four samples demonstrate the reliability of the procedures described. (orig.)

  17. Nickel and strontium nitrates as modifiers for the determination of selenium in wine by Zeeman electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Cvetković, J; Stafilov, T; Mihajlović, D

    2001-08-01

    A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 degrees C and 800 degrees C were chosen for aqueous and organic solutions, respectively; 2700 degrees C and 2100 degrees C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 degrees C and 1600 degrees C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 microg L(-1).

  18. Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2008-01-01

    Full Text Available A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU, copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4 of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

  19. Determining Nuclear Fingerprints: Glove Boxes, Radiation Protection, and the International Atomic Energy Agency.

    Science.gov (United States)

    Rentetzi, Maria

    2017-06-01

    In a nuclear laboratory, a glove box is a windowed, sealed container equipped with two flexible gloves that allow the user to manipulate nuclear materials from the outside in an ostensibly safe environment. As a routine laboratory device, it invites neglect from historians and storytellers of science. Yet, since especially the Gulf War, glove boxes have put the interdependence of science, diplomacy, and politics into clear relief. Standing at the intersection of history of science and international history, technological materials and devices such as the glove box can provide penetrating insight into the role of international diplomatic organizations to the global circulation and control of scientific knowledge. The focus here is on the International Atomic Energy Agency. Copyright © 2017 The Author. Published by Elsevier Ltd.. All rights reserved.

  20. Atmospheric reactions of methylcyclohexanes with Cl atoms and OH radicals: determination of rate coefficients and degradation products.

    Science.gov (United States)

    Ballesteros, Bernabé; Ceacero-Vega, Antonio A; Jiménez, Elena; Albaladejo, José

    2015-04-01

    As the result of biogenic and anthropogenic activities, large quantities of chemical compounds are emitted into the troposphere. Alkanes, in general, and cycloalkanes are an important chemical class of hydrocarbons found in diesel, jet and gasoline, vehicle exhaust emissions, and ambient air in urban areas. In general, the primary atmospheric fate of organic compounds in the gas phase is the reaction with hydroxyl radicals (OH). The oxidation by Cl atoms has gained importance in the study of atmospheric reactions because they may exert some influence in the boundary layer, particularly in marine and coastal environments, and in the Arctic troposphere. The aim of this paper is to study of the atmospheric reactivity of methylcylohexanes with Cl atoms and OH radicals under atmospheric conditions (in air at room temperature and pressure). Relative kinetic techniques have been used to determine the rate coefficients for the reaction of Cl atoms and OH radicals with methylcyclohexane, cis-1,4-dimethylcyclohexane, trans-1,4-dimethylcyclohexane, and 1,3,5-trimethylcyclohexane at 298 ± 2 K and 720 ± 5 Torr of air by Fourier transform infrared) spectroscopy and gas chromatography-mass spectrometry (GC-MS) in two atmospheric simulation chambers. The products formed in the reaction under atmospheric conditions were investigated using a 200-L Teflon bag and employing the technique of solid-phase microextraction coupled to a GC-MS. The rate coefficients obtained for the reaction of Cl atoms with the studied compounds are the following ones (in units of 10(-10) cm(3) molecule(-1) s(-1)): (3.11 ± 0.16), (2.89 ± 0.16), (2.89 ± 0.26), and (2.61 ± 0.42), respectively. For the reactions with OH radicals the determined rate coefficients are (in units of 10(-11) cm(3) molecule(-1) s(-1)): (1.18 ± 0.12), (1.49 ± 0.16), (1.41 ± 0.15), and (1.77 ± 0.23), respectively. The reported error is twice the standard deviation. A detailed

  1. Determining the band gap and mean kinetic energy of atoms from reflection electron energy loss spectra

    Energy Technology Data Exchange (ETDEWEB)

    Vos, M. [Atomic and Molecular Physics Laboratories, Research School of Physics and Engineering, Australian National University, Canberra ACT (Australia); Marmitt, G. G. [Atomic and Molecular Physics Laboratories, Research School of Physics and Engineering, Australian National University, Canberra ACT (Australia); Instituto de Fisica da Universidade Federal do Rio Grande do Sul, Avenida Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Finkelstein, Y. [Nuclear Research Center — Negev, Beer-Sheva 84190 (Israel); Moreh, R. [Physics Department, Ben-Gurion University of the Negev, Beer-Sheva 84105 (Israel)

    2015-09-14

    Reflection electron energy loss spectra from some insulating materials (CaCO{sub 3}, Li{sub 2}CO{sub 3}, and SiO{sub 2}) taken at relatively high incoming electron energies (5–40 keV) are analyzed. Here, one is bulk sensitive and a well-defined onset of inelastic excitations is observed from which one can infer the value of the band gap. An estimate of the band gap was obtained by fitting the spectra with a procedure that includes the recoil shift and recoil broadening affecting these measurements. The width of the elastic peak is directly connected to the mean kinetic energy of the atom in the material (Doppler broadening). The experimentally obtained mean kinetic energies of the O, C, Li, Ca, and Si atoms are compared with the calculated ones, and good agreement is found, especially if the effect of multiple scattering is taken into account. It is demonstrated experimentally that the onset of the inelastic excitation is also affected by Doppler broadening. Aided by this understanding, we can obtain a good fit of the elastic peak and the onset of inelastic excitations. For SiO{sub 2}, good agreement is obtained with the well-established value of the band gap (8.9 eV) only if it is assumed that the intensity near the edge scales as (E − E{sub gap}){sup 1.5}. For CaCO{sub 3}, the band gap obtained here (7 eV) is about 1 eV larger than the previous experimental value, whereas the value for Li{sub 2}CO{sub 3} (7.5 eV) is the first experimental estimate.

  2. Determination of total tin in canned food using inductively coupled plasma atomic emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Perring, Loic; Basic-Dvorzak, Marija [Department of Quality and Safety Assurance, Nestle Research Centre, P.O. Box 44, Vers chez-les-Blanc, 1000, Lausanne (Switzerland)

    2002-09-01

    Tin is considered to be a priority contaminant by the Codex Alimentarius Commission. Tin can enter foods either from natural sources, environmental pollution, packaging material or pesticides. Higher concentrations are found in processed food and canned foods. Dissolution of the tinplate depends on the of food matrix, acidity, presence of oxidising reagents (anthocyanin, nitrate, iron and copper) presence of air (oxygen) in the headspace, time and storage temperature. To reduce corrosion and dissolution of tin, nowadays cans are usually lacquered, which gives a marked reduction of tin migration into the food product. Due to the lack of modern validated published methods for food products, an ICP-AES (Inductively coupled plasma-atomic emission spectroscopy) method has been developed and evaluated. This technique is available in many laboratories in the food industry and is more sensitive than atomic absorption. Conditions of sample preparation and spectroscopic parameters for tin measurement by axial ICP-AES were investigated for their ruggedness. Two methods of preparation involving high-pressure ashing or microwave digestion in volumetric flasks were evaluated. They gave complete recovery of tin with similar accuracy and precision. Recoveries of tin from spiked products with two levels of tin were in the range 99{+-}5%. Robust relative repeatabilities and intermediate reproducibilities were <5% for different food matrices containing >30 mg/kg of tin. Internal standard correction (indium or strontium) did not improve the method performance. Three emission lines for tin were tested (189.927, 283.998 and 235.485 nm) but only 189.927 nm was found to be robust enough with respect to interferences, especially at low tin concentrations. The LOQ (limit of quantification) was around 0.8 mg/kg at 189.927 nm. A survey of tin content in a range of canned foods is given. (orig.)

  3. Direct determination of the atomic mass difference of Re187 and Os187 for neutrino physics and cosmochronology

    CERN Document Server

    Nesterenko, D A; Blaum, K; Block, M; Chenmarev, S; Doerr, A; Droese, C; Filianin, P E; Goncharov, M; Ramirez, E Minaya; Novikov, Yu N; Schweikhard, L; Simon, V V

    2016-01-01

    For the first time a direct determination of the atomic mass difference of 187Re and 187Os has been performed with the Penning-trap mass spectrometer SHIPTRAP applying the novel phase-imaging ion-cyclotron-resonance technique. The obtained value of 2492(30stat)(15sys) eV is in excellent agreement with the Q values determined indirectly with microcalorimetry and thus resolves a long-standing discrepancy with older proportional counter measurements. This is essential for the determination of the neutrino mass from the beta-decay of 187Re as planned in future microcalorimetric measurements. In addition, an accurate mass difference of 187Re and 187Os is also important for the assessment of 187Re for cosmochronology.

  4. Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

    Science.gov (United States)

    Viets, J.G.

    1978-01-01

    Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

  5. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Science.gov (United States)

    Angeli, Valeria; Biagi, Simona; Ghimenti, Silvia; Onor, Massimo; D'Ulivo, Alessandro; Bramanti, Emilia

    2011-11-01

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H 2 miniaturized flame after sodium borohydride reduction to Hg 0, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H 2 microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10 - 5 mol L - 1 ), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L - 1 (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 μmol L - 1 were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were never less than 91%. Flow injection

  6. Chromium speciation by solid phase extraction on Dowex M 4195 chelating resin and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saygi, Kadriye Ozlem; Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)], E-mail: msoylak@gmail.com; Elci, Latif [Pamukkale University, Faculty of Science and Arts, Chemistry Department, 20020 Denizli (Turkey)

    2008-05-30

    A solid phase extraction procedure has been established for chromium speciation in natural water samples prior to determination by atomic absorption spectrometry. The procedure is based on the solid phase extraction of the Cr(VI)- Dowex M 4195 chelating resin. After oxidation of Cr(III) to Cr(VI) by using H{sub 2}O{sub 2}, the presented method was applied to the determination of the total chromium. The level of Cr(III) is calculated by difference of total chromium and Cr(VI) levels. The procedure was optimized for some analytical parameters including pH, eluent type, flow rates of sample and eluent, matrix effects, etc. The presented method was applied for the speciation of chromium in natural water samples with satisfactory results (recoveries >95%, RSDs <10%). In the determinations of chromium species, flame atomic absorption spectrometer was used. The results were checked by using NIST SRM 2711 Montana soil and GBW 07603 Bush branched and leaves.

  7. Determination of lead in wine and rum samples by flow injection-hydride generation-atomic absorption spectrometry.

    Science.gov (United States)

    Elçi, Latif; Arslan, Zikri; Tyson, Julian F

    2009-03-15

    A method for direct determination of lead in wine and rum samples was developed, using a flow injection hydride generation system coupled to an atomic absorption spectrometer with flame-quartz atomizer (FI-HG-AAS). Lead hyride (PbH(4)) was generated using potassium ferricyanide (K(3)Fe(CN)(6)), as oxidant and sodium tetrahydroborate (NaBH(4)) as reductant. Samples were acidified to 0.40% (v/v) HCl for wine and to 0.30% (v/v) HCl for rum, which were then mixed on-line with 3% (m/v) K(3)Fe(CN)(6) solution in 0.03% (v/v) HCl prior to reaction with 0.2% (m/v) alkaline NaBH(4) solution. Lead contents of a rum and two different red wine samples were determined by FI-HG-AAS agreed with those obtained by ICP-MS. The analytical figures of merit of method developed were determined. The calibration curve was linear up to 8.0 microg L(-1) Pb with a regression coefficient of 0.998. The relative error was lower than 4.58%. The relative standard deviation (n=7) was better than 12%. A detection limit of 0.16 microg L(-1) was achieved for a sample volume of 170 microL.

  8. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dancsak, Stacia E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Silva, Sidnei G.; Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2014-01-02

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg{sup −1}. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg{sup −1} for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg{sup −1} for Na and K, and between 0.22 and 0.43 mg kg{sup −1} for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated

  9. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    OpenAIRE

    Andrada,Daniel; Pinto,Frederico G.; Magalhães, Cristina Gonçalves; Nunes,Berta R.; Franco,Milton B.; Silva,José Bento Borba da

    2006-01-01

    The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cup...

  10. An abbreviated fire-assay atomic-absorption method for the determination of gold and silver in ores and concentrates.

    Science.gov (United States)

    Moloughney, P E

    1977-02-01

    A simplified scheme, combining aspects of the classical fire-assay with an atomic-absorption finish, is presented for the determination of gold and silver in ores and concentrates. The lead assay button is scorified to approximately 2 g and then parted in nitric acid. The filtrate is analysed by AAS for silver; the residue is dissolved in aqua regia and subsequently analysed for gold by AAS. The precision and accuracy of the method have been established by application to four diverse certified reference materials. The proposed method eliminates the need for such time-consuming steps as inquartation, multiple scorifications, and cupellation.

  11. Determination of the fine structure constant based on BLOCH oscillations of ultracold atoms in a vertical optical lattice.

    Science.gov (United States)

    Cladé, Pierre; de Mirandes, Estefania; Cadoret, Malo; Guellati-Khélifa, Saïda; Schwob, Catherine; Nez, François; Julien, Lucile; Biraben, François

    2006-01-27

    We report an accurate measurement of the recoil velocity of 87Rb atoms based on Bloch oscillations in a vertical accelerated optical lattice. We transfer about 900 recoil momenta with an efficiency of 99.97% per recoil. A set of 72 measurements of the recoil velocity, each one with a relative uncertainty of about 33 ppb in 20 min integration time, leads to a determination of the fine structure constant with a statistical relative uncertainty of 4.4 ppb. The detailed analysis of the different systematic errors yields to a relative uncertainty of 6.7 ppb. The deduced value of alpha-1 is 137.035 998 78(91).

  12. [Determination of Pb and Al in blood and hair of child using transverse heated graphite furnace atomic absorption spectroscopy].

    Science.gov (United States)

    Niu, Feng-lan; Xie, Wen-bing; Li, Chen-xu; Dong, Wei-yan

    2005-04-01

    Pb and Al in blood and hair of child were determined by transverse heated graphite furnace atomic absorption spectrometry with NH4H2PO4 and Mg(NO3)2 as a modifier, which enhanced the temperature of ashing, eliminated the matrix interference and memorial effect. The method is rapid, simple and accurate. The characteristic mass of the method was 2.3 x 10(-11) g and 2.2 x 10(-11) g for Pb and Al respectively. The relative standard deviation of Pb and Al was 3.0% and 11.4%, respectively, and the recovery was 96%-102%.

  13. Total uncertainty budget calculation for the determination of mercury in incineration ash (BCR 176R) by atomic fluorescence spectrometry.

    Science.gov (United States)

    Tirez, Kristof; Beutels, Filip; Brusten, Wilfried; Noten, Bart; De Brucker, Nicole

    2002-11-01

    The mercury mass fraction has been determined by atomic fluorescence spectrometry (AFS) in the framework of the project "Certification of a reference material (trace elements in fly ash) in replacement of BCR CRM 176". Calculation of the uncertainty budget, as described in this manuscript, emphasizes a practical and realistic approach to estimation of uncertainty components on the basis of statistical assumptions. GUM Workbench software was used, and resulted in a mercury mass fraction of 1.58+/-0.11 mg kg(-1) (with coverage factor k=2.2, 95% probability) related to dry mass, submitted in the certification exercise. The calculated total uncertainty budget applies to analogous samples analyzed by this procedure.

  14. Practical application of failure criteria in determining safe mud weight windows in drilling operations

    Institute of Scientific and Technical Information of China (English)

    R. Gholami; A. Moradzadeh; V. Rasouli; J. Hanachi

    2014-01-01

    Wellbore instability is reported frequently as one of the most significant incidents during drilling oper-ations. Analysis of wellbore instability includes estimation of formation mechanical properties and the state of in situ stresses. In this analysis, the only controllable parameter during drilling operation is the mud weight. If the mud weight is larger than anticipated, the mud will invade into the formation, causing tensile failure of the formation. On the other hand, a lower mud weight can result in shear failures of rock, which is known as borehole breakouts. To predict the potential for failures around the wellbore during drilling, one should use a failure criterion to compare the rock strength against induced tangen-tial stresses around the wellbore at a given mud pressure. The Mohr-Coulomb failure criterion is one of the commonly accepted criteria for estimation of rock strength at a given state of stress. However, the use of other criteria has been debated in the literature. In this paper, Mohr-Coulomb, Hoek-Brown and Mogi-Coulomb failure criteria were used to estimate the potential rock failure around a wellbore located in an onshore field of Iran. The log based analysis was used to estimate rock mechanical proper-ties of formations and state of stresses. The results indicated that amongst different failure criteria, the Mohr-Coulomb criterion underestimates the highest mud pressure required to avoid breakouts around the wellbore. It also predicts a lower fracture gradient pressure. In addition, it was found that the results obtained from Mogi-Coulomb criterion yield a better comparison with breakouts observed from the caliper logs than that of Hoek-Brown criterion. It was concluded that the Mogi-Coulomb criterion is a better failure criterion as it considers the effect of the intermediate principal stress component in the failure analysis.

  15. Practical application of failure criteria in determining safe mud weight windows in drilling operations

    Directory of Open Access Journals (Sweden)

    R. Gholami

    2014-02-01

    Full Text Available Wellbore instability is reported frequently as one of the most significant incidents during drilling operations. Analysis of wellbore instability includes estimation of formation mechanical properties and the state of in situ stresses. In this analysis, the only controllable parameter during drilling operation is the mud weight. If the mud weight is larger than anticipated, the mud will invade into the formation, causing tensile failure of the formation. On the other hand, a lower mud weight can result in shear failures of rock, which is known as borehole breakouts. To predict the potential for failures around the wellbore during drilling, one should use a failure criterion to compare the rock strength against induced tangential stresses around the wellbore at a given mud pressure. The Mohr–Coulomb failure criterion is one of the commonly accepted criteria for estimation of rock strength at a given state of stress. However, the use of other criteria has been debated in the literature. In this paper, Mohr–Coulomb, Hoek–Brown and Mogi–Coulomb failure criteria were used to estimate the potential rock failure around a wellbore located in an onshore field of Iran. The log based analysis was used to estimate rock mechanical properties of formations and state of stresses. The results indicated that amongst different failure criteria, the Mohr–Coulomb criterion underestimates the highest mud pressure required to avoid breakouts around the wellbore. It also predicts a lower fracture gradient pressure. In addition, it was found that the results obtained from Mogi–Coulomb criterion yield a better comparison with breakouts observed from the caliper logs than that of Hoek–Brown criterion. It was concluded that the Mogi–Coulomb criterion is a better failure criterion as it considers the effect of the intermediate principal stress component in the failure analysis.

  16. Methodology for determining of the weighted mean coolant temperature in the primary circuit hot legs of WWER-1000 reactor plants

    Energy Technology Data Exchange (ETDEWEB)

    Saunin, Yuri V.; Dobrotvorski, Alexander N.; Semenikhin, Alexander V. [JSC ' Atomtechenergo' , Filial ' Novovoronezhatomtechenergo' , Novovorenezh (Russian Federation); Ryasny, Sergei I. [JSC ' Atomtechenergo' , Mytishi (Russian Federation)

    2016-09-15

    At WWER-1000 NPPs, as well as at PWR NPPs, there is a problem of determining the correct weighted mean coolant temperature in the primary circuit hot legs based on the measuring channels information. The problem is caused by the coolant temperature stratification. The technical documentation for engineering support and maintenance of I and C systems does not provide any regulatory guidelines to consider this effect. Therefore, it is very important to represent a new methodology for determining the weighted mean coolant temperature in the primary circuit hot legs of the WWER-1000 reactor plants. The given paper presents the basic preconditions and approaches applied during the methodology development. They were worked out on the basis of the executed numerical and experimental research taking into account the analysis of the extensive material obtained by the authors from full-scale tests during the commissioning of WWER-1000 power units, as well as operational data obtained from several power units with different fuel loadings.

  17. Food availability as a determinant of weight gain among renal transplant recipients.

    Science.gov (United States)

    Bloodworth, Robin F; Ward, Kenneth D; Relyea, George E; Cashion, Ann K

    2014-06-01

    Excessive weight gain is common after renal transplantation, but it is unknown whether environmental factors, such as food availability, contribute to this important clinical problem. We evaluated the effects of food availability (fast food restaurants, convenience stores, and grocery stores within 1, 2, and 3 mile buffers of transplant recipients' residences) on body mass index (BMI) change during the first year post-transplant. Participants (n = 299) resided in Memphis, Tennessee. BMI increased by 1.42 units (p restaurants and convenience stores were not significantly associated with BMI change.

  18. Determination of trace lead in rice of sewage irrigation by graphite furnace atomic-absorption spectrometry

    Institute of Scientific and Technical Information of China (English)

    JIXueping; RENJujie

    1994-01-01

    The early literatures reported that a lot of matrix interference were encounted in the determination of lend content in various samples. Chlorides produced serious interference on analysis of lead content. All acids except phosphoric acid reduced sensitivity of determination of Pb. Hinderberger et al.

  19. Laboratory installation for the study of atomic-oxygen and ozone detectors and certain methodological aspects concerning the determination of oxygen-atom concentration by the methods of NO and NO2 titration

    Science.gov (United States)

    Bromberg, D. V.; Perov, S. P.

    A laboratory installation is described which can be used to study various characteristics of atomic oxygen and ozone in the pressure range from 0.01 to 50 Pa. The installation can be used to calibrate rocketborne sensors intended for measurements in the middle atmosphere. Systematic and random errors connected with the determination of oxygen-atom concentration by the NO2 and NO titration methods are examined.

  20. A method for determining weights for excess relative risk and excess absolute risk when applied in the calculation of lifetime risk of cancer from radiation exposure

    Energy Technology Data Exchange (ETDEWEB)

    Walsh, Linda [Federal Office for Radiation Protection, Department of Radiation Protection and Health, Oberschleissheim (Germany); University of Manchester, The Faculty of Medical and Human Sciences, Manchester (United Kingdom); Schneider, Uwe [University of Zurich, Vetsuisse Faculty, Zurich (Switzerland); Radiotherapy Hirslanden AG, Aarau (Switzerland)

    2013-03-15

    Radiation-related risks of cancer can be transported from one population to another population at risk, for the purpose of calculating lifetime risks from radiation exposure. Transfer via excess relative risks (ERR) or excess absolute risks (EAR) or a mixture of both (i.e., from the life span study (LSS) of Japanese atomic bomb survivors) has been done in the past based on qualitative weighting. Consequently, the values of the weights applied and the method of application of the weights (i.e., as additive or geometric weighted means) have varied both between reports produced at different times by the same regulatory body and also between reports produced at similar times by different regulatory bodies. Since the gender and age patterns are often markedly different between EAR and ERR models, it is useful to have an evidence-based method for determining the relative goodness of fit of such models to the data. This paper identifies a method, using Akaike model weights, which could aid expert judgment and be applied to help to achieve consistency of approach and quantitative evidence-based results in future health risk assessments. The results of applying this method to recent LSS cancer incidence models are that the relative EAR weighting by cancer solid cancer site, on a scale of 0-1, is zero for breast and colon, 0.02 for all solid, 0.03 for lung, 0.08 for liver, 0.15 for thyroid, 0.18 for bladder and 0.93 for stomach. The EAR weighting for female breast cancer increases from 0 to 0.3, if a generally observed change in the trend between female age-specific breast cancer incidence rates and attained age, associated with menopause, is accounted for in the EAR model. Application of this method to preferred models from a study of multi-model inference from many models fitted to the LSS leukemia mortality data, results in an EAR weighting of 0. From these results it can be seen that lifetime risk transfer is most highly weighted by EAR only for stomach cancer. However

  1. Maternal factors associated with fetal growth and birthweight are independent determinants of placental weight and exhibit differential effects by fetal sex.

    Directory of Open Access Journals (Sweden)

    Marie Cecilie Paasche Roland

    Full Text Available INTRODUCTION: Maternal nutritional and metabolic factors influence the developmental environment of the fetus. Virtually any nutritional factor in the maternal blood has to pass the placental membranes to reach the fetal blood. Placental weight is a commonly used measure to summarize placental growth and function. Placental weight is an independent determinant of fetal growth and birthweight and modifies the associations between maternal metabolic factors and fetal growth. We hypothesized that maternal factors known to be related to fetal growth, newborn size and body composition are determinants of placental weight and that effects of maternal metabolic factors on placental weight differ between the genders. METHODS: The STORK study is a prospective longitudinal study including 1031 healthy pregnant women of Scandinavian heritage with singleton pregnancies. Maternal determinants (parity, body mass index, gestational weight gain and fasting plasma glucose of placental weight were explored by linear regression models, stratified by fetal sex. RESULTS: Parity, maternal BMI, gestational weight gain and fasting glucose had positive effects on placental weight. There was a sex specific effect in these associations. Fasting glucose was significantly associated with placental weight in females but not in males. CONCLUSION: Maternal factors known to influence fetal growth, birthweight and neonatal body composition are determinants of placental weight. The effect of maternal factors on placental weight is influenced by sex as illustrated in the relation between maternal glucose and placental weight.

  2. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Maranhão, Tatiane De A.; Borges, Daniel L. G.; da Veiga, Márcia A. M. S.; Curtius, Adilson J.

    2005-06-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g-1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  3. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maranhao, Tatiane de A. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)]. E-mail: daniel@qmc.ufsc.br; Veiga, Marcia A.M.S. da [Instituto de Quimica, Universidade de Sao Paulo, 05513-970, CP 26077, Sao Paulo, SP (Brazil); Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil)

    2005-06-30

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 deg. C for both elements and atomization temperatures of 1400 and 1600 deg. C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3{sigma} {sub B}) of 6 and 40 ng g{sup -1}, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H{sub 2}O{sub 2} and HNO{sub 3}. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  4. Simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Zambrzycka-Szelewa, Elżbieta; Lulewicz, Marta; Godlewska-Żyłkiewicz, Beata

    2017-07-01

    In the present paper a fast, simple and sensitive analytical method for simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) was developed. Among six pairs of absorption atomic lines of Rh and Ru, which are close enough to enable their simultaneous detection, two pairs were selected for further studies. Best results were obtained for measurements of the resonance line of rhodium at 343.489 nm and the adjacent secondary line of ruthenium at 343.674 nm (23% intensity of this line). For evaluated lines, the absorbance values were obtained using three pixels. The pyrolysis and atomization temperatures were 1200 °C and 2600 °C, respectively. Under these conditions the limits of detection achieved for Rh and Ru were found to be 1.0 μg L- 1 and 1.9 μg L- 1, respectively. The characteristic mass was 12.9 pg for Rh and 71.7 pg for Ru. Repeatability of the results expressed as a relative standard deviation was typically below 6%. The trueness of the method was confirmed by analysis of the certified reference material - platinum ore (SARM 76). The recovery of Rh and Ru from the platinum ore was 93.0 ± 4.6% and 90.1 ± 2.5%, respectively. The method was successfully applied to the direct simultaneous determination of trace amounts of rhodium and ruthenium in spiked river water, road runoff, and municipal sewage. Separation of interfering matrix on cation exchange resin was required before analysis of road dust and tunnel dust (CW-7) by HR-CS GFAAS.

  5. Determination of mercury by cold vapor atomic absorption spectrophotometer in Tongkat Ali preparations obtained in Malaysia.

    Science.gov (United States)

    Ang, Hooi-Hoon; Lee, Ee-Lin; Cheang, Hui-Seong

    2004-01-01

    The DCA (Drug Control Authority), Malaysia, has implemented the phase 3 registration of traditional medicines on 1 January 1992, with special emphasis on the quality, efficacy, and safety (including the presence of heavy metals) in all pharmaceutical dosage forms of traditional medicine preparations. As such, a total of 100 products in various pharmaceutical dosage forms of a herbal preparation, containing Tongkat Ali, were analyzed for mercury content using cold vapor atomic absorption spectrophotometer. Results showed that 36% of the above products possessed 0.52 to 5.30 ppm of mercury and, therefore, do not comply with the quality requirement for traditional medicines in Malaysia. Out of these 36 products, 5 products that possessed 1.05 to 4.41 ppm of mercury were in fact have already registered with the DCA, Malaysia. However, the rest of the products that contain 0.52 to 5.30 ppm of mercury still have not registered with the DCA, Malaysia. Although this study showed that only 64% of the products complied with the quality requirement for traditional medicines in Malaysia pertaining to mercury, they cannot be assumed safe from mercury contamination because of batch-to-batch inconsistency.

  6. Water replacement hypothesis in atomic detail--factors determining the structure of dehydrated bilayer stacks.

    Science.gov (United States)

    Golovina, Elena A; Golovin, Andrey V; Hoekstra, Folkert A; Faller, Roland

    2009-07-22

    According to the water replacement hypothesis, trehalose stabilizes dry membranes by preventing the decrease of spacing between membrane lipids under dehydration. In this study, we use molecular-dynamics simulations to investigate the influence of trehalose on the area per lipid (APL) and related structural properties of dehydrated bilayers in atomic detail. The starting conformation of a palmitoyloleolylphosphatidylcholine lipid bilayer in excess water was been obtained by self-assembly. A series of molecular-dynamics simulations of palmitoyloleolylphosphatidylcholine with different degrees of dehydration (28.5, 11.7, and 5.4 waters per lipid) and different molar trehalose/lipid ratios (1:1) were carried out in the NPT ensemble. Water removal causes the formation of multilamellar "stacks" through periodic boundary conditions. The headgroups reorient from pointing outward to inward with dehydration. This causes changes in the electrostatic interactions between interfaces, resulting in interface interpenetration. Interpenetration creates self-spacing of the bilayers and prevents gel-phase formation. At lower concentrations, trehalose does not separate the interfaces, and acting together with self-spacing, it causes a considerable increase of APL. APL decreases at higher trehalose concentrations when the layer of sugar physically separates the interfaces. When interfaces are separated, the model confirms the water replacement hypothesis.

  7. Water Replacement Hypothesis in Atomic Detail—Factors Determining the Structure of Dehydrated Bilayer Stacks

    Science.gov (United States)

    Golovina, Elena A.; Golovin, Andrey V.; Hoekstra, Folkert A.; Faller, Roland

    2009-01-01

    Abstract According to the water replacement hypothesis, trehalose stabilizes dry membranes by preventing the decrease of spacing between membrane lipids under dehydration. In this study, we use molecular-dynamics simulations to investigate the influence of trehalose on the area per lipid (APL) and related structural properties of dehydrated bilayers in atomic detail. The starting conformation of a palmitoyloleolylphosphatidylcholine lipid bilayer in excess water was been obtained by self-assembly. A series of molecular-dynamics simulations of palmitoyloleolylphosphatidylcholine with different degrees of dehydration (28.5, 11.7, and 5.4 waters per lipid) and different molar trehalose/lipid ratios (1:1) were carried out in the NPT ensemble. Water removal causes the formation of multilamellar “stacks” through periodic boundary conditions. The headgroups reorient from pointing outward to inward with dehydration. This causes changes in the electrostatic interactions between interfaces, resulting in interface interpenetration. Interpenetration creates self-spacing of the bilayers and prevents gel-phase formation. At lower concentrations, trehalose does not separate the interfaces, and acting together with self-spacing, it causes a considerable increase of APL. APL decreases at higher trehalose concentrations when the layer of sugar physically separates the interfaces. When interfaces are separated, the model confirms the water replacement hypothesis. PMID:19619463

  8. Determination of selenium and tellurium in the gas phase using specific columns and atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Muangnoicharoen, S.; Chiou, K.Y.; Manuel, O.K.

    1986-11-01

    Total selenium and tellurium in the gas phase were analyzed after adsorption on gold-coated beads and charcoal. The thermally eluting gas was trapped on columns filled with quartz beads that were cooled in an ice bath. The beads were boiled in dilute HCl, and the resulting solution was analyzed for Se and Te by graphite furnace atomic absorption spectrometry. Their results demonstrate that gold-coated beads efficiently trap gaseous Se and Te at a low gas flow rate, but at higher flow rates charcoal traps are more expedient. With charcoal traps, it was found that local air samples contain Se in the range of 0.92-3.05 ng m/sup -3/ and Te in the range of 0.10-0.34 ng m/sup -3/. Detection limits down to about 0.1 ng m/sup -3/ allow the ready detection of Se and Te in rural air with a precision of about +/- 6% at the nanogram level of Te and about +/- 4% at the nanogram level of Se.

  9. Determination of toxic metals in some herbal drugs through atomic absorption spectroscopy.

    Science.gov (United States)

    Hina, Bushra; Rizwani, Ghazala Hafeez; Naseem, Shahid

    2011-07-01

    This study presents a picture of occurrence of heavy metals (Pb, Cd, Cu, Cr, Co, Fe, Ni, Zn) in some selected valuable herbal drugs (G. glabra, O. bracteatum, V. odorata , F. vulgare, C. cyminum, C. sativum, and Z. officinalis) purchased from three different zones (southern, eastern, and western) of Karachi city using atomic absorption spectrophotometer. Heavy metal concentrations in these drugs were found in the range of: 3.26-30.46 for Pb, 1.6-4.91 for Cd, 0.65-120.21 for Cu, 83.74-433.76 for Zn, 1.61-186.75 for Cr, 0.48-76.97 for Ni, 5.54-77.97 for Co and 65.68-1652.89 µg/g for Fe. Percentage of heavy metals that were found beyond the permissible limits were: 71.4% for Pb, 28.51% for Cd, 14.2% for Cu, and 9.5 % for Cr. Significant difference was noticed for each heavy metal among herbal drugs as well as their zones of collection using two way ANOVA followed by least significant (LSD) test at p<0.05.Purpose of this research is to detect each type of heavy metal contaminant of herbal drugs by environmental pollution, as well as to highlight the health risks associated with the use of such herbal drugs that contain high levels of toxic heavy metals.

  10. Preconcentration and determination of cadmium in water and food samples by in situ surfactant-based solid-phase extraction and flame atomic absorption spectrometry

    National Research Council Canada - National Science Library

    Jamali, Mohammad Reza; Boromandi, Afsaneh

    2014-01-01

    In situ surfactant-based solid-phase extraction (ISS-SPE) is proposed as a preconcentration procedure for the determination of cadmium in water and food samples by flame atomic absorption spectrometry...

  11. Determination of nanoparticle size distribution together with density or molecular weight by 2D analytical ultracentrifugation

    KAUST Repository

    Carney, Randy P.

    2011-06-07

    Nanoparticles are finding many research and industrial applications, yet their characterization remains a challenge. Their cores are often polydisperse and coated by a stabilizing shell that varies in size and composition. No single technique can characterize both the size distribution and the nature of the shell. Advances in analytical ultracentrifugation allow for the extraction of the sedimentation (s) and diffusion coefficients (D). Here we report an approach to transform the s and D distributions of nanoparticles in solution into precise molecular weight (M), density (?P) and particle diameter (dp) distributions. M for mixtures of discrete nanocrystals is found within 4% of the known quantities. The accuracy and the density information we achieve on nanoparticles are unparalleled. A single experimental run is sufficient for full nanoparticle characterization, without the need for standards or other auxiliary measurements. We believe that our method is of general applicability and we discuss its limitations. 2011 Macmillan Publishers Limited. All rights reserved.

  12. Determination of free inositols and other low molecular weight carbohydrates in vegetables.

    Science.gov (United States)

    Hernández-Hernández, Oswaldo; Ruiz-Aceituno, Laura; Sanz, María Luz; Martínez-Castro, Isabel

    2011-03-23

    Different low molecular weight carbohydrates including saccharides, polyalcohols, sugar acids, and glycosides have been identified and quantified in different edible vegetables from Asteraceae, Amarantaceae, Amarylidaceae, Brassicaceae, Dioscoreaceae, and Solanaceae families by gas chromatography-mass spectrometry. Apart from glucose, fructose, and sucrose, other saccharides such as sedoheptulose in chicory, spinach, cabbage, purple yam, eggplant, radish, and oak leaf lettuce, rutinose in eggplant skin, and a glycosyl-inositol in spinach have been identified. chiro-Inositol was found in all vegetables of the Asteraceae family (3.1-32.6 mg 100 g(-1)), whereas scyllo-inositol was detected in those of purple yam, eggplant, artichoke, chicory, escarole, and endive (traces-23.2 mg 100 g(-1)). α-Galactosides, kestose, glucaric acid, and glycosyl-glycerols were also identified and quantified in some of the analyzed vegetables. Considering the bioactivity of most of these compounds, mainly chicory leaves, artichokes, lettuces, and purple yam could constitute beneficial sources for human health.

  13. Exact Determination of Optimal Weights for Fastest Distributed Consensus Algorithm in Path Network via SDP

    CERN Document Server

    Jafarizadeh, Saber

    2010-01-01

    Providing an analytical solution for the problem of finding Fastest Distributed Consensus (FDC) is one of the challenging problems in the field of sensor networks. Most of the methods proposed so far deal with the FDC averaging algorithm problem by numerical convex optimization methods and in general no closed-form solution for finding FDC has been offered up to now except in [3] where the conjectured answer for path has been proved. Here in this work we present an analytical solution for the problem of Fastest Distributed Consensus for the Path network using semidefinite programming particularly solving the slackness conditions, where the optimal weights are obtained by inductive comparing of the characteristic polynomials initiated by slackness conditions.

  14. Determination of glucose concentration from near-infrared spectra using locally weighted partial least square regression.

    Science.gov (United States)

    Malik, Bilal; Benaissa, Mohammed

    2012-01-01

    This paper proposes the use of locally weighted partial least square regression (LW-PLSR) as an alternative multivariate calibration method for the prediction of glucose concentration from NIR spectra. The efficiency of the proposed model is validated in experiments carried out in a non-controlled environment or sample conditions using mixtures composed of glucose, urea and triacetin. The collected data spans the spectral region from 2100 nm to 2400 nm with spectra resolution of 1 nm. The results show that the standard error of prediction (SEP) decreases to 23.85 mg/dL when using LW-PLSR in comparison to the SEP values of 49.40 mg/dL, and 27.56 mg/dL using Principal Component Regression (PCR) and Partial Least Square (PLS) regression respectively.

  15. Insights and Perspectives on Emerging Inputs to Weight of Evidence Determinations for Food Safety: Workshop Proceedings

    Science.gov (United States)

    Bialk, Heidi; Llewellyn, Craig; Kretser, Alison; Canady, Richard; Lane, Richard; Barach, Jeffrey

    2013-01-01

    This workshop aimed to elucidate the contribution of computational and emerging in vitro methods to the weight of evidence used by risk assessors in food safety assessments. The following issues were discussed: using in silico and high-throughput screening (HTS) data to confirm the safety of approved food ingredients, applying in silico and HTS data in the process of assessing the safety of a new food ingredient, and utilizing in silico and HTS data in communicating the safety of food ingredients while enhancing the public’s trust in the food supply. Perspectives on integrating computational modeling and HTS assays as well as recommendations for optimizing predictive methods for risk assessment were also provided. Given the need to act quickly or proceed cautiously as new data emerge, this workshop also focused on effectively identifying a path forward in communicating in silico and in vitro data. PMID:24296863

  16. Age determination of the nuclear stellar population of Active Galactic Nuclei using Locally Weighted Regression

    CERN Document Server

    Estrada-Piedra, T; Terlevich, R J; Fuentes, O; Terlevich, E; Estrada-Piedra, Trilce; Torres-Papaqui, Juan Pablo; Terlevich, Roberto; Fuentes, Olac; Terlevich, Elena

    2003-01-01

    We present a new technique to segregate old and young stellar populations in galactic spectra using machine learning methods. We used an ensemble of classifiers, each classifier in the ensemble specializes in young or old populations and was trained with locally weighted regression and tested using ten-fold cross-validation. Since the relevant information concentrates in certain regions of the spectra we used the method of sequential floating backward selection offline for feature selection. The application to Seyfert galaxies proved that this technique is very insensitive to the dilution by the Active Galactic Nucleus (AGN) continuum. Comparing with exhaustive search we concluded that both methods are similar in terms of accuracy but the machine learning method is faster by about two orders of magnitude.

  17. Insights and perspectives on emerging inputs to weight of evidence determinations for food safety: workshop proceedings.

    Science.gov (United States)

    Bialk, Heidi; Llewellyn, Craig; Kretser, Alison; Canady, Richard; Lane, Richard; Barach, Jeffrey

    2013-01-01

    This workshop aimed to elucidate the contribution of computational and emerging in vitro methods to the weight of evidence used by risk assessors in food safety assessments. The following issues were discussed: using in silico and high-throughput screening (HTS) data to confirm the safety of approved food ingredients, applying in silico and HTS data in the process of assessing the safety of a new food ingredient, and utilizing in silico and HTS data in communicating the safety of food ingredients while enhancing the public's trust in the food supply. Perspectives on integrating computational modeling and HTS assays as well as recommendations for optimizing predictive methods for risk assessment were also provided. Given the need to act quickly or proceed cautiously as new data emerge, this workshop also focused on effectively identifying a path forward in communicating in silico and in vitro data.

  18. Motor ability and weight status are determinants of out-of-school activity participation for children with developmental coordination disorder.

    Science.gov (United States)

    Fong, Shirley S M; Lee, Velma Y L; Chan, Nerita N C; Chan, Rachel S H; Chak, Wai-Kwong; Pang, Marco Y C

    2011-01-01

    According to the International Classification of Functioning, Disability and Health model endorsed by the World Health Organization, participation in everyday activities is integral to normal child development. However, little is known about the influence of motor ability and weight status on physical activity participation in children with developmental coordination disorder (DCD). This study aimed to (1) compare motor performance, weight status and pattern of out-of-school activity participation between children with DCD and those without; and (2) identify whether motor ability and weight status were determinants of participation patterns among children with DCD. We enrolled 81 children with DCD (boys, n = 63; girls, n = 18; mean age, 8.07 ± 1.5 years) and 67 typically developing children (boys, n = 48; girls, n = 19; mean age, 8.25 ± 1.6 years). Participation patterns (diversity, intensity, companionship, location, and enjoyment) were evaluated with the Children Assessment of Participation and Enjoyment. Motor ability was evaluated with the Movement Assessment Battery for Children, second edition (MABC-2). Other factors that may influence participation such as age, gender, and body weight were also recorded. Analysis of variance was used to compare outcome variables of the two groups, and significant determinants of activity participation were identified by multiple regression analysis. Children with DCD participated in fewer activities (i.e., limited participation diversity) and participated less frequently (i.e., limited participation intensity) than their typically developing peers; however, companionship, location of participation, and enjoyment level did not differ between the two groups. Children in the DCD group demonstrated significantly worse motor ability as assessed by the MABC-2. Further, a greater proportion of children in the DCD group were in the overweight/obese category compared with their typically developing peers. After accounting for the

  19. Application of microemulsions in determination of chromium naphthenate in gasoline by flame atomic absorption spectroscopy.

    Science.gov (United States)

    Du, B; Wei, Q; Wang, S; Yu, W

    1997-10-01

    A new method using microemulsified samples is presented. It is for the determination of chromium naphthenate in gasoline by flame absorption spectroscopy. The method has the advantage of simplicity, speed and the use of aqueous standards for calibration instead of organic standards. Coexistent elements do not disturb the determination. Results obtained by this method were better than those obtained by other methods for the same samples.

  20. Determination of vanadium in urine by electrothermal atomic absorption spectrometry using hot injection and preconcentration into the graphite tube

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, Kelly G.; Nobrega, Joaquim A. [Sao Carlos Univ., SP (Brazil). Dept. de Quimica; Nogueira, Ana Rita A. [Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)]. E-mail: anarita@cppse.embrapa.br; Gomes Neto, Jose A. [UNESP, Araraquara, SP (Brazil). Inst. de Quimica

    2004-10-01

    In this work it was developed a procedure for the determination of vanadium in urine samples by electrothermal atomic absorption spectrometry using successive injections for preconcentration into a preheated graphite tube. Three 60 {mu}L volumes were sequentially injected into the atomizer preheated to a temperature of 110 deg C. Drying and pyrolysis steps were carried out after each injection. A chemical modifier, barium difluoride (100 mg L{sup -1}), and a surfactant, Triton X-100 (0.3% v v{sup -1}), were added to the urine sample. When injecting into a hot graphite tube, the sample flow-rate was 0.5 {mu} s{sup -1}. The limits of detection and quantification were 0.54 and 1.82 without preconcentration, and 0.11 and 0.37 {mu}g L{sup -1} with preconcentration, respectively. The accuracy of the procedure was evaluated by an addition-recovery experiment employing urine samples. Recoveries varied from 96.0 to 103% for additions ranging from 0.8 to 3.5 {mu}g L{sup -1} V. The developed procedure allows the determination of vanadium in urine without any sample pretreatment and with minimal dilution of the sample. (author)

  1. [Determination of trace silver in water samples by solid phase extraction portable tungsten-coil electrothermal atomic absorption spectrometry].

    Science.gov (United States)

    Fan, Guang-yu; Jiang, Xiao-ming; Zheng, Cheng-bin; Hou, Xian-deng; Xu, Kai-lai

    2011-07-01

    A simple method has been developed for the determination of silver in environmental water samples using solid phase extraction with tungsten-coil electrothermal atomic absorption spectrometry. Silica gel was used as an adsorbent and packed into a syringe barrel for solid phase extraction of silver prior to its determination by using a portable tungsten-coil electrothermal atomic absorption spectrometer. Optimum conditions for adsorption and desorption of silver ion, as well as interferences from co-existing ions, were investigated. A sample pH value of 6.0, a sample loading flow rate of 4.0 mL x min(-1), and the mixture of 4% (m/v) thiourea and 2% (phi) nitrate acid with the eluent flow rate of 0.5 mL x min(-1) for desorption were selected for further studies. Under optimal conditions, a linear range of 0.20-4.00 ng x mL(-1), a limit of detection (3sigma) of 0.03 ng x mL(-1) and a preconcentration factor of 94 were achieved. The proposed method was validated by testing three environmental water samples with satisfactory results.

  2. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  3. Coprecipitation of trace amounts of silicon with aluminum hydroxide and the determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2014-01-01

    Full Text Available A simple preconcentration method of silicon based on coprecipitation with aluminum hydroxide prior to its flame atomic absorption (FAAS determination was established. The recovery values of analyte ion was higher than 95%. The parameters including types of hydroxide ion source for precipitation, acid type for dissolution step, amount of aluminum ion as collector, pH, temperature, standing and centrifuge time, and sample volume were optimized for the quantitative recovery of the analyte. The influences of matrix ions were also examined. The relative standard deviation was found to be 3.2%. The limit of detection was calculated as (0.1 mg L-1. The preconcentration factor is 100 for (200 mL solution. The proposed method was successfully applied for the determination of silicon in some water and alloy samples.

  4. Membrane filtration of nickel(II) on cellulose acetate filters for its preconcentration, separation, and flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Soylak, Mustafa [Chemistry Dept., Faculty of Science Arts, University of Erciyes, Kayseri (Turkey); Unsal, Yunus Emre; Aydin, Ayse [Fen Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey); Kizil, Nebiye [Saglik Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey)

    2010-01-15

    An enrichment method for trace amounts of Ni(II), as 8-hydroxyquinoline chelates, has been established on a cellulose acetate membrane filter. Ni(II)-8-hydroxyquinoline chelates adsorbed on a membrane filter were eluted using 5 mL of 1 M HNO{sub 3}. The eluent nickel concentration was determined by a flame atomic absorption spectrometer. The influence of some analytical parameters, including pH, amount of reagent, sample volume, etc., on recovery was investigated. The interference of co-existent ions was studied. The nickel detection limit was 4.87 {mu}g/L. The method was applied to real samples for the determination of nickel(II) ions. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  5. New Atomic Data for Trans-Iron Elements and Their Application to Abundance Determinations in Planetary Nebulae

    CERN Document Server

    Sterling, N C; Esteves, D A; Bilodeau, R C; Kilcoyne, A L D; Red, E C; Phaneuf, R A; Alna'Washi, G; Aguilar, A

    2010-01-01

    [Abridged] Investigations of neutron(n)-capture element nucleosynthesis and chemical evolution have largely been based on stellar spectroscopy. However, the recent detection of these elements in several planetary nebulae (PNe) indicates that nebular spectroscopy is a promising new tool for such studies. In PNe, n-capture element abundance determinations reveal details of s-process nucleosynthesis and convective mixing in evolved low-mass stars, as well as the chemical evolution of elements that cannot be detected in stellar spectra. Only one or two ions of a given trans-iron element can typically be detected in individual nebulae. Elemental abundance determinations thus require corrections for the abundances of unobserved ions. Such corrections rely on the availability of atomic data for processes that control the ionization equilibrium of nebulae. Until recently, these data were unknown for virtually all n-capture element ions. For the first five ions of Se, Kr, and Xe -- the three most widely detected n-cap...

  6. Determination of mercury in estuarine sediments by flow injection-cold vapour atomic absorption spectrometry after microwave extraction

    Energy Technology Data Exchange (ETDEWEB)

    Martinez-Garcia, M.L.; Carlosena, A.; Lopez-Mahia, P.; Muniategui, S.; Prada, D. [University of La Coruna (Spain). Dept. Analytical Chemistry

    1999-01-01

    A flow injection-cold vapour atomic absorption spectrometric (CVAAS) method was developed for the determination of mercury at trace level in estuarine sediments using sodium tetra-hydro-borate (III) as reductant. The mercury was solubilized with nitric acid in closed vessels nd microwave oven heating. Instrumental and operational conditions (volume and concentration of reagents, reaction time, etc.) were optimized. The effect of several ions on the analytical signal was also studied; no interferences were recorded excepting for copper and nickel which caused a serious depressing effect. The detection limit obtained was 0.01 {mu}g g{sup -1}. The validation of the method was performed analyzing a certified reference sediment, BCR CRM 277 Estuarine Sediment. Good recovery (c.a. 98 %) and precision (< 3 %, RSD) were achieved. The proposed method was successfully applied to the determination of mercury in sediment samples from Ares-Betanzos Estuary (Galicia, NW Spain). (authors) 19 refs.

  7. Development of a cloud point extraction and preconcentration method for Cd and Ni prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Manzoori, Jamshid L. [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: manzoori@tabrizu.ac.ir; Karim-Nezhad, Ghasem [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2004-09-13

    In this work a new cloud point extraction (CPE) methodology was developed for the separation and preconcentration of cadmium and nickel. The analyte in the initial aqueous solution was complexed with dithizone and Triton X-114 was added as surfactant. After phase separation, based on the cloud point of the mixture, and dilution of the surfactant-rich phase with tetrahydrofuran (THF), the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions and preconcentration of only 10 ml of sample in the presence of 0.05% Triton X-114, the enhancement factors of 52 and 39 and the detection limits of 0.31 {mu}g l{sup -1} and 1.2 {mu}g l{sup -1} were obtained for cadmium and nickel respectively. The proposed method was applied satisfactorily to the determination of cadmium and nickel in water samples.

  8. Gas temperature determination in an argon non-thermal plasma at atmospheric pressure from broadenings of atomic emission lines

    Science.gov (United States)

    Yubero, C.; Rodero, A.; Dimitrijevic, M. S.; Gamero, A.; García, M. C.

    2017-03-01

    In this work a new spectroscopic method, allowing gas temperature determination in argon non-thermal plasmas sustained at atmospheric pressure, is presented. The method is based on the measurements of selected pairs of argon atomic lines (Ar I 603.2 nm/Ar I 549.6 nm, Ar I 603.2 nm/Ar I 522.1 nm, Ar I 549.6 nm/Ar I 522.1 nm). For gas temperature determination using the proposed method, there is no need of knowing the electron density, neither making assumptions on the degree of thermodynamic equilibrium existing in the plasma. The values of the temperatures obtained using this method, have been compared with the rotational temperatures derived from the OH ro-vibrational bands, using both, the well-known Boltzmann-plot technique and the best fitting to simulated ro-vibrational bands. A very good agreement has been found.

  9. Temperature dependence of viscosity and density of viscous liquids determined from thermal noise spectra of uncalibrated atomic force microscope cantilevers.

    Science.gov (United States)

    McLoughlin, Neal; Lee, Stephen L; Hähner, Georg

    2007-08-01

    We demonstrate that the thermal response of uncalibrated atomic force microscope cantilevers can be used to extract the density and the viscosity of viscous liquids with good accuracy. Temperature dependent thermal noise spectra were measured in water/poly(ethylene glycol) mixtures. Empirical parameters characteristic of the resonance behavior of the system were extracted from data recorded for one of the solutions at room temperature. These parameters were then employed to determine both viscosity and density values of the solutions simultaneously at different temperatures. In addition, activation energies for viscous flow were determined from the viscosity values obtained. The method presented is both fast and reliable and has the potential to be applied in connection with microfluidic systems, making macroscopic amounts of liquid and separate measurements with a viscometer and a densimeter redundant.

  10. Solid phase extraction of gold(III) on Amberlite XAD-2000 prior to its flame atomic absorption spectrometric determination.

    Science.gov (United States)

    Elci, Latif; Sahan, Derya; Basaran, Aydan; Soylak, Mustafa

    2007-09-01

    A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer (FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III) from 1.5 mol l(-1) HCl solution and the recovery of gold with 0.07 mol l(-1) NH3 solution were quantitative (>or=95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 microg l(-1). The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples.

  11. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Science.gov (United States)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

  12. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    Energy Technology Data Exchange (ETDEWEB)

    Kruger, Pamela C. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Parsons, Patrick J. [Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, P.O. Box 509, Albany, NY 12201-0509 (United States); Lead Poisoning/Trace Elements Laboratory, Wadsworth Center, New York State Department of Health, P.O. Box 509, Albany, NY 12201-0509 (United States)], E-mail: patrick.parsons@wadsworth.org

    2007-03-15

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass (m{sub 0}), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 {+-} 0.6 pg, compared to 16.1 {+-} 0.7 pg for the Z5100, and 23.3 {+-} 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection

  13. Determination of lead and cadmium in ceramicware leach solutions by graphite furnace atomic absorption spectroscopy: method development and interlaboratory trial.

    Science.gov (United States)

    Hight, S C

    2001-01-01

    This method was developed to improve sensitivity and eliminate time consuming, evaporative pre-concentration in AOAC Method 973.82 and American Society for Testing and Materials method C738 for testing foodware. The method was developed using leach solutions obtained by leaching 9 differently decorated ceramic vessels with 4% acetic acid for 24 h at room temperature. Lead and cadmium concentrations in leach solutions were 0.005-17,600 and 0.0004-0.500 microg/mL, respectively. Concentrations were determined using peak area, phosphate chemical modifier (8.3 microg PO4(-3)), and a standard curve for quantitation. Optimized pre-atomization and atomization temperatures were 1,300 and 1,800 degrees C, respectively, for Pb and 1,100 and 1,700 degrees C, respectively, for Cd. Characteristic masses (mo) were 10 and 0.4 pg for Pb and Cd, respectively. Precision of repeated analyses of calibration solutions was < or =3% relative standard deviation. Precision of duplicate leach solution analyses on different days was 0-9% relative difference. Recovery from fortified leach solutions was 96-106%. Results obtained by this method agreed 92-110% with those of confirmatory analyses. Results of certified reference material solutions agreed 94-100% with certificate values. Pb and Cd limits of quantitation (LOQ) were 0.005 and 0.0005 microg/mL, respectively. Results from 3 trial laboratories for 4 leach solutions containing Pb and Cd concentrations of 0.017-1.47 and <0.0005-0.0864 microg/mL, respectively, agreed 89-102% with results of the author. Two attributes of this method were noteworthy: (1) Background absorbance due to organic matter was entirely absent from atomization profiles, making the use of short pre-atomization hold times (2 s) possible. (2) Instrument precision was excellent and only one determination per solution was needed. Acceptance criteria for quality control measurements and a practical procedure for estimating the method LOQ during routine regulatory analyses

  14. Determination of Mercury in Milk by Cold Vapor Atomic Fluorescence: A Green Analytical Chemistry Laboratory Experiment

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel

    2011-01-01

    Green analytical chemistry principles were introduced to undergraduate students in a laboratory experiment focused on determining the mercury concentration in cow and goat milk. In addition to traditional goals, such as accuracy, precision, sensitivity, and limits of detection in method selection and development, attention was paid to the…

  15. Independent genetic control of maize (Zea mays L.) kernel weight determination and its phenotypic plasticity.

    Science.gov (United States)

    Alvarez Prado, Santiago; Sadras, Víctor O; Borrás, Lucas

    2014-08-01

    Maize kernel weight (KW) is associated with the duration of the grain-filling period (GFD) and the rate of kernel biomass accumulation (KGR). It is also related to the dynamics of water and hence is physiologically linked to the maximum kernel water content (MWC), kernel desiccation rate (KDR), and moisture concentration at physiological maturity (MCPM). This work proposed that principles of phenotypic plasticity can help to consolidated the understanding of the environmental modulation and genetic control of these traits. For that purpose, a maize population of 245 recombinant inbred lines (RILs) was grown under different environmental conditions. Trait plasticity was calculated as the ratio of the variance of each RIL to the overall phenotypic variance of the population of RILs. This work found a hierarchy of plasticities: KDR ≈ GFD > MCPM > KGR > KW > MWC. There was no phenotypic and genetic correlation between traits per se and trait plasticities. MWC, the trait with the lowest plasticity, was the exception because common quantitative trait loci were found for the trait and its plasticity. Independent genetic control of a trait per se and genetic control of its plasticity is a condition for the independent evolution of traits and their plasticities. This allows breeders potentially to select for high or low plasticity in combination with high or low values of economically relevant traits.

  16. Extraction, Characterization, and Molecular Weight Determination of Senna tora (L. Seed Polysaccharide

    Directory of Open Access Journals (Sweden)

    Harshal A. Pawar

    2015-01-01

    Full Text Available The objective of the present work was extraction of polysaccharide from Senna tora L. seed and its characterization as a pharmaceutical excipient. Polysaccharide extraction was based on mechanical separation of the endosperm of seeds of Senna tora, water dissolution, centrifugation, and precipitation with acetone. Standard procedures were used to study the viscosity, micromeritic properties, and microbial bioburden. Accelerated stability study was carried out on isolated polysaccharide for six months at 40°C/75 RH as per ICH guidelines. The gum obtained from S. tora seeds was an amorphous free flowing odourless powder with dull brown colour (yield = 35% w/w. The bulk density, tapped density, and angle of repose data reveal that S. tora gum possesses good flow property. The intrinsic viscosity obtained was 1.568 dL/g. The average molecular weight of purified S. tora gum was found to be 198 kDa by intrinsic viscosity method. The results indicated that viscosity of gum solution increases with increase in temperature. FTIR study revealed the absence of degradation or decomposition of polysaccharide at accelerated stability conditions for six months. It has been concluded that extracted polysaccharide can be used as pharmaceutical excipient in terms of flow behavior, microbial properties, and stability.

  17. Determination of the linear coefficient of thermal expansion in polymer films at the nanoscale: influence of the composition of EVA copolymers and the molecular weight of PMMA.

    Science.gov (United States)

    González-Benito, J; Castillo, E; Cruz-Caldito, J F

    2015-07-28

    Nanothermal-expansion of poly(ethylene-co-vinylacetate), EVA, and poly(methyl methacrylate), PMMA, in the form of films was measured to finally obtain linear coefficients of thermal expansion, CTEs. The simple deflection of a cantilever in an atomic force microscope, AFM, was used to monitor thermal expansions at the nanoscale. The influences of: (a) the structure of EVA in terms of its composition (vinylacetate content) and (b) the size of PMMA chains in terms of the molecular weight were studied. To carry out this, several polymer samples were used, EVA copolymers with different weight percents of the vinylacetate comonomer (12, 18, 25 and 40%) and PMMA polymers with different weight average molecular weights (33.9, 64.8, 75.600 and 360.0 kg mol(-1)). The dependencies of the vinyl acetate weight fraction of EVA and the molecular weight of PMMA on their corresponding CTEs were analyzed to finally explain them using new, intuitive and very simple models based on the rule of mixtures. In the case of EVA copolymers a simple equation considering the weighted contributions of each comonomer was enough to estimate the final CTE above the glass transition temperature. On the other hand, when the molecular weight dependence is considered the free volume concept was used as novelty. The expansion of PMMA, at least at the nanoscale, was well and easily described by the sum of the weighted contributions of the occupied and free volumes, respectively.

  18. Mercury determination in non- and biodegradable materials by cold vapor capacitively coupled plasma microtorch atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Frentiu, Tiberiu, E-mail: ftibi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Mihaltan, Alin I., E-mail: alinblaj2005@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Ponta, Michaela, E-mail: mponta@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Darvasi, Eugen, E-mail: edarvasi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Frentiu, Maria, E-mail: frentiu.maria@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Cordos, Emil, E-mail: emilcordos@gmail.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania)

    2011-10-15

    Highlights: {yields} Use of a miniaturized analytical system with microtorch plasma for Hg determination. {yields} Determination of Hg in non- and biodegradable materials using cold vapor generation. {yields} Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min{sup -1} Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl{sub 2} reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO{sub 3}-H{sub 2}SO{sub 4} mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml{sup -1} or 0.08 {mu}g g{sup -1} in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg{sup -1}, while recovery in two polyethylene certified reference materials in the range 98.7 {+-} 4.5% (95% confidence level).

  19. Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

    Science.gov (United States)

    Campos, Reinaldo C.; Gonçalves, Rodrigo A.; Brandão, Geisamanda P.; Azevedo, Marlo S.; Oliveira, Fabiana; Wasserman, Julio

    2009-06-01

    The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C 18 column was used as stationary phase, and post column treatment was performed by UV irradiation (60 °C, 13 W). The eluate was then merged with 3 mol L - 1 HCl, reduction was performed by a NaBH 4 solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 µg L - 1 were obtained for ionic (Hg 2+) and HgCH 3+, for an injection volume of 200 µL. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sediments.

  20. Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

    Energy Technology Data Exchange (ETDEWEB)

    Campos, Reinaldo C. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil)], E-mail: rccampos@puc-rio.br; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil); Oliveira, Fabiana; Wasserman, Julio [Institut of Geosciences, Fluminense Federal University, Av. Gal. Milton Tavares de Souza, s/n, 24.210-340, Niteroi, Rio de Janeiro (Brazil)

    2009-06-15

    The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C{sub 18} column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L{sup -1} HCl, reduction was performed by a NaBH{sub 4} solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 {mu}g L{sup -1} were obtained for ionic (Hg{sup 2+}) and HgCH{sub 3}{sup +}, for an injection volume of 200 {mu}L. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sedi0011men.

  1. Determination of {sup 233}U by inductively coupled argon plasma - atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Patwardhan, A.B.; Kulkarni, V.T.; Radhakrishnan, K.; Ramanujam, A.; Page, A.G. [Bhabha Atomic Research Centre, Bombay (India)

    1994-09-01

    The paper describes studies carried out for the determination of {sup 233}U at various stages during the recovery and purification of {sup 233}U from {sup 233}U-Al alloy scraps generated during the fabrication of {sup 233}U-Al alloy fuel. Employing a high resolution sequential spectrometer and Inductively Coupled argon Plasma (ICP) as the spectral excitation source, isotope shift for {sup 233}U with respect to {sup 238}U has been resolved and recorded. The shift for the 424.437 nm emission line of {sup 238}U is found to be of the order of 0.040 nm on the lower wavelength side for {sup 233}U and this isotopic effect has been utilised for the quantitative determination of {sup 233}U. The overall precision of the method is 5% RSD with the detection limit of 0.01 {mu}g/ml.

  2. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry.

    Science.gov (United States)

    Dancsak, Stacia E; Silva, Sidnei G; Nóbrega, Joaquim A; Jones, Bradley T; Donati, George L

    2014-01-02

    High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg(-1) for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg(-1) for Na and K, and between 0.22 and 0.43 mg kg(-1) for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated. Powers of detection are comparable to other traditional methods.

  3. Endocrine determinants of changes in insulin sensitivity and insulin secretion during a weight cycle in healthy men.

    Directory of Open Access Journals (Sweden)

    Judith Karschin

    Full Text Available Changes in insulin sensitivity (IS and insulin secretion occur with perturbations in energy balance and glycemic load (GL of the diet that may precede the development of insulin resistance and hyperinsulinemia. Determinants of changes in IS and insulin secretion with weight cycling in non-obese healthy subjects remain unclear.In a 6wk controlled 2-stage randomized dietary intervention 32 healthy men (26±4y, BMI: 24±2kg/m2 followed 1wk of overfeeding (OF, 3wks of caloric restriction (CR containing either 50% or 65% carbohydrate (CHO and 2wks of refeeding (RF with the same amount of CHO but either low or high glycaemic index at ±50% energy requirement. Measures of IS (basal: HOMA-index, postprandial: Matsuda-ISI, insulin secretion (early: Stumvoll-index, total: tAUC-insulin/tAUC-glucose and potential endocrine determinants (ghrelin, leptin, adiponectin, thyroid hormone levels, 24h-urinary catecholamine excretion were assessed.IS improved and insulin secretion decreased due to CR and normalized upon RF. Weight loss-induced improvements in basal and postprandial IS were associated with decreases in leptin and increases in ghrelin levels, respectively (r = 0.36 and r = 0.62, p<0.05. Weight regain-induced decrease in postprandial IS correlated with increases in adiponectin, fT3, TSH, GL of the diet and a decrease in ghrelin levels (r-values between -0.40 and 0.83, p<0.05 whereas increases in early and total insulin secretion were associated with a decrease in leptin/adiponectin-ratio (r = -0.52 and r = -0.46, p<0.05 and a decrease in fT4 (r = -0.38, p<0.05 for total insulin secretion only. After controlling for GL associations between RF-induced decrease in postprandial IS and increases in fT3 and TSH levels were no longer significant.Weight cycling induced changes in IS and insulin secretion were associated with changes in all measured hormones, except for catecholamine excretion. While leptin, adiponectin and ghrelin seem to be the major

  4. Determination of gaseous semi-and low-volatile organic halogen compounds by barrier-discharge atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    Yifei Sun; Nobuhisa Watanabe; Wei Wang; Tianle Zhu

    2013-01-01

    A group parameter approach using "total organic halogen" is effective for monitoring gaseous organic halogen compounds,including fluorine,chlorine,and bromine compounds,generated from combustion.We described the use of barrier-discharge radiofrequencyhelium-plasma/atomic emission spectrometry,for the detection of semi-and low-volatile organic halogen compounds (SLVOXs),which can be collected by CarbotrapTM adsorbents and analyzed using thermal desorption.The optimal carrier gas flow rates at the injection and desorption lines were established to be 100 mL/min.The detection range for SLVOXs in the gaseous samples was from 10 ng to tens of micrograms.Measuring F was more diflicult than measuring Cl or Br,because the wavelength ofF is dose to that of air.The barrierdischarge radiofrequency-helium-plasma/atomic emission spectrometry measured from 85% to 103% of the SLVOXs in the gas sample.It has been found that Carbotrap B is appropriate for high-boiling-point compounds,and Carbotrap C is suitable for the determination of organic halogen compounds with lower boiling points,in the range 200-230℃.Under optimal analysis conditions,a chlorinecontaining plastic was destroyed using different oxygen concentrations.Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds.

  5. Determination of mercury in an assortment of dietary supplements using an inexpensive combustion atomic absorption spectrometry technique.

    Science.gov (United States)

    Levine, Keith E; Levine, Michael A; Weber, Frank X; Hu, Ye; Perlmutter, Jason; Grohse, Peter M

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 mug per week.

  6. Determination and characterization of phytochelatins by liquid chromatography coupled with on line chemical vapour generation and atomic fluorescence spectrometric detection.

    Science.gov (United States)

    Bramanti, Emilia; Toncelli, Daniel; Morelli, Elisabetta; Lampugnani, Leonardo; Zamboni, Roberto; Miller, Keith E; Zemetra, Joseph; D'Ulivo, Alessandro

    2006-11-10

    Liquid chromatography (LC) coupled on line with UV/visible diode array detector (DAD) and cold vapour generation atomic fluorescence spectrometry (CVGAFS) has been developed for the speciation, determination and characterization of phytochelatins (PCs). The method is based on a bidimensional approach, e.g. on the analysis of synthetic PC solutions (apo-PCs and Cd(2+)-complexed PCs) (i) by size exclusion chromatography coupled to UV diode array detector (SEC-DAD); (ii) by the derivatization of PC -SH groups in SEC fractions by p-hydroxymercurybenzoate (PHMB) and the indirect detection of PC-PHMB complexes by reversed phase liquid chromatography coupled to atomic fluorescence detector (RPLC-CVGAFS). MALDI-TOF/MS (matrix assisted laser desorption ionization time of flight mass spectrometry) analysis of underivatized synthetic PC samples was performed in order have a qualitative information of their composition. Quantitative analysis of synthetic PC solutions has been performed on the basis of peak area of PC-PHMB complexes of the mercury specific chromatogram and calibration curve of standard solution of glutathione (GSH) complexed to PHMB (GS-PHMB). The limit of quantitation (LOQ) in terms of GS-PHMB complex was 90 nM (CV 5%) with an injection volume of 35 microL, corresponding to 3.2 pmol (0.97 ng) of GSH. The method has been applied to analysis of extracts of cell cultures from Phaeodactylum tricornutum grown in Cd-containing nutrient solutions, analysed by SEC-DAD-CVGAFS and RPLC-DAD-CVGAFS.

  7. a Proposal for a General Method for Determining Semi-Experimental Equilibrium Structures of Carbon Atom Backbones

    Science.gov (United States)

    Craig, Norman C.

    2010-06-01

    Semi-experimental equilibrium structures are determined from ground state rotational constants derived from the analysis of rotational transitions in high-resolution spectra and from the quantum chemical calculation of spectroscopic alphas. In the full application of this method, spectra of numerous isotopic species must be investigated. Most of these isotopic species require specialized synthesis. We now propose focusing on the carbon atoms, for which microwave spectroscopy routinely yields spectra for polar molecules with 13C substitution in natural abundance. Needed spectroscopic alphas can be computed with Gaussian software. Application of the Kraitchman substitution relationships gives Cartesian coordinates for the carbon atoms and thence bond parameters for the carbon backbone. This method will be evaluated with ethylene, 1,1-difluoroethylene, 1,1-difluorocyclopropane, propene, and butadiene. The method will then be applied to cis-hexatriene and the two conformers of glycidol. R. D. Suenram, B. H. Pate, A. Lessari, J. L. Neill, S. Shipman, R. A. Holmes, M. C. Leyden, and N. C. Craig, J. Phys. Chem. A 113, 1864-1868 (2009). A. R. Conrad, N. H. Teumelsan, P. E. Wang, and M. J. Tubergen, J. Phys. Chem. A 114, 336-342 (2010).

  8. Determination of thermodynamic affinities of various polar olefins as hydride, hydrogen atom, and electron acceptors in acetonitrile.

    Science.gov (United States)

    Cao, Ying; Zhang, Song-Chen; Zhang, Min; Shen, Guang-Bin; Zhu, Xiao-Qing

    2013-07-19

    A series of 69 polar olefins with various typical structures (X) were synthesized and the thermodynamic affinities (defined in terms of the molar enthalpy changes or the standard redox potentials in this work) of the polar olefins obtaining hydride anions, hydrogen atoms, and electrons, the thermodynamic affinities of the radical anions of the polar olefins (X(•-)) obtaining protons and hydrogen atoms, and the thermodynamic affinities of the hydrogen adducts of the polar olefins (XH(•)) obtaining electrons in acetonitrile were determined using titration calorimetry and electrochemical methods. The pure C═C π-bond heterolytic and homolytic dissociation energies of the polar olefins (X) in acetonitrile and the pure C═C π-bond homolytic dissociation energies of the radical anions of the polar olefins (X(•-)) in acetonitrile were estimated. The remote substituent effects on the six thermodynamic affinities of the polar olefins and their related reaction intermediates were examined using the Hammett linear free-energy relationships; the results show that the Hammett linear free-energy relationships all hold in the six chemical and electrochemical processes. The information disclosed in this work could not only supply a gap of the chemical thermodynamics of olefins as one class of very important organic unsaturated compounds but also strongly promote the fast development of the chemistry and applications of olefins.

  9. Determination of lead in wine by hydride generation atomic fluorescence spectrometry in the presence of hexacyanoferrate(III).

    Science.gov (United States)

    Karadjova, Irina B; Lampugnani, Leonardo; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L

    2007-06-01

    A rapid, accurate, and precise method is described for the determination of Pb in wine using continuous-flow hydride generation atomic fluorescence spectrometry (CF-HGAFS). Sample pretreatment consists of ten-fold dilution of wine followed by direct plumbane generation in the presence of 0.1 mol L(-1) HCl and 1% m/v K(3)[Fe(CN)(6)] with 1% m/v NaBH(4) as reducing agent. An aqueous standard calibration curve is recommended for Pb quantification in wine sample. The method provides a limit of detection and a limit of quantification of 0.3 microg L(-1) and 1 microg L(-1), respectively. The relative standard deviation varies between 2-6% (within-run) and 4-11% (between-run) at 3-30 microg L(-1) Pb levels in wine. Good agreement has been demonstrated between results obtained by CF-HGAFS and direct electrothermal atomic absorption spectrometry in analyses of red and white wines within the concentration range of 9.2-25.8 microg L(-1) Pb.

  10. Quantitative composition determination at the atomic level using model-based high-angle annular dark field scanning transmission electron microscopy.

    Science.gov (United States)

    Martinez, G T; Rosenauer, A; De Backer, A; Verbeeck, J; Van Aert, S

    2014-02-01

    High angle annular dark field scanning transmission electron microscopy (HAADF STEM) images provide sample information which is sensitive to the chemical composition. The image intensities indeed scale with the mean atomic number Z. To some extent, chemically different atomic column types can therefore be visually distinguished. However, in order to quantify the atomic column composition with high accuracy and precision, model-based methods are necessary. Therefore, an empirical incoherent parametric imaging model can be used of which the unknown parameters are determined using statistical parameter estimation theory (Van Aert et al., 2009, [1]). In this paper, it will be shown how this method can be combined with frozen lattice multislice simulations in order to evolve from a relative toward an absolute quantification of the composition of single atomic columns with mixed atom types. Furthermore, the validity of the model assumptions are explored and discussed.

  11. Determination of functional collective motions in a protein at atomic resolution using coherent neutron scattering

    Science.gov (United States)

    Hong, Liang; Jain, Nitin; Cheng, Xiaolin; Bernal, Ana; Tyagi, Madhusudan; Smith, Jeremy C.

    2016-01-01

    Protein function often depends on global, collective internal motions. However, the simultaneous quantitative experimental determination of the forms, amplitudes, and time scales of these motions has remained elusive. We demonstrate that a complete description of these large-scale dynamic modes can be obtained using coherent neutron-scattering experiments on perdeuterated samples. With this approach, a microscopic relationship between the structure, dynamics, and function in a protein, cytochrome P450cam, is established. The approach developed here should be of general applicability to protein systems. PMID:27757419

  12. Pressurized liquid extraction followed by gas chromatography with atomic emission detection for the determination of fenbutatin oxide in soil samples.

    Science.gov (United States)

    Canosa, P; Montes, R; Lamas, J P; García-López, M; Orriols, I; Rodríguez, I

    2009-08-15

    A novel method for the determination of the miticide bis[tris(2-methyl-2-phenylpropyl)tin] oxide, also known as fenbutatin oxide (FBTO), in agricultural soils is presented. Pressurized liquid extraction (PLE) followed by analyte derivatization and extraction into isooctane was the used sample preparation approach. Selective determination was achieved by gas chromatography with atomic emission detection (GC-AED). Influence of different parameters on the performance of the extraction process is thoroughly discussed; moreover, some relevant aspects related to derivatization, determination and quantification steps are also presented. As regards PLE, the type of solvent and the temperature were the most relevant variables. Under optimized conditions, acetone, without any acidic modifier, was employed as extractant at 80 degrees C. Cells were pressurized at 1500 psi, and 2 static cycles of 1 min each were applied. Acetone extracts (ca. 25 mL) were concentrated to 1 mL, derivatized with sodium tetraethyl borate (NaBEt(4)) and the FBTO derivative, resulting from cleavage of the Sn-O-Sn bond followed by ethylation of the hydroxyl fragments, extracted into isooctane and determined by GC-AED. Under final working conditions, the proposed method provided recoveries from 76 to 99% for spiked soil samples, a limit of quantification of 2 ng g(-1) and an acceptable precision. Analysis of samples from vineyards sprayed with FBTO, confirmed the persistence of the miticide in soil for more than 1 year after being applied.

  13. Interlaboratory bias in the determination of mercury concentrations in commercially available fish utilizing thermal decomposition/amalgamation atomic absorption spectrophotometry.

    Science.gov (United States)

    Butala, Steven J M; Scanlan, Larry P; Chaudhuri, Sanwat N; Perry, Deborah D; Taylor, Robert J

    2007-10-01

    Four commercially available fish fillets were freeze-dried, homogenized, and analyzed for mercury by the Texas A&M Trace Element Research Laboratory and the Utah Public Health Laboratory (UPHL) utilizing thermal decomposition/amalgamation atomic absorption spectrophotometry. Two-way analysis of variance detected bias in the data between the two laboratories. Some of the bias could be attributed to different calibration curve quantitation and near detection limit quantitation, albeit causal explanations could be confounded with other effects. Knowledge of analytical bias will aid interpretation of interlaboratory data. The swordfish mercury content, as determined by both laboratories, was about 1 ppm, while mercury content found in the Atlantic salmon was about 0.021 ppm. For the Alaskan halibut, the Texas A&M measured a mercury concentration of 0.155 ppm, while the UPHL measured a mercury concentration of 0.181 ppm for the same fish. The Texas A&M determined that the Canadian-raised salmon contained about 0.019 ppm of mercury, while the UPHL determined a mercury content of about 0.025 ppm for the same fish. The mercury found within the fish fillets did not exceed nationwide mercury mean values determined by the U.S. Food and Drug Administration.

  14. [Investigation of determining strontium in M. nitida Benth. var. hirsutissima. Z. Wei. by flame atomic absorption spectra].

    Science.gov (United States)

    Zhang, Ling; Rao, Zhi-Jun; Guan, Yuan-Yuan; Zhang, Hai-Ming

    2010-12-01

    The present paper is aimed to establish the method of determining the strontium in M. nitida Benth. var. hirsutissima. Z. Wei. by means of air-acetylene flame atomic absorption spectra, and also provide reference for the determination of the strontium in other traditional Chinese medicine. M. Nitida Benthvarhirsutissima Z. Wei. was taken as the object. The authors used nitric-perchloric acid as digestion solution to digest samples by microwave which was controlled by pressure, and used EDTA-2Na as the releasing agent to add in the samples for determining the strontium in M. nitida Benth. var. hirsutissima. Z. Wei. by FAAS. The results showed that the samples were entirely digested by microwave. The working curve was Y = 0.036 5x -0.001 1, r = 0.999 4, the range was 0-1.6 microg x mL(-1), the average recovery rate was 101.5% with RSD 2.04%, and the method detection limit was 0.008 2 microg x mL(-1) (n = 21). It is concluded that this method is simple and accurate. It has high sensitivity and can be effectively used for determining the strontium in this traditional Chinese medicine.

  15. Determination of Trace Amounts of Nickel (Ⅱ) by Graphite Furnace Atomic Absorption Spectrometry Coupled with Cloud Point Extraction

    Institute of Scientific and Technical Information of China (English)

    SHAH Syed Mazhar; WANG Hao-nan; SU Xing-guang

    2011-01-01

    A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ)and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed,8-hydroxyquinoline and Triton X-100 were usedl as the ligand and surfactant respectively. Nickel(Ⅱ) can form a hydrophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature(CPT) for GFAAS determination. The factors affecting the cloud point extraction,such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation(RSD) of 2.9% were obtained for Ni(Ⅱ) determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel(Ⅱ) in certified reference material and different types of water samples and the recovery was in a range of 95% 103%.

  16. Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

    2009-07-15

    A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

  17. Determination of Cd, Pb and As in sediments of the Sava River by electrothermal atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    SIMONA MURKO

    2010-01-01

    Full Text Available The applicability of nitric acid, palladium nitrate and a mixture of palladium and magnesium nitrate as matrix modifiers were estimated for the accurate and reproducible determination of cadmium (Cd, lead (Pb and arsenic (As in sediments of the Sava River by electrothermal atomic absorption spectrometry, ETAAS. Decomposition of the samples was done in a closed vessel microwave-assisted digestion system using nitric, hydrochloric and hydrofluoric acids, followed by the addition of boric acid to convert the fluorides into soluble complexes. The parameters for the determination of Cd, Pb and As in sediments were optimised for each individual element and for each matrix modifier. In addition, two sediment reference materials were also analysed. In determination of Cd and Pb, nitric acid was found to be the most appropriate matrix modifier. The accurate and reliable determination of Cd and Pb in sediments was possible also in the presence of boric acid. The use of a mixture of palladium and magnesium nitrate efficiently compensated for matrix effects and enabled the accurate and reliable determination of As in the sediments. Quantification of Cd and As was performed by calibration using acid matched standard solutions, while the standard addition method was applied for the quantification of Pb. The repeatability of the analytical procedure for the determination of Cd, Pb and As in sediments was ±5 % for Cd, ±4 % for Pb and ±2 % for As. The LOD values of the analytical procedure were found to be 0.05 mg/kg for Cd and 0.25 mg/kg for Pb and As, while the LOQ values were 0.16 mg/kg for Cd and 0.83 mg/kg for Pb and As. Finally, Cd, Pb and As were successfully determined in sediments of the Sava River in Slovenia.

  18. Total Mercury Determination in Petroleum Green Coke and Oily Sludge Samples by Cold Vapor Atomic Fluorescence Spectrometry

    National Research Council Canada - National Science Library

    Camera, Adriana S; Maranhão, Tatiane A; Oliveira, Fernando J. S; Silva, Jessee S. A; Frescura, Vera L. A

    2015-01-01

    ...+ before the atomic vapor formation. Accuracy of the method was evaluated through certified reference material, for green coke, and comparison with cold vapor atomic absorption spectrometry (CV AAS), for oily sludge...

  19. Minimizing chemical interference errors for the determination of lithium in brines by flame atomic absorption spectroscopy analysis

    Institute of Scientific and Technical Information of China (English)

    WEN Xianming; MA Peihua; ZHU Geqin; WU Zhiming

    2006-01-01

    Chemical interferences (ionization and oxide/hydroxide formation) on the atomic absorbance signal of lithium in FAAS analysis of brine samples are elaborated in this article. It is suggested that inadequate or overaddition of deionization buffers can lead to loss of sensitivities under particular operating conditions. In the analysis of brine samples, signal enhancing and oxide/hydroxide formation inducing signal reduction resulting from overaddition of deionization buffers can be seen with varying amounts of chemical buffers. Based on experimental results, the authors have arrived at the op timized operating conditions for the detection of lithium, under which both ionization and stable compound formation can be suppressed. This is a simplified and quick method with adequate accuracy and precision for the determination of lithium in routine brine samples from chemical plants or R&D laboratories, which contain comparable amounts of lithium with some other components.

  20. Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

    Science.gov (United States)

    Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

    2006-12-01

    A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

  1. Cloud point extraction-thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

    Energy Technology Data Exchange (ETDEWEB)

    Wu Peng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China); Zhang Yunchang [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Lv Yi [College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China); Hou Xiandeng [Analytical and Testing Center, Sichuan University, Chengdu, Sichuan 610064 (China) and College of Chemistry, Sichuan University, Chengdu, Sichuan 610064 (China)]. E-mail: houxd@scu.edu.cn

    2006-12-15

    A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 {mu}g/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

  2. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

    2013-01-01

    A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

  3. Speciation determination of chromium(III) and (VI) using preconcentration cloud point extraction with flame atomic absorption spectrometry (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Kiran, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Kumar, K. Suresh; Prasad, B.; Suvardhan, K. [Department of Chemistry, S. V. University, Tirupati, 517502 A.P. (India); Lekkala, Ramesh Babu [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India); Janardhanam, K. [Department of Environmental Sciences, S.V. University, Tirupati, 517502 A.P. (India)], E-mail: Kandukurijanardhanam@gmail.com

    2008-02-11

    bis-[2-Hydroxy-1-naphthaldehyde] thiourea was synthesized and preconcentration cloud point extraction (CPE) for speciation determination of chromium(III) and (VI) in various environmental samples with flame atomic absorption spectrometry (FAAS) has been developed. Chromium(III) complexes with bis-[2-hydroxynaphthaldehyde] thiourea is subsequently entrapped in the surfactant micelles. After complexation of chromium(III) with reagent, the analyte was quantitatively extracted to the surfactant-rich phase in the non-ionic surfactant Triton X-100 after centrifugation. The effect of pH, concentration of chelating agent, surfactant, equilibration temperature and time on CPE was studied. The relative standard deviation was 2.13% and the limits of detection were around 0.18 {mu}g L{sup -1}.

  4. Determination of trace elements in plutonium by solvent extraction and ICP-atomic emission spectrometry

    Science.gov (United States)

    Patwardhan, A. B.; Joshi, M. V.; Kulkarni, V. T.; Radhakrishnan; Sumathi, S.; Jacob, Mary

    This report describes the studies carried out for the determination of trace metallic impurities in plutonium solutions. Plutonium is separated from the impurity elements by the selective extraction of plutonium in tri-butyl-phosphate. The aqueous phase containing the impurities is fed to the high temperature source of excitation such as inductively coupled argon plasma and the analysis is carried out employing computer controlled multichannel direct reading spectrometer. Based on the above studies a method has been standardized for the analysis of sixteen elements in plutonium oxide/nitrate samples. The relative standard deviation of the method for various elements is in the range of +/- 1 to 5%. The method offers distinct advantages over the conventional carrier distillation technique in terms of precision, range, and sensitivity.

  5. Trace element determination-I Use of 2,9-dimethyl-1,10-phenanthroline in determination of copper in heavy matrices by carbon furnace atomic-absorption spectrometry.

    Science.gov (United States)

    Battistoni, P; Bruni, P; Cardellini, L; Fava, G; Gobbi, G

    1980-08-01

    A method for the determination of copper in complex matrices by electrothermal atomic-absorption spectrometry has been developed. It uses neocuproine as complexing agent. The detection limit is 0.2 ng/ml, and interferences are minimized.

  6. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chappuy, M. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Caudron, E., E-mail: eric.caudron@eps.aphp.fr [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Groupe de Chimie Analytique de Paris-Sud, EA 4041, IFR 141, School of Pharmacy, Univ Paris-Sud, 92296 Chatenay-Malabry (France); Bellanger, A. [Department of Pharmacy, Pitie-Salpetriere Hospital (Paris Public Hospital Authority), 47 boulevard de l' hopital, 75013 Paris (France); Pradeau, D. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France)

    2010-04-15

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 {mu}g mL{sup -1}. In optimal conditions, the limit of detection was 0.2 ng mL{sup -1}, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL{sup -1}. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  7. Determination of aluminum by electrothermal atomic absorption spectroscopy in lubricating oils emulsified in a sequential injection analysis system.

    Science.gov (United States)

    Burguera, José L; Burguera, Marcela; Antón, Raquel E; Salager, Jean-Louis; Arandia, María A; Rondón, Carlos; Carrero, Pablo; de Peña, Yaneira Petit; Brunetto, Rosario; Gallignani, Máximo

    2005-12-15

    The sequential injection (SIA) technique was applied for the on-line preparation of an "oil in water" microemulsion and for the determination of aluminum in new and used lubricating oils by electrothermal atomic absorption spectrometry (ET AAS) with Zeeman-effect background correction. Respectively, 1.0, 0.5 and 1.0ml of surfactants mixture, sample and co-surfactant (sec-butanol) solutions were sequentially aspirated to a holding coil. The sonication and repetitive change of the flowing direction improved the stability of the different emulsion types (oil in water, water in oil and microemulsion). The emulsified zone was pumped to fill the sampling arm of the spectrometer with a sub-sample of 200mul. Then, 10mul of this sample solution were introduced by means of air displacement in the graphite tube atomizer. This sequence was timed to synchronize with the previous introduction of 15mug of Mg(NO(3))(2) (in a 10mul) by the spectrometer autosampler. The entire SIA system was controlled by a computer, independent of the spectrometer. The furnace program was carried out by employing a heating cycle in four steps: drying (two steps at 110 and 130 degrees C), pyrolisis (at 1500 degrees C), atomization (at 2400 degrees C) and cleaning (at 2400 degrees C). The calibration graph was linear from 7.7 to 120mugAll(-1). The characteristic mass (mo) was 33.2pg/0.0044s and the detection limit was 2.3mugAll(-1). The relative standard (RSD) of the method, evaluated by replicate analyses of different lubricating oil samples varied in all cases between 1.5 and 1.7%, and the recovery values found in the analysis of spiked samples ranged from 97.2 to 100.4%. The agreement between the observed and reference values obtained from two NIST Standard Certified Materials was good. The method was simple and satisfactory for determining aluminum in new and used lubricating oils.

  8. Determination of trace elements in heroin by inductively coupled plasma atomic emission spectrometry using ultrasonic nebulization

    Science.gov (United States)

    Budič, Bojan; Klemenc, Sonja

    2000-06-01

    A method for the determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, P, S, Sr and Zn in heroin samples by ICP-AES using ultrasonic nebulization is described. The samples were microwave digested with HNO 3. To improve the detection limits and minimise the matrix interferences the experimental parameters were optimised by variation of the operating power, carrier gas flow rate and observation height above the load coil. Optimum operating conditions for most of the analytes were at operating power 1550 W, carrier gas flow rate between 0.8 and 1.0 l min -1 and observation height between 10 and 12 mm above load coil. The limits of detection were below 0.5 μg g -1 (dry mass) for most of the elements investigated. The analytical recoveries of spiked samples were in the range between 94 and 103% and precision was on average better than 6%. The analysis of heroin samples shows that the method is simple, rapid and capable of providing accurate results for all the analytes investigated with the exception of nickel which was below the limit of detection in the analyzed samples.

  9. A method optimization study for atomic absorption spectrophotometric determination of total zinc in insulin using direct aspiration technique

    Directory of Open Access Journals (Sweden)

    Sadia Ata

    2015-03-01

    Full Text Available A sensitive, reliable and relative fast method has been developed for the determination of total zinc in insulin by atomic absorption spectrophotometer. This designed study was used to optimize the procedures for the existing methods. Spectrograms of both standard and sample solutions of zinc were recorded by measuring the absorbance at 213.9 nm for determination of total zinc. System suitability parameters were evaluated and were found to be within the limits. Linearity was evaluated through graphical representation of concentration versus absorbance. Repeatability (intra-day and intermediate precision (inter-day were assessed by analyzing working standard solutions. Accuracy and robustness were experimented from the standard procedures. The percentage recovery of zinc was found to be 99.8%, relative standard deviation RSD 1.13%, linearity of determination LOD 0.0032 μg/mL, and limit of quantization LOQ 0.0120 μg/mL. This developed and proposed method was then validated in terms of accuracy, precision, linearity and robustness which can be successfully used for the quantization of zinc in insulin.

  10. Formulation of geopotential difference determination using optical-atomic clocks onboard satellites and on ground based on Doppler cancellation system

    Science.gov (United States)

    Shen, Ziyu; Shen, Wen-Bin; Zhang, Shuangxi

    2016-08-01

    In this study, we propose an approach for determining the geopotential difference using high-frequency-stability microwave links between satellite and ground station based on Doppler cancellation system. Suppose a satellite and a ground station are equipped with precise optical-atomic clocks (OACs) and oscillators. The ground oscillator emits a signal with frequency fa towards the satellite and the satellite receiver (connected with the satellite oscillator) receives this signal with frequency fb which contains the gravitational frequency shift effect and other signals and noises. After receiving this signal, the satellite oscillator transmits and emits, respectively, two signals with frequencies fb and fc towards the ground station. Via Doppler cancellation technique, the geopotential difference between the satellite and the ground station can be determined based on gravitational frequency shift equation by a combination of these three frequencies. For arbitrary two stations on ground, based on similar procedures as described above, we may determine the geopotential difference between these two stations via a satellite. Our analysis shows that the accuracy can reach 1 m2 s- 2 based on the clocks' inaccuracy of about 10-17 (s s-1) level. Since OACs with instability around 10-18 in several hours and inaccuracy around 10-18 level have been generated in laboratory, the proposed approach may have prospective applications in geoscience, and especially, based on this approach a unified world height system could be realized with one-centimetre level accuracy in the near future.

  11. Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Zhimei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Department of Chemistry and Biology, Huainan Normal University, Huainan 232001 (China); Liang Pei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)]. E-mail: liangpei@mail.ccnu.edu.cn; Ding Qiong [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Cao Jing [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)

    2006-09-21

    A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni{sup 2+} with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni{sup 2+} with 10 mL solution. Under the optimal conditions, the detection limit of Ni{sup 2+} is 0.12 ng mL{sup -1} with R.S.D. of 4.3% (n = 10, c = 100 ng mL{sup -1}). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.

  12. FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry (FAAS). The Cu2+ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL~0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2.1ng/mL in the original solution (3σ, n=9). Determination of copper in standard ions showed that the proposed method has good accuracy (recovery was more than 95%). The method was successfully applied for recovery and determination of copper in cereals food samples.

  13. FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

    Institute of Scientific and Technical Information of China (English)

    XU Wanzhen; ZHANG Xinghua; YAN Yongsheng; LIU Aiqin; JING Junjie

    2007-01-01

    A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry (FAAS). The Cu2+ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL~0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2.1ng/mL in the original solution (3σ, n=9). Determination of copper in standard ions showed that the proposed method has good accuracy (recovery was more than 95%). The method was successfully applied for recovery and determination of copper in cereals food samples.

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

    Science.gov (United States)

    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.

  15. Flame Atomic Absorption Determination of Gold Ion in Aqueous Samples after Preconcentration Using 9-Acridinylamine Functionalized γ-Alumina Nanoparticles

    Directory of Open Access Journals (Sweden)

    Mohammad Karimi

    2013-01-01

    Full Text Available A simple and sensitive solid phase extraction utilizing 9-acridinylamine functionalized alumina nanoparticles was developed, and their potential use for preconcentration and subsequent determination of gold by flame atomic absorption spectrometry (FAAS was investigated. A number of parameters, namely, type, concentration, and volume of eluent, pH of the sample solution, flow rate of extraction, and volume of the sample, were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. Gold ions were found to be recovered quantitatively at pH 3.0, with 0.1 mol L−1 thiourea in 2 mol L−1 H2SO4 as eluent. The limit of detection (LOD, defined as five times the standard deviation of the blank, was determined to be lower than 13.0 ppb. Under optimum conditions, the accuracy and precision (RSD% of the method were >98.0 and <1.5%, respectively. To gauge its ability in terms of application to real samples, the proposed method was successfully applied for determination of gold concentration in waste water samples and one soil standard material, and satisfactory results were obtained.

  16. Sensitive determination of cadmium in water samples by room temperature ionic liquid-based preconcentration and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Olsina, Roberto A. [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)], E-mail: rwuilloud@mendoza-conicet.gov.ar

    2008-10-17

    A sensitive preconcentration methodology for Cd determination at trace levels in water samples was developed in this work. 1-Butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]) room temperature ionic liquid (RTIL) was successfully used for Cd preconcentration, as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex [Cd-5-Br-PADAP]. Subsequently, Cd was back-extracted from the RTIL phase with 500 {mu}L of 0.5 mol L{sup -1} nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). A preconcentration factor of 40 was achieved with 20 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 3 ng L{sup -1} and the relative standard deviation (R.S.D.) for 10 replicates at 1 {mu}g L{sup -1} Cd{sup 2+} concentration level was 3.5%, calculated at peak heights. The calibration graph was linear from concentration levels near the detection limits up to at least 5 {mu}g L{sup -1}. A correlation coefficient of 0.9997 was achieved. Validation of the methodology was performed by standard addition method and analysis of certified reference material (CRM). The method was successfully applied to the determination of Cd in river and tap water samples.

  17. [Determination of trace elements in Lophatherum gracile brongn from different habitat by microwave digestion-atomic absorption spectroscopy].

    Science.gov (United States)

    Yuan, Ke; Xue, Yue-Qin; Gui, Ren-Yi; Sun, Su-Qin; Yin, Ming-Wen

    2010-03-01

    A method of microwave digestion technique was proposed to determine the content of Zn, Fe, Cu, Mn, K, Ca, Mg, Ni, Cd, Pb, Cr, Co, Al, Se and As in Lophatherum gracile brongn of different habitat by atomic absorption spectroscopy. The RSD of the method was between 1.23% and 3.32%, and the recovery rates obtained by standard addition method were between 95.8% and 104.20%. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of metal elements in Lophatherum gracile brongn. The experimental results also indicated that different areas' Lophantherum gracile brongn had different trace elements content. The content of trace elements K, Mg, Ca, Fe and Mn beneficial to the human body was rich. The content of the heavy metal trace element Pb in Lophantherum gracile brongn of Hunan province was slightly high. The content of the heavy metal trace element Cu in Lophantherum gracile brongn of Guangdong province and Anhui province is also slightly higher. Beside, the contents of harmful trace heavy metal elements Cd, Cu, Cr, Pb and As in Lophatherum gracile brongn of different habitat are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation and National Food Sanitation Standard. These determination results provided the scientific data for further discussing the relationship between the content of trace elements in Lophantherum gracile brongn and the medicine efficacy.

  18. Standard test method for determining elements in waste Streams by inductively coupled plasma-atomic emission spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This test method covers the determination of trace, minor, and major elements in waste streams by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) following an acid digestion of the sample. Waste streams from manufacturing processes of nuclear and non-nuclear materials can be analyzed. This test method is applicable to the determination of total metals. Results from this test method can be used to characterize waste received by treatment facilities and to formulate appropriate treatment recipes. The results are also usable in process control within waste treatment facilities. 1.2 This test method is applicable only to waste streams that contain radioactivity levels that do not require special personnel or environmental protection. 1.3 A list of the elements determined in waste streams and the corresponding lower reporting limit is found in Table 1. 1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids. The com...

  19. Determination of total arsenic content in water by atomic absorption spectroscopy (AAS) using vapour generation assembly (VGA).

    Science.gov (United States)

    Behari, Jai Raj; Prakash, Rajiv

    2006-03-01

    Analysis of arsenic in water is important in view of contamination of ground water with arsenic in some parts of the world including West Bengal in India and neighboring country Bangladesh. WHO has fixed the threshold for arsenic in drinking water to 10ppb (microg/l) level, hence the methodology for determination of arsenic is required to be sensitive at ppb level. Atomic absorption spectrophotometry with vapour generation assembly (AAS-VGA) is well known technique for the trace analysis of arsenic. However, total arsenic analysis [As(III)+As(V)] is very crucial and it requires reduction of As(V) to As(III) for correct analysis. As(III) is reduced to AsH3 vapours and finally to free As atoms, which are responsible for absorption signal in AAS. To accomplish this the vapour generation assembly attached to AAS has acid channel filled with 10 M HCl and the reduction channel with sodium borohydride. Further sample can be reduced either before aspiration for analysis, using potassium iodide (KI) or the sample can be introduced in the instrument directly and KI can be added in the reduction channel along with the sodium borohydride. The present work shows that samples prepared in 3 M HCl can be reduced with KI for 30 min before introduction in the instrument. Alternatively samples can be prepared in 6 M HCl and directly aspirated in AAS using KI in VGA reduction channel. The latter methodology is more useful when the sample size is large and time cycle is difficult to maintain. It is observed that the acid concentration of the sample in both the situations plays an important role. Further reduction in acid concentration and analysis time is achieved for the arsenic analysis by using modified method. Analysis in both the methods is sensitive at ppb level.

  20. Determination of manganese in diesel, gasoline and naphtha by graphite furnace atomic absorption spectrometry using microemulsion medium for sample stabilization

    Science.gov (United States)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; de Castro, Eustáquio Vinicius Ribeiro; de Jesus, Honério Coutinho

    2008-08-01

    The determination of Mn in diesel, gasoline and naphtha samples at µg L - 1 level by graphite furnace atomic absorption spectrometry, after sample stabilization in a three-component medium (microemulsion) was investigated. Microemulsions were prepared by mixing appropriate volumes of sample, propan-1-ol and nitric acid aqueous solution, and a stable system was immediately and spontaneously formed. After multivariate optimization by central composite design the optimum microemulsion composition as well as the temperature program was defined. In this way, calibration using aqueous analytical solution was possible, since the same sensitivity was observed in the optimized microemulsion media and 0.2% v/v HNO 3. The use of modifier was not necessary. Recoveries at the 3 µg L - 1 level using both inorganic and organic Mn standards spiked solutions ranged from 98 to 107% and the limits of detection were 0.6, 0.5 and 0.3 µg L - 1 in the original diesel, gasoline and naphtha samples, respectively. The Mn characteristic mass 3.4 pg. Typical relative standard deviation ( n = 5) of 8, 6 and 7% were found for the samples prepared as microemulsions at concentration levels of 1.3, 0.8, and 1.5 µg L - 1 , respectively. The total determination cycle lasted 4 min for diesel and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h - 1 for duplicate determinations in diesel and 10 h - 1 for duplicate determinations in gasoline and naphtha. Accuracy was also assessed by using other method of analysis (ASTM D 3831-90). No statistically significant differences were found between the results obtained with the proposed method and the reference method in the analysis of real samples.

  1. Direct and combined methods for the determination of chromium, copper, and nickel in honey by electrothermal atomic absorption spectroscopy.

    Science.gov (United States)

    Rodríguez García, J C; Barciela García, J; Herrero Latorre, C; García Martín, S; Peña Crecente, R M

    2005-08-24

    In the present work, direct methods for the determination of chromium, copper, and nickel in honey by electrothermal atomic absorption spectroscopy were developed using experimental design as an optimization tool. Once the optimum conditions for the individual methods were established, a direct method for the combined determination of the three elements was optimized using the response surface tool. Palladium was used as chemical modifier in all cases. Honey was diluted in water, hydrogen peroxide, and nitric acid. Triton X-100 was added to minimize the matrix effect and the viscosity of the sample. The RSD (better than 10%) and the analytical recovery (98-103%) were acceptable for all of the developed methods. Calibration graphs were used in the four methods to determine the concentration of the analytes in the sample. The detection limits of the combined method (0.21, 0.35, and 0.37 microg L(-)(1) for Cr, Cu, and Ni, respectively) were similar to those obtained for the individual methods (LOD = 0.17, 0.21, 0.33 microg L(-)(1) for Cr, Cu, and Ni, respectively). The direct-combined proposed method has been applied to the determination of chromium, copper, and nickel content in representative honey samples from Galicia (northwestern Spain). The concentrations found in the analyzed samples were in the range of (5.75 +/- 0.64)-(26.4 +/- 0.38) ng g(-)(1) of Cr, (79 +/- 7.8)-(2049 +/- 80) ng g(-)(1) of Cu, and (12.6 +/- 1.36)-(172 +/- 6.88) ng g(-)(1) of Ni.

  2. Electrothermal atomic absorption spectrometric determination of cobalt, copper, lead and nickel traces in aragonite following flotation and extraction separation.

    Science.gov (United States)

    Zendelovska, D; Pavlovska, G; Cundeva, K; Stafilov, T

    2001-03-30

    A method of determination of Co, Cu, Pb and Ni in nanogram quantities from aragonite is presented. Flotation and extraction of Co, Cu, Pb and Ni is suggested as methods for elimination matrix interferences of calcium. The method of flotation is performed by iron(III) hexamethylenedithiocarbamate, Fe(HMDTC)(3), as a colloid precipitate collector. The liquid-liquid extraction of Co, Cu, Pb and Ni is carried out by sodium diethyldithiocarbamate, NaDDTC, as complexing reagent into methylisobutyl ketone, MIBK. The electrothermal atomic absorption spectrometry (ETAAS) is used for determination of analytes. The detection limits of ETAAS followed by flotation are: 7.8 ng.g(-1) for Co, 17.1 ng.g(-1) for Cu, 7.2 ng.g(-1) for Pb and 9.0 mug.g(-1) for Ni. The detection limits of ETAAS followed by extraction are found to be: 12.0 ng.g(-1) for Co, 51.0 ng.g(-1) for Cu, 24.0 ng.g(-1) for Pb and 21.0 ng.g(-1) for Ni.

  3. Mercury determination in non- and biodegradable materials by cold vapor capacitively coupled plasma microtorch atomic emission spectrometry.

    Science.gov (United States)

    Frentiu, Tiberiu; Mihaltan, Alin I; Ponta, Michaela; Darvasi, Eugen; Frentiu, Maria; Cordos, Emil

    2011-10-15

    A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min(-1) Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl(2) reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO(3)-H(2)SO(4) mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml(-1) or 0.08 μg g(-1) in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg(-1), while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level).

  4. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Qingxiang, E-mail: zhouqx@cup.edu.cn [School of Chemistry and Environmental Sciences, Henan Normal University, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huaihe River Water Environment and Pollution Control, Ministry of Education, Xinxiang 453007 (China); State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Zhao, Na [State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Xie, Guohong [College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003 (China)

    2011-05-15

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL{sup -1} (r{sup 2} = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L{sup -1}. Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%.

  5. Cloud point extraction for the preconcentration of silver and palladium in real samples and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, Hossein; Yazdandoust, Saeed; Yazdandoust, Mozhdeh [Department of Chemistry, Payame Noor University (PNU), Shiraz (Iran)

    2010-03-15

    A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag{sup +} and Pd{sup 2+} in various samples. After complexation with 2-((2-((1H-benzo[d]imidazole-2-yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X-114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0.10{sup -5} mol/L BIMPI and 0.036% (w/v) Triton X-114), calibration graphs were linear in the range of 28.0-430.0 {mu}g/L and 57.0-720.0 {mu}g/L with detection limits of 10.0 and 25.0 {mu}g/L for Ag{sup +} and Pd{sup 2+}, respectively. The enrichment factors were 35.0 and 28.0 for Ag{sup +} and Pd{sup 2+}, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  6. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of fluoroquinolone antibiotics using ammonium reineckate ion-pair complex formation

    Science.gov (United States)

    Ragab, Gamal H.; Amin, Alaa S.

    2004-03-01

    Three accurate, rapid and simple atomic absorption spectrometric, conductometric and colorimetric methods were developed for the determination of norfloxacin (NRF), ciprofloxacin (CIP), ofloxacin (OFL) and enrofloxacin (ENF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone in the range 5.0-65, 4.0-48, 5.0-56 and 6.0-72 μg ml -1 of NRF, CPF, OFL and ENF, respectively. The optimizations of various experimental conditions were described. The results obtained showed good recoveries of 99.15±1.15, 99.30±1.40, 99.60±1.50, and 99.00±1.25% with relative standard deviations of 0.81, 1.06, 0.97, and 0.69% for NRF, CPF, OFL, and ENF, respectively. Applications of the proposed methods to representative pharmaceutical formulations are successfully presented.

  7. Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo

    2005-01-01

    In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix by inductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line of yttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium. In this work, a method based on wavelet transform was proposed for the spectral interference correction. Haar wavelet was selected as the mother wavelet. The discrete detail after the third decomposition, D3,was chosen for quantitative analysis based on the consideration of both separation degree and peak height. The linear correlation coefficient between the height of the left positive peak in D3 and the concentration of Y was calculated to be 0.9926.Six synthetic samples were analyzed, and the recovery for yttrium varied from 96.3% to 110.0%. The amounts of yttrium in three ytterbium metal samples were determined by the proposed approach with an average relative standard deviation (RSD)of 2.5%, and the detection limit for yttrium was 0.016%. This novel correction technique is fast and convenient, since neither complicated model assumption nor time-consuming iteration is required. Furthermore, it is not affected by the wavelength drift inherent in monochromators that will severely reduce the accuracy of results obtained by some chemometric methods.

  8. Determination of total arsenic in coal and wood using oxygen flask combustion method followed by hydride generation atomic absorption spectrometry.

    Science.gov (United States)

    Geng, Wenhua; Furuzono, Takuya; Nakajima, Tsunenori; Takanashi, Hirokazu; Ohki, Akira

    2010-04-15

    A simple and sensitive procedure for the determination of total arsenic in coal and wood was conducted by use of oxygen flask combustion (OFC) followed by hydride generation atomic absorption spectrometry (HGAAS). The effect of various items (composition of absorbent, standing time between the combustion and filtration, particle size and mass of sample) was investigated. Under the optimized conditions of the OFC method, nine certified reference materials were analyzed, and the values of arsenic concentration obtained by this method were in good accordance with the certified values. The limit of detection (LOD) and relative standard deviation (RSD) of the method were 0.29 microg g(-1) and less than 8%, respectively. In addition, eight kinds of coals and four chromated copper arsenate (CCA)-treated wood wastes were analyzed by the present method, and the data were compared to those from the microwave-acid digestion (MW-AD) method. The determination of arsenic in solid samples was discussed in terms of applicable scope and concentration range of arsenic.

  9. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A., E-mail: djan@terra.com.br

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v{sup −1} of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L{sup −1} with a limit of detection of 4.9 μg L{sup −1} and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L{sup −1} Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials. - Highlights: ► Molybdenum was determined in plants by flame AAS. ► Flame AAS sensitivity was improved using microextraction and discrete nebulization. ► The developed procedure can be easily implemented in routine analysis. ► Green chemistry principles are followed.

  10. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Teslima Daşbaşı

    2016-01-01

    Full Text Available A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4- complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n=13. The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1 and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water.

  11. Preconcentration procedure using cloud point extraction in the presence of electrolyte for cadmium determination by flame atomic absorption spectrometry

    Science.gov (United States)

    Coelho, Luciana Melo; Arruda, Marco Aurélio Zezzi

    2005-06-01

    This paper describes a micelle-mediated phase separation in the presence of electrolyte as a preconcentration method for cadmium determination by flame atomic absorption spectrometry (FAAS). Cadmium was complexed with ammonium O,O-diethyldithiophosphate (DDTP) in an acidic medium (0.32 mol l- 1 HCl) using Triton X-114 as surfactant and quantitatively extracted into a small volume (about 20 μl) of the surfactant-rich phase after centrifugation. The chemical variables that affect the cloud point extraction, such as complexing time (0 20 min), Triton X114 concentration (0.043 0.87% w/v) and complexing agent concentration (0.01 0.1 mol l- 1), were investigated. The cloud point is formed in the presence of NaCl at room temperature (25 °C), and the electrolyte concentration (0.5 5% w/v) was also investigated. Under optimized conditions, only 8 ml of sample was used in the presence of 0.043% w/v Triton X-114 and 1% (w/v) NaCl. This method permitted limits of detection and quantification of 0.9 μg l- 1 and 2.9 μg l- 1 Cd, respectively, and a linear calibration range from 3 to 400 μg l- 1 Cd. The proposed method was applied to Cd determination in physiological solutions (containing 0.9% (w/v) of NaCl), mineral water, lake water and cigarette samples (tobacco).

  12. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Mei, E-mail: sunmei@ustc.edu.cn [Hefei National Laboratory for Physical Sciences on Microscale, University of Science and Technology of China, No. 96, Jinzhai Road, Hefei 230026 (China); Wu Qianghua [Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL{sup -1}. The relative standard deviation (n = 7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin.

  13. Selective speciation of inorganic antimony on tetraethylenepentamine bonded silica gel column and its determination by graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mendil, Durali; Bardak, Hilmi; Tuzen, Mustafa; Soylak, Mustafa

    2013-03-30

    A speciation system for antimony (III) and antimony (V) ions that based on solid phase extraction on tetraethylenepentamine bonded silica gel has been established. Antimony was determined by graphite furnace atomic absorption spectrometry (GF-AAS). Analytical conditions including pH, sample volume, etc., were studied for the quantitative recoveries of Sb (III) and Sb (V). Matrix effects on the recovery were also investigated. The recovery values and detection limit for antimony (III) at optimal conditions were found as >95% and 0.020 μg L(-1), respectively. Preconcentration factor was calculated as 50. The capacity of adsorption for the tetraethylenepentamine bonded silica gel was 7.9 mg g(-1). The validation was checked by analysis of NIST SRM 1573a Tomato laves and GBW 07605 Tea certified reference materials. The procedure was successfully applied to speciation of antimony in tap water, mineral water and spring water samples. Total antimony was determined in refined salt, unrefined salt, black tea, rice, tuna fish and soil samples after microwave digestion and presented enrichment method combination. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Woińska, Sylwia; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L - 1 thiourea in 0.3 mol L - 1 HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL - 1 for Pt and 0.012 ng mL - 1 for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g - 1 for Pt and 1.24 mg g - 1 for Pd.

  15. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  16. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woinska, Sylwia; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L{sup -1} thiourea in 0.3 mol L{sup -1} HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL{sup -1} for Pt and 0.012 ng mL{sup -1} for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g{sup -1} for Pt and 1.24 mg g{sup -1} for Pd.

  17. Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).

    Science.gov (United States)

    Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur

    2014-10-01

    A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified.

  18. Immersed single-drop microextraction-electrothermal vaporization atomic absorption spectroscopy for the trace determination of mercury in water samples.

    Science.gov (United States)

    Bagheri, Habib; Naderi, Mehrnoush

    2009-06-15

    A new method based on single-drop microextraction (SDME) combined with electrothermal vaporization atomic absorption spectroscopy (ETV-AAS) was developed for the trace determination of mercury in water samples. A microdrop of m-xylene was applied as the extraction solvent. After extraction, the microdrop was introduced, directly, into a graphite furnace of AAS. Some important extraction parameters such as type of solvent, volume of solvent, sample stirring, ionic strength, sample pH, chelating agent concentration, sample temperature, and extraction time were investigated and optimized. The highest possible microdrop volume of 10 microL, a sampling temperature of 27 degrees C, and use of m-xylene containing dithizone, as complexing agent, are major parameters led to achieve a high enrichment factor of 970. Under the optimized conditions, the detection limit of the method was 0.01 microg L(-1) and the relative standard deviation was 6.1% (n=7). The proposed method has been successfully applied to the determination of Hg in two river water samples. The effects of interfering species such as Pt, Pd, Cu, Au, and Bi, having the tendency to form complexes with dithizone, at two concentration levels of 100 and 1000 microg L(-1) were also studied.

  19. Wealth status, mid upper arm circumference (MUAC and antenatal care (ANC are determinants for low birth weight in Kersa, Ethiopia.

    Directory of Open Access Journals (Sweden)

    Nega Assefa

    Full Text Available BACKGROUND: Low Birth Weight (LBW is one of the major risk factor for death in early life. However, little is known about predictors of LBW in sub-Saharan Africa. Therefore, the aim of this study was to measure the incidence and determinants of LBW in a rural population of Ethiopia. METHODS: An observational cohort study on pregnant women was conducted from December 2009 to November 2010. During the study period 1295 live birth were registered and the weights of 956 children were measured within 24 hours after birth. Socio-demographic, economic, maternal and organizational factors were considered as a predicators of LBW, defined as birth weight below 2500g. Logistic regression was used to analyze the data, odds ratio (OR and confidence intervals (CI are reported. RESULT: The incidence of LBW was 28.3%. It is significantly associated with poverty [OR 2.1; 95% CI: 1.42, 3.05], maternal Mid Upper Arm Circumference (MUAC less than 23 cm [OR 1.6; 95% CI: 1.19, 2.19], not attending ANC [OR 1.6; 95% CI: 1.12, 2.28], mother's experience of physical violence during pregnancy [OR 1.7; 95% CI: 1.12, 2.48], and longer time to walk to health facility [OR 1.6; 95% CI: 1.11, 2.40]. CONCLUSION AND RECOMMENDATION: The incidence of LBW was high in Kersa. Babies born to women who were poor, undernourished, experienced physical violence during pregnancy and who had poor access to health services were more likely to be LBW in this part of the country. In this largely poor community where ANC coverage is low, to reduce the incidence of LBW, it is essential to improve access for maternal health care. The involvement of husbands and the community at large to seek collective action on LBW is essential.

  20. Determination of the positions of aluminum atoms introduced into SSZ-35 and the catalytic properties of the generated Brønsted acid sites.

    Science.gov (United States)

    Miyaji, Akimitsu; Kimura, Nobuhiro; Shiga, Akinobu; Hayashi, Yoshihiro; Nishitoba, Toshiki; Motokura, Ken; Baba, Toshihide

    2017-03-01

    The positions of aluminum (Al) atoms in SSZ-35 together with the characteristics of the generated protons were investigated by (27)Al multiple quantum magic-angle spinning (MQ-MAS), (29)Si MAS, and (1)H MAS NMR data analyses accompanied by a variable temperature (1)H MAS NMR analysis. The origin of the acidic -OH groups (Brønsted acid sites) generated by introducing Al atoms into the T sites was investigated and the T sites introduced into the Al atoms were revealed. To further determine the catalytic properties of the acidic protons generated in SSZ-35, the influence of the concentration of the Al atoms on the catalytic activity and selectivity during the transformation of toluene was examined.

  1. On the opportunity of spectroscopic determination of absolute atomic densities in non-equilibrium plasmas from measured relative intensities within resonance multiplets distorted by self-absorption

    CERN Document Server

    Lavrov, B P

    2007-01-01

    The opportunities of the application of the recently proposed approach in optical emission spectroscopy of non-equilibrium plasmas have been studied. The approach consists of several methods of the determination of {\\em absolute} particle densities of atoms from measured {\\em relative} intensities within resonance multiplets distorted by self-absorption. All available spectroscopic data concerning resonance spectral lines of atoms having multiplet ground states from boron up to gallium were analyzed. It is found that in the case of C, O, F, S and Cl atoms an application of the methods needs VUV technique, while densities of B, Al, Si, Sc, Ti, V, Co, Ni, Ga atoms may be obtained by means of the intensity measurements in UV and visible parts of emission spectra suitable for ordinary spectrometers used for optical diagnostics and monitoring of non-equilibrium plasmas including industrial plasma technologies.

  2. Determination of phytate in high molecular weight, charged organic matrices by two-dimensional size exclusion-ion chromatography.

    Science.gov (United States)

    Elkin, Kyle R; Slingsby, Rosanne; Bryant, Ray B

    2016-08-15

    A two-dimensional chromatography method for analyzing phytate or other ionic targets in matrices containing high molecular weight, charged organic species is described. Prior to quantification by anion exchange chromatography, the sample matrix was prepared by size exclusion chromatography, which removed the majority of the matrix. Quantification of phytate on the AS11-HC was sensitive (0.25µM, 0.17mg/l) and reproducible (4.6% RSD) allowing this method to provide baseline separation of phytate from a manure extract within 14min. The method is simple, requiring only sample filtering, reproducible (between-run variation 5% RSD) and linear from 0.38 to 76µM (0.25-50mg/l). The method is suitable for routine determination of phytate in high organic matrices such as manure extracts.

  3. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hagarová, Ingrid, E-mail: hagarova@fns.uniba.sk; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb–dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l{sup −1} HNO{sub 3}. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l{sup −1}, quantification limit of 0.38 μg l{sup −1}, relative standard deviation of 4.2% (for 2 μg l{sup −1} of Pb; n = 26), linearity of the calibration graph in the range of 0.5–4.0 μg l{sup −1} (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91–96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters. - Highlights: • The potential of coacervates for the extraction of metal ions is examined. • No difficulties in coupling of ETAAS with the proposed CAE are observed. • Achieved preconcentration factor results in enhanced sensitivity. • Analytical performance is confirmed by the reliable determination of trace Pb. • The proposed CAE is ecofriendly and efficient.

  4. Atomic Force Microscopy Determination of Young’s Modulus of Bovine Extra-ocular Tendon Fiber Bundles

    Science.gov (United States)

    Yoo, Lawrence; Reed, Jason; Shin, Andrew; Demer, Joseph L.

    2014-01-01

    Extra-ocular tendons (EOTs) transmit the oculorotary force of the muscles to the eyeball to generate dynamic eye movements and align the eyes, yet the mechanical properties of the EOTs remain undefined. The EOTs are known to be composed of parallel bundles of small fibers whose mechanical properties must be determined in order to characterize the overall behavior of EOTs. The current study aimed to investigate the transverse Young’s modulus of EOT fiber bundles using atomic force microscopy (AFM). Fresh bovine EOT fiber bundle specimens were maintained under temperature and humidity control, and indented 100 nm by the inverted pyramid tip of an AFM (Veeco Digital Instruments, NY). Ten indentations were conducted for each of 3 different locations of 10 different specimens from each of 6 EOTs, comprising a total of 1,800 indentations. Young’s modulus for each EOT was determined using a Hertzian contact model. Young’s moduli for fiber bundles from all six EOTs were determined. Mean Young’s moduli for fiber bundles were similar for the six anatomical EOTs: lateral rectus 60.12 ± 2.69 (±SD) MPa, inferior rectus 59.69 ± 5.34 MPa, medial rectus 56.92 ±1.91 MPa, superior rectus 59.66 ±2.64 MPa, inferior oblique 57.7± 1.36 MPa, and superior oblique 59.15± 2.03. Variation in Young’s moduli among the six EOTs was not significant (P > 0.25). The Young’s modulus of bovine EOT fibers is highly uniform among the six extraocular muscles, suggesting that each EOT is assembled from fiber bundles representing the same biomechanical elements. This uniformity will simplify overall modeling. PMID:24767704

  5. Determination of the surface free energy of crystalline and amorphous lactose by atomic force microscopy adhesion measurement.

    Science.gov (United States)

    Zhang, Jianxin; Ebbens, Stephen; Chen, Xinyong; Jin, Zheng; Luk, Shen; Madden, Claire; Patel, Nikin; Roberts, Clive J

    2006-02-01

    This study was conducted to accurately measure the dispersive surface free energy of lactose solids in ordered and disordered states. Atomic force microscopy (AFM) was used to determine the contact adhesion force between an AFM tip and lactose under low humidity (ca. 1% RH). The geometry of the tip contacting apex was characterized by scanning a porous aluminum film with ultrasharp spikes (radius 2-3 nm). A sphere vs. flat surface model was employed to relate the adhesion force determined to the surface energy based upon the Johnson-Kendal-Roberts theory. Spray-dried amorphous lactose in a compressed-disk form and single crystals of alpha-lactose monohydrate were prepared as model samples. The condition of the smooth sample surface and sphere-shaped tip used was shown to be appropriate to the application of the JKR model. The surface energy of crystalline [(0,-1,-1) face] and amorphous lactose was determined to be 23.3 +/- 2.3 and 57.4 +/- 7.9 mJ m(-2), respectively. We have demonstrated the capability of AFM to measure the dispersive surface free energy of pharmaceutical materials directly through a blank probe at the nanometer scale. These data, although consistent with results from more traditional methods, illustrate some unique attributes of this approach, namely, surface energies are directly derived from solid-solid interactions, measurements may be made on specific crystalline faces, and the potential exists to identify the submicron heterogeneity of organic solids in terms of their molecular energy states (such as ordered and disordered lactose).

  6. Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

    2011-10-10

    Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

  7. Determination of Pb(Ⅱ) and Cu(Ⅱ) by Electrothermal Atomic Absorption Spectrometry after Preconcentration by a Schiff Base Adsorbed on Surfactant Coated Alumina

    Institute of Scientific and Technical Information of China (English)

    SABER TEHRANI Mohammad; RASTEGAR Faramarz; PARCHEHBAF Ayob; KHATAMIAN Masoomeh

    2006-01-01

    1,2-Bis(salicylidenamino)ethane loaded onto sodium dodecyl sulfate-coated alumina was used as a new chelating sorbent for the preconcentration of traces of Pb(Ⅱ) and Cu(Ⅱ) prior to atomic absorption spectrometric determination. The influence of pH, flow rates of sample and eluent solutions, and foreign ions on the recovery of Pb(Ⅱ)by electrothermal atomic absorption spectrometry (ETAAS). The data of limit of detection (3σ) for Pb(Ⅱ) and Cu(Ⅱ)posed method was successfully applied to determination of lead and copper in different water samples.

  8. {sup 252}Cf plasma desorption and laser desorption mass spectrometry for the determination of molecular weight distribution of coal derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, B.R.; Bartle, K.D.; Ross, A.B.; Herod, A.A.; Kandiyoti, R.; Larsen, J.W. [University of Leeds, Leeds (United Kingdom). School of Chemistry

    1999-11-01

    A detailed knowledge of the molecular mass (MM) distribution in coal and its derived products is essential for a fundamental understanding of coal structure, and of the processes occurring during coal conversion. Fractionation using size exclusion chromatography (s.e.c.) using N-methyl-2-pyrrolidinone as the mobile phase has been applied to such materials and has provided improved MM distributions. Absolute calibration has been provided using matrix assisted laser desorption ionisation mass spectrometry (MAl.d.I.-m.s.). An alternative method of volatilising and ionising large molecules for mass spectrometry (m.s.) is {sup 252}Cf plasma desorption ({sup 252}Cf p.d.-m.s.). This involves the use of energetic fission fragments from the decay of {sup 252}Cf and produces mass spectra consisting predominantly of molecular ions from a range of polymers and biomolecules. This has been used by other workers to determine the molecular weight distribution of heavy distillation residues obtained from coal liquefaction processes either unfractionated or fractionated into broad fractions. Generally, a good agreement was obtained between values of MM determined by {sup 252}Cf p.d.-m.s. and s.e.c. A comparison is reported of MM distribution determined by {sup 252}Cf p.d.-m.s. and laser desorption mass spectrometry (l.d.-m.s.) for narrower fractions separated by s.e.c. from a coal tar pitch. 19 refs., 4 figs., 1 tab.

  9. Development and evaluation of a questionnaire for assessment of determinants of weight disorders among children and adolescents: The Caspian-IV study

    Directory of Open Access Journals (Sweden)

    Roya Kelishadi

    2012-01-01

    Conclusion: The developed questionnaire is a valid and reliable tool for assessment of the determinants of weight disorders in a nationally representative sample of children and adolescents in the MENA.

  10. Freon (CHF3)-assisted atomization for the determination of titanium using ultrasonic slurry sampling-graphite furnace atomic absorption spectrometry (USS-GFAAS): a simple and advantageous method for solid samples.

    Science.gov (United States)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2004-06-01

    A simple and advantageous method for the determination of titanium using graphite furnace atomic absorption spectrometry with slurry sampling has been developed. Titanium is one of the refractory elements that form thermally stable carbides in the graphite tube, which leads to severe memory effects. Trifluoromethane (Freon-23) was applied in the purge gas during the atomization step or alternatively just prior to the atomization to successfully eliminate the problems of carbide formation and increase the lifetime of the furnace tube which could be used for more than 600 heating cycles. A flow rate of 40 mL min(-1) (5% of Freon in argon) was used to obtain symmetrical peaks with no tailing. However, when the gas flow rate was too high (250 mL min(-1)) the peak-tailing and memory effects reappeared. Ti was determined in various materials covering a wide range of concentrations, from 2.8 microg g(-1) to 12% (m/m) Ti. The accuracy of the method was confirmed by analyzing certified reference materials (CRMs) or by comparing the results with those obtained using inductively coupled plasma-atomic emission spectrometry (ICP-AES) after decomposition of the samples. The materials analyzed were soil, plant, human hair, coal, urban particulate matters, toothpaste, and powdered paint.

  11. Continuous Determination of Heavy Metals in Water by Atomic Fluorescence and Atomic Absorption Spectrometry%原子荧光和原子吸收法连续测定水中的重金属

    Institute of Scientific and Technical Information of China (English)

    谢倩

    2015-01-01

    通过剖析原子荧光和原子吸收法的不同消解体系,优化实验条件,确定了原子荧光和原子吸收法连续测定水中的硒、砷、锌、铜的含量的最佳消解条件和最佳仪器测定条件。经加标回收以及标样分析,连续测定的灵敏度高,回收率在95.9%~109%之间,相对标准误差低于4.41%,操作简便快速,结果精确。%By analyzing the different digestion system of atomic fluorescence and atomic absorption method and optimizing experimental conditions, the optimal digestion conditions and the best measurement conditions of instruments for continuous determination selenium, arsenic, zinc, copper content in water by atomic fluorescence and atomic absorption spectrometry were determined.Spiking recovery and standard analysis result showed that continuous measurement had high sensitivity, and the recoveries was between 95.9% and 109%, relative standard deviation was less than 4.41%, the operation was simple, rapid and accurate.

  12. Determination of Copper by Graphite Furnace Atomic Absorption Spectrophotometry: A Student Exercise in Instrumental Methods of Analysis.

    Science.gov (United States)

    Williamson, Mark A.

    1989-01-01

    Discusses a student exercise which requires the optimizing of the charring and atomization temperatures by producing a plot of absorbance versus temperature for each temperature parameter. Notes that although the graphite furnace atomic absorption spectroscopy technique has widespread industrial use, there are no published, structured experiments…

  13. Peptidylation for the determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Tang, Feng; Cen, Si-Ying; He, Huan; Liu, Yi; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-05-23

    Determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has been a great challenge in the analytical research field. Here we developed a universal peptide-based derivatization (peptidylation) strategy for the sensitive analysis of low-molecular-weight compounds by MALDI-TOF-MS. Upon peptidylation, the molecular weights of target analytes increase, thus avoiding serious matrix ion interference in the low-molecular-weight region in MALDI-TOF-MS. Since peptides typically exhibit good signal response during MALDI-TOF-MS analysis, peptidylation endows high detection sensitivities of low-molecular-weight analytes. As a proof-of-concept, we analyzed low-molecular-weight compounds of aldehydes and thiols by the developed peptidylation strategy. Our results showed that aldehydes and thiols can be readily determined upon peptidylation, thus realizing the sensitive and efficient determination of low-molecular-weight compounds by MALDI-TOF-MS. Moreover, target analytes also can be unambiguously detected in biological samples using the peptidylation strategy. The established peptidylation strategy is a universal strategy and can be extended to the sensitive analysis of various low-molecular-weight compounds by MALDI-TOF-MS, which may be potentially used in areas such as metabolomics.

  14. Determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry.

    Science.gov (United States)

    Silva, Laiana O B; Leao, Danilo J; dos Santos, Debora C; Matos, Geraldo D; de Andrade, Jailson B; Ferreira, Sergio L C

    2014-09-01

    The present paper describes the development of a method for the determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry (CVG AAS). Chemometric tools were employed to characterize the influence of several factors on the generation of volatile copper species. First, a two-level full factorial design was performed that included the following chemical variables: hydrochloric acid concentration, tetrahydroborate concentration, sulfanilamide concentration and tetrahydroborate volume, using absorbance as the response. Under the established experimental conditions, the hydrochloric acid concentration had the greatest influence on the generation of volatile copper species. Subsequently, a Box-Behnken design was performed to determine the optimum conditions for these parameters. A second chemometric study employing a two-level full factorial design was performed to evaluate the following physical factors: tetrahydroborate flow rate, flame composition, alcohol volume and sample volume. The results of this study demonstrated that the tetrahydroborate flow rate was critical for the process. The chemometric experiments determined the following experimental conditions for the method: hydrochloric acid concentration, 0.208 M; tetrahydroborate concentration, 4.59%; sulfanilamide concentration, 0.79%; tetrahydroborate volume, 2.50 mL; tetrahydroborate flow rate, 6.50 mL min(-1); alcohol volume, 200 µL; and sample volume, 7.0 mL. Thus, this method, using a slurry volume of 500 µL and a final dilution of 7 mL, allowed for the determination of copper with limits of detection and quantification of 0.30 and 0.99 µg L(-1), respectively. Precisions, expressed as RSD%, of 4.6 and 2.8% were obtained using copper solutions at concentrations of 5.0 and 50.0 µg L(-1), respectively. The accuracy was evaluated by the analysis of a certified reference material of urban particulate matter. The copper concentration

  15. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    Science.gov (United States)

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures.

  16. Lead concentrations and isotope ratios in street dust determined by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Nageotte, S M; Day, J P

    1998-01-01

    A major source of environmental lead, particularly in urban areas, has been from the combustion of leaded petrol. Street dust has previously been used to assess urban lead contamination, and the dust itself can also be a potential source of lead ingestion, particularly to children. The progressive reduction of lead in petrol, in recent years, would be expected to have been reflected in a reduction of lead in urban dust. We have tested this hypothesis by repeating an earlier survey of Manchester street dust and carrying out a comparable survey in Paris. Samples were collected from streets and parks, lead was extracted by digestion with concentrated nitric acid and determined by electrothermal atomic absorption spectrometry. Lead isotope ratios were measured by inductively coupled plasma mass spectrometry. Results for Manchester show that lead concentrations have fallen by about 40% (street dust averages, 941 micrograms g-1 (ppm) in 1975 down to 569 ppm in 1997). In Paris, the lead levels in street dust are much higher and significant differences were observed between types of street (not seen in Manchester). Additionally, lead levels in parks were much lower than in Manchester. Samples collected under the Eiffel Tower had very high concentrations and lead isotope ratios showed that this was unlikely to be fallout from motor vehicles but could be due to the paint used on the tower. Isotope ratios measurements also revealed that lead additives used in France and the UK come from different sources.

  17. On-line preconcentration of copper as its pyrocatechol violet complex on Chromosorb 105 for flame atomic absorption spectrometric determinations

    Energy Technology Data Exchange (ETDEWEB)

    Buke, Berrin [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey); Divrikli, Umit [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey)], E-mail: udivrikli@pamukkale.edu.tr; Soylak, Mustafa [Chemistry Department, Science and Arts Faculty, Erciyes University, 38039 Kayseri (Turkey); Elci, Latif [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey)

    2009-04-30

    An on-line solid phase extraction method for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry (FAAS) has been described. It is based on the adsorption of copper(II) ion onto a home made mini column of Chromosorb 105 resin loaded with pyrocatechol violet at the pH range of 5.0-8.0, then eluted with 1 mol L{sup -1} HNO{sub 3}. Several parameters, such as pH of the sample solution, amount of Chromosorb 105 resin, volume of sample and eluent, type of eluent, flow rates of sample and eluent, governing the efficiency and throughput of the method were evaluated. The concentration of the copper ion detected after preconcentration was in agreement with the added amount. At optimized conditions, for 15 min of preconcentration time (30 mL of sample volume), the system achieved a detection limit of 0.02 {mu}g L{sup -1}, with relative standard deviation 1.1% at 0.03 {mu}g mL{sup -1} copper. The present method was found to be applicable to the preconcentration of Cu(II) in natural water samples.

  18. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Senturk, Hasan Basri; Gundogdu, Ali [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 28049 Giresun (Turkey); Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-10-22

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L{sup -1} HNO{sub 3} in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 {mu}g L{sup -1}, respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g{sup -1}. The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

  19. Sequential injection ionic liquid dispersive liquid-liquid microextraction for thallium preconcentration and determination with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Anthemidis, Aristidis N.; Ioannou, Kallirroy-Ioanna G. [Aristotle University, Laboratory of Analytical Chemistry, Department of Chemistry, Thessaloniki (Greece)

    2012-08-15

    A novel, automatic on-line sequential injection dispersive liquid-liquid microextraction (SI-DLLME) method, based on 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF{sub 6}]) ionic liquid as an extractant solvent was developed and demonstrated for trace thallium determination by flame atomic absorption spectrometry. The ionic liquid was on-line fully dispersed into the aqueous solution in a continuous flow format while the TlBr{sub 4} {sup -} complex was easily migrated into the fine droplets of the extractant due to the huge contact area of them with the aqueous phase. Furthermore, the extractant was simply retained onto the surface of polyurethane foam packed into a microcolumn. No specific conditions like low temperature are required for extractant isolation. All analytical parameters of the proposed method were investigated and optimized. For 15 mL of sample solution, an enhancement factor of 290, a detection limit of 0.86 {mu}g L{sup -1} and a precision (RSD) of 2.7% at 20.0 {mu}g L{sup -1} Tl(I) concentration level, was obtained. The developed method was evaluated by analyzing certified reference materials while good recoveries from environmental and biological samples proved that present method was competitive in practical applications. (orig.)